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Wake Forest University<br />

Chemistry Department, Salem Hall<br />

CHEMICAL HYGIENE PLAN<br />

AND<br />

SAFETY MANUAL<br />

Date <strong>of</strong> Last Revision: June 13, 2007<br />

List <strong>of</strong> Contributors<br />

Michelle Adkins [WFU Environmental Health and Safety(EHS) Director], Dr. Rebecca Alexander (Chemistry Department),<br />

Dr. Uli Bierbach (Chemistry Department), Dr. Christa Colyer (Chemistry Department), Scott Frazier [WFU Assistant<br />

Environmental Health and Safety (EHS) Director], Dr. Willie Hinze (Chemistry Department), Dr. Paul Jones (Chemistry<br />

Department), Dr. Bruce King (Chemistry Department), Dr. Dilip Kondepudi (Chemistry Department), Dr. Abdu Lachgar<br />

(Chemistry Department), Dr. Ronald N<strong>of</strong>tle (Chemistry Department), Dr. Robert Sw<strong>of</strong><strong>for</strong>d, (Chemistry Department),<br />

Michael Thompson (Lab Manager, Chemistry Department), Dr. Suzanne Tobey, (Chemistry Department), Dr. Mark<br />

Welker, (Chemistry Department), and various graduate students <strong>of</strong> the Chemistry Department


I. INTRODUCTION ..................................................................................................................................... 5<br />

II. TELEPHONE #S OF EMERGENCY PERSONNEL / EMERGENCY FACILITIES ...................... 7<br />

A. HAZARDOUS CHEMICALS EMERGENCY AND INFORMATION PHONE #S ........................................................ 8<br />

B. EMERGENCY EXIT PLAN FOR ALL SALEM HALL LABORATORIES ................................................................ 9<br />

III. THE CHEMICAL HYGIENE PLAN FOR EACH LABORATORY IN SALEM HALL ............. 10<br />

A. EMERGENCY TELEPHONE NUMBERS OF LAB SUPERVISORS AND LAB WORKERS ...................................... 11<br />

1. Dr. Alexander – Lab Room #108B ..................................................................................................... 12<br />

2. Dr. Bierbach – Lab Room #107 ......................................................................................................... 13<br />

3. Dr. Brown – Lab Room # 114 ............................................................................................................ 14<br />

4. Dr. Buchmueller – Lab Room #1 ........................................................................................................ 15<br />

5. Dr. Colyer – Lab Room #114 ............................................................................................................. 16<br />

6. Dr. Hinze – Lab Room #109 ............................................................................................................... 17<br />

7. Dr. Brad Jones – Lab Room #118 ...................................................................................................... 18<br />

8. Dr. Paul Jones – Lab Room #113 ...................................................................................................... 19<br />

9. Dr. Bruce King – Lab Room #17 and 18 ............................................................................................ 20<br />

10. Dr. Kondepudi – Lab Room #5 ........................................................................................................ 21<br />

11. Dr. Lachgar – Lab Room #6 .............................................................................................................. 22<br />

12. Dr. N<strong>of</strong>tle – Lab Room #117 .............................................................................................................. 23<br />

13. Dr. Sw<strong>of</strong><strong>for</strong>d – Lab Room #7 .............................................................................................................. 24<br />

14. Dr. Tobey – Room # 2 ........................................................................................................................ 25<br />

15. Dr. Welker – Lab Room #s 13 and 18 ................................................................................................ 26<br />

16. Undergraduate – Lab Room #s 7, 101, 102, 103, 104, 105, 106 and 111 ......................................... 27<br />

B. GENERAL SAFETY PROCEDURES ............................................................................................................... 28<br />

1. BASIC SAFETY RULES FOR ALL UNDERGRADUATE LABORATORIES ....................................... 28<br />

2. Cleanliness in the Research Laboratory ............................................................................................... 31<br />

3. Housekeeping <strong>for</strong> All Labs ................................................................................................................... 33<br />

4. Eyewash Fountains and Safety Showers .............................................................................................. 34<br />

5. Lab Fires and <strong>Use</strong> <strong>of</strong> Fire Extinguishers ............................................................................................. 36<br />

C. PROCEDURES FOR HANDLING HAZARDOUS CHEMICAL WASTE ................................................................. 38<br />

D. PROTECTIVE DEVICES, EQUIPMENT, AND APPAREL .................................................................................. 50<br />

1. Personal Protective Equipment: Eyewear ........................................................................................... 50<br />

2. Personal Protective Equipment: Lab Coats and Gloves ..................................................................... 51<br />

3. VENTILATION AND PROPER USE OF HOODS ............................................................................... 53<br />

4. Chemical Storage in Research Labs ..................................................................................................... 61<br />

E. LABORATORY OPERATIONS WHICH REQUIRE PRIOR APPROVAL FROM CHEMISTRY DEPARTMENT<br />

INSTRUCTORS ................................................................................................................................................. 63<br />

F. PROVISIONS FOR ADDITIONAL PROTECTION WHEN WORKING WITH PARTICULARLY HAZARDOUS<br />

CHEMICALS .................................................................................................................................................... 65<br />

2. INIMICAL CHEMICALS: RULES OF ENGAGEMENT ..................................................................... 66<br />

G. SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE ................................................... 67<br />

1. Dr. Alexander – Lab Room #108 ........................................................................................................ 68<br />

2. Dr. Bierbach – Lab Room #107 ......................................................................................................... 69<br />

3. Dr. Brown – Lab Room #14 ............................................................................................................... 71<br />

4. Dr. Buchmueller – Lab Room #1 ........................................................................................................ 74<br />

5. Dr. Colyer – Lab Room # 114 ............................................................................................................ 75<br />

6. Dr. Hinze – Lab Room # 109 .............................................................................................................. 77<br />

7. Dr. Brad Jones – Lab Room # 118 ..................................................................................................... 78<br />

8. Dr. Paul Jones – Lab Room # 14 ....................................................................................................... 79<br />

9. Dr. Bruce King – Lab Room # 17 ....................................................................................................... 80<br />

10. Dr. Kondepudi – Lab Room # 5 ....................................................................................................... 81<br />

ii


11. Dr. Lachgar – Lab Room # 6 ............................................................................................................. 82<br />

12. Dr. N<strong>of</strong>tle – Lab Room # 118 ............................................................................................................. 84<br />

13. Dr. Sw<strong>of</strong><strong>for</strong>d – Lab Room # 1 ............................................................................................................. 85<br />

14. Dr. Tobey – Lab Room # 2 ................................................................................................................. 86<br />

15. Dr. Welker – Lab Room # 13 .............................................................................................................. 89<br />

16. Undergraduate – Lab Rooms # 7, 101, 102, 103, 104, 105, 106, 111 ............................................... 90<br />

H. SPECIFIC DECONTAMINATION PROCEDURES FOR EQUIPMENT AND BENCH TOP SURFACES WHICH HAVE<br />

COME INTO CONTACT WITH HIGHLY TOXIC WASTE ........................................................................................ 91<br />

1. Dr. Alexander – Lab Room # 108 ....................................................................................................... 94<br />

2. Dr. Bierbach – Lab Room # 107 ........................................................................................................ 95<br />

3. Dr. Brown – Lab Room # 14 .............................................................................................................. 96<br />

4. Dr. Buchmueller – Lab Room # 1 ....................................................................................................... 97<br />

5. Dr. Colyer – Lab Room # 114 ............................................................................................................ 98<br />

6. Dr. Hinze – Lab Room # 109 .............................................................................................................. 99<br />

7. Dr. Brad Jones – Lab Room # 118 ................................................................................................... 100<br />

8. Dr. Paul Jones – Lab Room # 14 ..................................................................................................... 101<br />

9. Dr. Bruce King – Lab Room # 17 ..................................................................................................... 102<br />

10. Dr. Kondepudi – Lab Room # 5 ..................................................................................................... 103<br />

11. Dr. Lachgar – Lab Room # 6 ........................................................................................................... 104<br />

12. Dr. N<strong>of</strong>tle – Lab Room # 117 ........................................................................................................... 105<br />

13. Dr. Sw<strong>of</strong><strong>for</strong>d – Lab Room # 1 ........................................................................................................... 106<br />

14. Dr. Tobey – Lab Room # 2 ............................................................................................................... 107<br />

15. Dr. Welker – Lab Room # 13 and 18 ................................................................................................ 108<br />

16. Undergraduate Lab Rooms # 7, 101, 102, 103, 104, 105, 106, 111 ................................................ 109<br />

I. LABORATORY AND FUME HOOD INSPECTIONS ......................................................................................... 110<br />

1. Laboratory Inspection Form .............................................................................................................. 111<br />

J. LABORATORY EMERGENCIES .................................................................................................................... 112<br />

1. Emergency Procedure and First Aid Overview ................................................................................... 112<br />

2. Chemical Fire and Large Building Fire Emergency Procedures: ..................................................... 113<br />

3. Chemical Spills ................................................................................................................................... 114<br />

K. PROVISIONS FOR MEDICAL EXAMS, CONSULTATION & EXPOSURE ASSESSMENTS ..................................... 117<br />

1. A Guide to OSHA Air Concentration Acronyms ................................................................................. 117<br />

2. Air Monitoring .................................................................................................................................... 118<br />

3. Medical Monitoring ............................................................................................................................ 119<br />

4. In<strong>for</strong>mation Regarding Student First Aid and Medical Insurance ..................................................... 120<br />

5. Worker’s Compensation Procedures and Reporting In<strong>for</strong>mation ...................................................... 121<br />

6. Accident and Chemical Exposure Assessment Report ........................................................................ 122<br />

L. STANDARD OPERATING PROCEDURES (SOPS) FOR WORKING WITH HAZARDOUS CHEMICALS................. 123<br />

1. Sources <strong>of</strong> Chemical Risk Assessment In<strong>for</strong>mation <strong>for</strong> SOPs ............................................................. 123<br />

2. Summary <strong>of</strong> Regulated Chemicals Covered by this CHP ................................................................... 125<br />

3. An Introduction to Standard Operating Procedure (SOPs) ............................................................... 126<br />

4. SOPs <strong>for</strong> all laboratories <strong>of</strong> Salem Hall ............................................................................................. 127<br />

5. Laboratory Specific SOPs .................................................................................................................. 140<br />

IV. TRAINING .......................................................................................................................................... 149<br />

A. INTRODUCTION TO TRAINING .................................................................................................................. 150<br />

B. CHEMICAL HYGIENE PLAN (CHP) FOR FRESHMAN CHEMISTRY LABS .................................................... 151<br />

1. Additional Safety In<strong>for</strong>mation, Chemistry Lab 108L and 111L.......................................................... 152<br />

2. HMIS / NFPA Chemical Hazard Ratings on Departmental MSDS Sheets ......................................... 153<br />

3. HMIS and MSDS Clarifications ......................................................................................................... 154<br />

4. INTERPRETING CHEMICAL HAZARD HMIS RATINGS ................................................................ 155<br />

5. SOME HMIS RATINGS FOR COMMON CHEMICALS .................................................................... 156<br />

6. Summary <strong>of</strong> HMIS Ratings ................................................................................................................. 157<br />

7. Hazard Communication Training Log Form ....................................................................................... 159<br />

C. CHEMICAL HYGIENE PLAN (CHP) FOR ORGANIC CHEMISTRY LABS ....................................................... 160<br />

1. Health Hazards <strong>of</strong> Some Common Chemicals .................................................................................... 164<br />

iii


D. TRAINING FOR GRADUATE STUDENTS, POST-DOCTORATES, AND RESEARCH UNDERGRADUATES .......... 168<br />

1. Certification <strong>of</strong> Safety Training Form <strong>for</strong> Graduate Students, Post-Graduates, and Summer School<br />

Undergraduate Research Students .......................................................................................................... 169<br />

2. Yearly Announcement <strong>of</strong> Gas Cylinder Safety and New Graduate Student Safety Review ................ 170<br />

3. Summer School Safety Training Announcement <strong>for</strong> Research Undergrads: ...................................... 171<br />

4. New Graduate Student and new Undergraduate Research Student Safety Orientation Announcement,<br />

in August <strong>of</strong> each year: ............................................................................................................................ 172<br />

V. CHEMISTRY DEPARTMENT PURCHASE ORDER REQUEST SYSTEM .............................. 173<br />

VI. PURCHASING PROCEDURE FOR DEA CONTROLLED SUBSTANCES ............................... 182<br />

VII. ALCOHOL DISPENSING PROCEDURE..................................................................................... 183<br />

VIII. OSHA/EPA INSPECTION PROCEDURE FOR SALEM HALL ............................................... 183<br />

IX. CHEMICAL INVENTORIES ............................................................................................................ 184<br />

A. INVENTORY OF ALL CHEMICALS AND MSDS SHEETS IN THE CHEMISTRY DEPARTMENT ........................ 184<br />

B. INSTRUCTIONS FOR THE USE OF THE ONLINE INVENTORY SYSTEM ......................................................... 185<br />

C. GENERAL INFORMATION FOR USERS ....................................................................................................... 187<br />

D. INDIVIDUAL CHEMICAL INVENTORIES OF THE CHEMISTRY DEPARTMENT, SALEM HALL: ....................... 188<br />

iv


I. INTRODUCTION<br />

A hardcopy <strong>of</strong> this Chemical Hygiene Plan and Safety Manual will be kept in the Chemistry<br />

Department Stockroom, Room 110, near the MSDS sheet collection, <strong>for</strong> your reference. Individual lab<br />

copies <strong>of</strong> the National Research Council’s Prudent Practices in the Laboratory, 2nd edition. Washington,<br />

D.C.: National Academy Press, 1995, hereinafter referred to as Prudent Practices, 2nd edition, will be<br />

kept in each research Lab as well as the stockroom. View the online Chemical Hygiene Plan and Safety<br />

Manual from the University Web site at http://www.wfu.edu/chem/cheminventory/index.html ,<br />

Throughout this manual, you will find specific references to suggested reading <strong>of</strong> certain sections<br />

<strong>of</strong> Prudent Practices, 2nd edition (indicated in boldface type throughout).<br />

You are REQUIRED to read OSHA’s “Laboratory Standard”, a copy <strong>of</strong> which is located in<br />

Appendix A on pages 219-225 <strong>of</strong> that monograph (or at the internet site http://www.oshaslc.gov/OshStd_data/1910_1450.html).<br />

This is a reprint <strong>of</strong> the most recent governmental regulation<br />

governing all chemical laboratories under US jurisdiction. Upon graduation and exposure to any workplace<br />

laboratory in the country you will soon discover that companies and institutions will appreciate spending<br />

less time training new employees in their particular CHP as a direct result <strong>of</strong> your having read and<br />

understood the present one.<br />

This document was prepared in a Workbook <strong>for</strong>mat, with the help and assistance <strong>of</strong> students, staff,<br />

and Faculty personnel within the Chemistry and Physics departments. All sections in black type in this<br />

manual are meant to be read by all Lab workers in this building. All sections in red type are presented only<br />

as an elaboration <strong>of</strong> the Laws presently governing Laboratory work involving the use <strong>of</strong> chemicals. They<br />

need not be read by anyone other than WFU Safety staff members involved with interpreting OSHA Laws<br />

and as guidelines <strong>for</strong> interested Faculty members and students. For example, it is not necessary to read the<br />

chapter titled “Emergency Telephone numbers <strong>of</strong> Lab Supervisors and Lab Workers”. Likewise, the<br />

chapter titled “Summary <strong>of</strong> Regulated Chemicals Covered by this SOP (Standard Operating Procedure)” is<br />

meant only <strong>for</strong> WFU Safety Personnel and interested Faculty members wishing to review what the Law<br />

stipulates in a particular situation<br />

Also, it is not necessarily important to read all SOPs in the chapter titled “Laboratory Specific<br />

SOPs (Standard Operating Procedures)”. Please read only the SOPs (Standard Operating Procedures)<br />

which apply to your particular Research Laboratory.<br />

The following Safety Record-keeping <strong>for</strong>ms will be filled out and recorded by the Chemistry<br />

Department’s Laboratory Manager, Chemistry Department Faculty members, Graduate Students, qualified<br />

Undergraduate stockroom personnel, Physical Facilities personnel, or Mr. Scott Frazier [WFU Assistant<br />

Environmental Health and Safety (EHS) Director] (phone #758-4329, or 758-4224) or Michelle Adkins,<br />

CHMM, Wake Forest University Director <strong>of</strong> Environmental Health and Safety: adkinsmm@wfu.edu,<br />

phone: 336-758-5385, cell: 336-480-8480, fax: 336-758-3088).<br />

The particular Safety Record-Keeping Forms and their storage locations in the Chemistry<br />

Department or elsewhere are listed below. Generally, the <strong>for</strong>ms will be kept in the Chemistry Stockroom,<br />

room #110, in the top two file drawers <strong>of</strong> the tan colored OSHA file storage cabinet, next to the side-room<br />

#110D. If any particular <strong>for</strong>m is kept elsewhere in the building or with the WFU Environmental Health and<br />

Safety Department, its location will be listed below.<br />

Spare Keys to the Chemistry Department‟s OSHA drawer are kept with the WFU Environmental<br />

Health and Safety Department, c/o Mr. Scott Frazier or Ms. Michelle Adkins.<br />

� Eyewash Fountain and Safety Shower Inspections, Physical Facilities, c/o Scott Frazier<br />

� Fume Hood Air-Flow Inspections, Physical Facilities, c/o Scott Frazier<br />

� Filled out Accident and Chemical Exposure Assessment Report <strong>for</strong>ms, OSHA drawer, Chemistry<br />

Department Stockroom # 110<br />

� Sophomore Chemistry Lab 221L Safety Quizzes, OSHA drawer, Chemistry Department<br />

Stockroom # 110<br />

5


� Freshman Chemistry Lab Safety Agreement Forms, room #8A, wooden storage cabinets in back <strong>of</strong><br />

room<br />

� WFU Hazard Communication Training Log – signature <strong>for</strong>ms, OSHA drawer, Chemistry<br />

Department Stockroom # 110<br />

� Signed “Basic Safety Rules For All Undergraduate Labs” Forms, room #8A, wooden storage<br />

cabinets in back <strong>of</strong> room<br />

� Signed “Certification <strong>of</strong> Safety Training <strong>for</strong> Graduate Students” Forms, OSHA drawer, Chemistry<br />

Department Stockroom # 110<br />

� Alcohol <strong>Use</strong> Logbooks, over the 200 pro<strong>of</strong> alcohol containers, locked <strong>Solvent</strong> room # 20, Loading<br />

Dock area<br />

� Yearly Bureau <strong>of</strong> Alcohol, Tobacco, and Firearms “Special Tax Stamp” receipt <strong>for</strong> Chemistry<br />

Department (and rest <strong>of</strong> Reynolda Campus), locked <strong>Solvent</strong> room # 20, Loading Dock area, near<br />

the 5 gallon size containers 190 Pro<strong>of</strong> alcohol<br />

� Filled Out “Weekly Hazardous Waste Storage Area Inspection” Forms, in locked <strong>Solvent</strong> Room #<br />

20, Loading Dock area, near the 55 gallon Hazardous Waste <strong>Solvent</strong> drums<br />

� Logbook <strong>for</strong> 55-Gallon <strong>Solvent</strong> Hazardous Waste Drum in locked <strong>Solvent</strong> Room #20, Loading<br />

dock area, on top <strong>of</strong> the spare 55 gallon waste solvent drum<br />

� All WFU Chemical Waste records, including copies <strong>of</strong> manifests and records having to do with<br />

chemical waste companies, c/o Scott Frazier [WFU Assistant Environmental Health and<br />

Safety (EHS) Director], campus phone number 758-4329, cell phone # 336-782-6107, and<br />

Copies <strong>of</strong> the Waste Company‟s Packing Slip listing <strong>of</strong> all waste chemicals collected from the<br />

Chemistry Department are kept by the Chemistry Department laboratory manager in the top drawer<br />

<strong>of</strong> the OSHA file cabinet, Chemistry Department Stockroom # 110<br />

� All original WFU Chemical Waste records, including Hazardous Chemical Waste Manifests and<br />

records having to do with chemical waste companies, at the WFI , c/o Scott Frazier [WFU<br />

Assistant Environmental Health and Safety (EHS) Director], campus phone number 758-<br />

4329, cell phone # 336-782-6107. The Chemistry Department Lab Manager keeps copies <strong>of</strong> the<br />

Chemistry Department‟s Hazardous Chemical Waste Manifests as well as original typed lists <strong>of</strong> the<br />

actual specific names <strong>of</strong> all the Chemistry Department‟s waste chemicals <strong>for</strong> RECRA (Resource<br />

Conservation and Recovery Act) records<br />

6


II. Telephone #s <strong>of</strong> Emergency Personnel / Emergency Facilities<br />

THE DEPARTMENTAL EMERGENCY TELEPHONE IS LOCATED IN THE<br />

STOCK ROOM #110, PHONE # 758-4712.<br />

THE DEPARTMENTAL FAX # FOR THE FAX MACHINE LOCATED IN THE<br />

MAIN OFFICE, ROOM #110B, IS 336-758-4656.<br />

THIS NOTICE IS ALSO POSTED ON THE WALLS NEXT TO EACH INDIVIDUAL<br />

RESEARCH LABORATORY TELEPHONE IN SALEM HALL<br />

WFU ASSISTANT ENVIRONMENTAL HEALTH AND SAFETY DIRECTOR<br />

NAME: Scott A. Frazier<br />

OFFICE TELEPHONE: 758-4329 (or 4224)<br />

HOME TELEPHONE: 945-9184<br />

PAGER: 607-8945<br />

CELLULAR PHONE 782-6107<br />

SAFETY DIRECTOR AND CHEMICAL HYGIENE OFFICER FOR SALEM HALL<br />

NAME: Michael A. Thompson<br />

TITLE: Laboratory Manager, Chemistry Dept.<br />

OFFICE TELEPHONE: 758-5324 (5325)<br />

HOME TELEPHONE 306-5209<br />

EMERGENCY TELEPHONE NUMBERS<br />

Located on Campus<br />

University Police Department: 5911 (Non Emergency 5591)<br />

Student Health Services: 5218<br />

DIAL 911 FOR ALL EMERGENCIES INVOLVING REQUESTS<br />

FOR CITY FIRE, POLICE, OR AMBULANCE ASSISTANCE<br />

Your emergency call to 5911 will be coordinated by the Wake Forest University<br />

Police Department. They will determine whether the situation can be handled by<br />

University Emergency personnel or City/County Emergency agencies.<br />

Call Student Health Services (at 5218) <strong>for</strong> minor medical problems<br />

In Charlotte, Carolinas Medical Center<br />

Carolinas Poison Control Center: 1-800-848-6946<br />

7


A. Hazardous Chemicals Emergency and In<strong>for</strong>mation Phone #s<br />

Local Emergency Contacts Phone #<br />

WFU SAFETY RESPONSE TEAM (For Chemical Spills) 758-4329 (or 4224)<br />

C/O Scott Frazier [WFU Assistant Environmental Health and Safety (EHS) Director],<br />

Physical Facilities, Reynolda Campus<br />

Mr. Mel Sadler, or August M. Vernon (For Chemical Spill Reporting) 767-6161<br />

Winston-Salem/Forsyth County<br />

OFFICE OF EMERGENCY MANAGEMENT<br />

Room 104-Smith Reynolds Airport<br />

Winston-Salem, NC 27105<br />

Fire Captains Harvey Wagner and D.W. Mabe 727-2454<br />

#8 Fire Station<br />

2417 Reynolda Road<br />

Winston-Salem, NC 27109<br />

Chief Bernard Smith, Fire Marshall 773-7972<br />

Winston-Salem Fire Department<br />

725 N. Cherry Street<br />

Winston-Salem, NC 27102<br />

Mr. Reed Jarvis, Deputy Fire Marshall 727-8084<br />

Forsyth County Fire Department<br />

3000 Aviation Drive<br />

Winston-Salem, NC 27105<br />

STATE EMERGENCY MANAGEMENT OFFICE (919) 733-3867 or<br />

(For Chemical Spill Reporting) 1-800-858-0368<br />

Rich Berman 1-919-733-3825 (or 1361)<br />

NC Division <strong>of</strong> Emergency Management<br />

4713 Mail Service Center<br />

Raleigh, NC 27699-4713<br />

8


B. Emergency Exit Plan <strong>for</strong> All Salem Hall Laboratories<br />

In all cases which require evacuation <strong>of</strong> the building, be prepared to tell emergency personnel what<br />

chemical hazards exist in your lab. The fire department will be especially interested your descriptions <strong>of</strong><br />

what to expect when attempting to put out fires in your lab room (See chapters titled “Lab Fires and <strong>Use</strong> <strong>of</strong><br />

Fire extinguishers” and “Chemical Fire and Large Building Fire Emergency Procedures”).<br />

The Chemistry department will conduct periodic fire drills. Note the location <strong>of</strong> your nearest<br />

hallway Emergency Exit Plan Maps, located in the central hallway <strong>of</strong> each floor <strong>of</strong> the building. Go<br />

though the nearest building door exit and try to account <strong>for</strong> all members <strong>of</strong> your research group or teaching<br />

lab. In any case, WFU security requires immediate exit <strong>of</strong> all building personnel after an alarm has<br />

sounded.<br />

The gathering place <strong>for</strong> all Salem Hall personnel after a building evacuation through the nearest<br />

building exit is the lawn between Salem Hall and the main library to the east. The fire code requires each<br />

working lab to have two ways out in case <strong>of</strong> a fire. Know where both are when you begin routinely working<br />

in any lab.<br />

Do not return to the building until the alarm ends and you are allowed to do so by Scott<br />

Frazier [WFU Assistant Environmental Health and Safety (EHS) Director] or Michelle Adkins<br />

(WFU Director <strong>of</strong> Environmental Health and Safety), or Sissy Hastings (Wake Forest University<br />

EHS Coordinator) or the Fire Marshall, or WFU Security.<br />

(Here is more specific contact in<strong>for</strong>mation <strong>for</strong> Michelle Adkins, CHMM, Director <strong>of</strong> Environmental<br />

Health and Safety: adkinsmm@wfu.edu, phone: 336-758-5385, cell: 336-480-8480, fax: 336-758-<br />

3088).<br />

9


III. The Chemical Hygiene Plan <strong>for</strong> Each Laboratory in Salem Hall<br />

10


A. Emergency Telephone Numbers <strong>of</strong> Lab Supervisors and Lab Workers<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number Salem Hall, Reynolda Campus<br />

Laboratory phone # (or nearest building phone #)<br />

Laboratory Instructor Office Phone<br />

Office Room # Home Phone<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

11


1. Dr. Alexander – Lab Room #108B<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 108 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-5576<br />

Laboratory Instructor Dr. Rebecca Alexander Office Phone 758-5568<br />

Office Room # 108A Home Phone 723-3532<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Michael E. Budiman 703-0283<br />

Susan A. Walker 704-639-0927<br />

Lela Lackey<br />

Pam Edwards<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

Research includes mechanistic investigation <strong>of</strong> enzymes involved in the protein<br />

biosynthesis pathway. Operations include growth <strong>of</strong> bacterial strains (non-pathogenic E.<br />

coli) <strong>for</strong> purification <strong>of</strong> proteins and nucleic acids. Radioactive materials are used in<br />

minute quantities <strong>for</strong> trace labeling and kinetic assays. Our license covers use <strong>of</strong> 32 P,<br />

35 S, and 3 H radionuclides. 32 P is a high energy beta emitter whose decay particles are<br />

stopped by 0.25 inches <strong>of</strong> plexiglass. 35 S and 3 H are low energy beta emitters whose<br />

decay particles are stopped by paper or clothing. Our stock vials (containing less than 1<br />

mL each) are stored in locked, shielded containers in the lab refridgerator and freezer.<br />

Small quantities <strong>of</strong> flammable solvents (methanol, ethanol, acetone, acetonitrile) are<br />

stored in the flammable solvents cabinet (under the hood) or in the refridgerator (rated <strong>for</strong><br />

flammables).<br />

12


2. Dr. Bierbach – Lab Room #107<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 107 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-3386<br />

Laboratory Instructor Dr. Ulrich Bierbach Office Phone 758-3507<br />

Office Room # 3B Home Phone 794-0451<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Hemanta Baruah 794-0051<br />

Jennifer Butler 766-0682<br />

Colin Barry 759-3582<br />

Meg Ackley 703-0812<br />

Eric Routh 758-8144<br />

Todd Augustus 758-1434<br />

Ernie Murray 758-6236<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

Research includes investigation <strong>of</strong> metal-containing anti-tumor drugs and their<br />

mechanism <strong>of</strong> DNA interaction. Operations include inorganic and organic synthesis and<br />

routine purification procedures. Hazards arise from solvents used to synthesize starting<br />

materials. Most hazards in this laboratory involve common flammable organic solvents<br />

and several compressed gas cylinders, including lecture bottles <strong>of</strong> amines and carbon<br />

monoxide. The poison cabinet contains biohazardous sulfur compounds.<br />

13


3. Dr. Brown – Lab Room # 114<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 114 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-5097<br />

Laboratory Instructor Dr. Bernard A Brown Office Phone 758-5514<br />

Office Room # 16A Home Phone 924-5014<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Heather Angell 993-0869<br />

Blythe Ashcraft 661-2769<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

This is a biochemistry research laboratory containing a few hazardous chemicals,<br />

concentrated acids, non- pathogenic BL1-level organisms (E. coli, yeasts), and<br />

compressed liquid nitrogen gas-cylinders. All chemical solutions are labeled and are<br />

stored with similar chemical classes around the laboratory. Flammable organic solvents<br />

(methanol, ethanol, isopropanol, acetone) are stored in the cabinet below the fume hood<br />

in the right rear <strong>of</strong> the lab (Room 14). Several small bottles <strong>of</strong> toxic heavy-metalcontaining<br />

chemicals (e.g.,: mercury, gold, platinum, lead) are stored in the chemical<br />

cabinet in the left rear <strong>of</strong> the lab (Room 14). There are no water-reactive chemicals<br />

stored in this laboratory. Fire extinguishers are located in the left-front, and right-rear<br />

<strong>of</strong> Room 14, and at the immediate left <strong>of</strong> the door-way leading from Room 14 to 16.<br />

14


4. Dr. Buchmueller – Lab Room #1<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 1 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-5196<br />

Laboratory Instructor Dr. Karen Buchmueller Office Phone 758-3144<br />

Office Room # 3A Home Phone 765-4139<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Meredith Parkinson<br />

Kavita Bhatt<br />

Lawrena Ngo<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

Research involves the study <strong>of</strong> DNA structure and function. Operations include<br />

growth <strong>of</strong> bacterial strains (non-pathogenic E. coli) <strong>for</strong> purification <strong>of</strong> proteins and<br />

nucleic acids. Radioactive materials are used in minute quantities <strong>for</strong> trace labeling and<br />

binding assays. Our license covers use <strong>of</strong> 32 P and 35 S. 32 P is a high energy beta emitter<br />

whose decay particles are stopped by 0.25 inches <strong>of</strong> plexiglass. 35 S is a low energy beta<br />

emitter whose decay particles are stopped by paper or clothing. Our stock vials<br />

(containing less than 1 mL each) are stored in shielded containers in a locked lab<br />

refridgerator/freezer.<br />

Small quantities <strong>of</strong> flammable solvents (methanol, ethanol, acetone, acetonitrile) are<br />

stored in the flammable solvents cabinet (under the hood) or in the refridgerator (rated <strong>for</strong><br />

flammables).<br />

15


5. Dr. Colyer – Lab Room #114<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 114 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-6162<br />

Laboratory Instructor Dr. Christa L. Colyer Office Phone 758-4936<br />

Office Room # Salem Hall – 116B Home Phone 760-2494<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Beverly Paul 352-262-0693<br />

Pera Viskari 896-0606<br />

Frank Welder 724-6434<br />

Amy Sloat 724-0793<br />

Tim Grambow 758-1649<br />

Hinda Boutrid 692-4591<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

Analytical chemical laboratory devoted to study <strong>of</strong> biochemicals (including amino<br />

acids, proteins, enzymes, organic compounds, etc.) mainly with use <strong>of</strong> capillary<br />

electrophoresis instrumentation. Few chemicals in this lab, although it does have a few<br />

full size gas cylinders <strong>of</strong> argon and nitrogen. Conceivable electrical hazards arising from<br />

several analytical instruments. Also, makes use <strong>of</strong> one small laser instrument.<br />

16


6. Dr. Hinze – Lab Room #109<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 107 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-4917<br />

Laboratory Instructor Dr. Willie Hinze Office Phone 758-5509<br />

Office Room # Salem Hall – 108A Home Phone 759-9856<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Amanda C Davis 919-426-5506<br />

Jennifer Rust 585-0666<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

Analytical chemical lab associated with chemical separations, such as liquid<br />

chromotography, extractions (liquid/liquid and cloud point), novel gel separations,<br />

including various surfactants. The lab contains a great many chemicals in rather small<br />

bottles, some <strong>of</strong> which are fairly toxic, and one or two compressed gas cylinders <strong>of</strong> inert<br />

gases (nitrogen and argon). Most chemicals are housed in one large wooden cabinet<br />

in the center section <strong>of</strong> the left wall, with some on wall shelves just as you enter the room.<br />

Volatile organic solvents are stored in metal cabinents under the hood, in back <strong>of</strong> room.<br />

17


7. Dr. Brad Jones – Lab Room #118<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 118 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-4937<br />

Laboratory Instructor Dr. Bradley T. Jones Office Phone 758-5512<br />

Office Room # Salem Hall – 116B Home Phone 785-2804<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Dan Hou 767-9662<br />

Heather Peters 985-3349<br />

Zheng Yang 577-6823<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

This laboratory‟s primary research involves the design and development <strong>of</strong><br />

instrumental methods <strong>for</strong> the determination <strong>of</strong> trace metals. As a result, the vast majority<br />

<strong>of</strong> chemicals found in the lab are dilute aqueous metal standards which pose no<br />

significant<br />

health risk. There are several compressed gas cylinders, most <strong>of</strong> which are located in one<br />

holding area in Room 118, on the right wall, midsection <strong>of</strong> room.. There are acetylene,<br />

dinitrogen oxide, argon, and 12% Hydrogen in balance <strong>of</strong> argon mixture gas cylinders.<br />

In room 117 (in back <strong>of</strong> labroom) there are three gas cylinders, one each <strong>of</strong> hydrogen,<br />

Oxygen, and helium.<br />

18


8. Dr. Paul Jones – Lab Room #113<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 14 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-5097<br />

Laboratory Instructor Dr. Paul Jones Office Phone 758-3708<br />

Office Room # 16-A Home Phone 758-1846<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

John Reynolds 924-9181<br />

Lara Voltz 759-3384<br />

Dan Zuidema 767-1055<br />

Rob Brinson 775-2663<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

This laboratory conducts research involving synthetic organic chemistry and the<br />

purification <strong>of</strong> organic molecules. Research involving biological systems also occurs.<br />

Hazards include toxic and caustic chemicals in all phases, electrical appliances, high<br />

intensity light sources (<strong>for</strong> use in photochemical experiments), and pressurized gas<br />

cylinders (argon, nitrogen, compressed air, and hydrogen). Against the rear wall, left <strong>of</strong><br />

the one window in the room are housed a number <strong>of</strong> pyrophoric and moisture sensitive<br />

chemicals. Avoid spraying water or aqueous solutions in this area. These chemicals<br />

include sodium and lithium metal, alkyl lithiums, and trialkylaluminums.<br />

19


9. Dr. Bruce King – Lab Room #17 and 18<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 17, 18 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-5728 (or 758-5097)<br />

Laboratory Instructor Dr. Bruce King Office Phone 758-5774<br />

Office Room # Salem Hall – 15B Home Phone 595-2954<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Jinming Huang 758-1836<br />

Bubing Zeng 794-1451<br />

Dennis Parrish 760-0561<br />

Zhou Zou 757-1114<br />

Shuana Heyward 765-6444<br />

Xin Sha 767-8699<br />

Mark Sperry 1139<br />

Richard Pennington<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

Synthetic organic chemistry laboratory with an emphasis on the preparation <strong>of</strong> new<br />

donors <strong>of</strong> nitric oxide (NO) or compounds capable <strong>of</strong> interaction with the enzyme nitric<br />

oxide synthase (NOS). <strong>Use</strong> <strong>of</strong> typical flammable laboratory solvents, mineral acids,<br />

solvent stills and compressed gas cylinders. Flammable solvents are stored in a nonflammable<br />

cabinet in the back <strong>of</strong> the laboratory. Water reactive materials are stored in<br />

the explosion pro<strong>of</strong> freezer in the back right <strong>of</strong> the laboratory and on the middle shelf in<br />

Room 15. Mineral acids are stored beneath hoods on the right side <strong>of</strong> lab. <strong>Solvent</strong> stills<br />

are located at the front left side <strong>of</strong> the lab. Compressed gases include argon and nitrogen<br />

and one (3 ft.) tank <strong>of</strong> ammonia located at the front left side <strong>of</strong> the lab. Lecture bottles <strong>of</strong><br />

nitric oxide gas are found in the front right side hood. Laboratory contains several<br />

vacuum pumps, rotary evaporators, an analytical balance and other analytical equipment<br />

including a gas chromtograph and high pressure liquid chromatograph (HPLC).<br />

20


10. Dr. Kondepudi – Lab Room #5<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 5 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-4826<br />

Laboratory Instructor Dr. Dilip Kondepudi Office Phone 758-5131<br />

Office Room # Salem Hall - 204 Home Phone 659-1085<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Kennith Crook 768-2608<br />

Natalee Sheppe 758-6464<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

Chemical laboratory currently devoted to various studies <strong>of</strong> chiral symmetry-<br />

breaking during recrystallization <strong>of</strong> chemical compounds, such as sodium chlorate. There<br />

are only limited amounts <strong>of</strong> toxic and flammable compounds present, such as cobalt salts<br />

and generally benign amino acids, and very few organic solvents.<br />

21


11. Dr. Lachgar – Lab Room #6<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 6 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-4533<br />

Laboratory Instructor Dr. Abdu Lachgar Office Phone 758-4676<br />

Office Room # 4A Home Phone 924-5883<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Zhihua Yan 661-3536<br />

Thirumacai Duraisamy 703-0285<br />

Yue Zhao 661-3536<br />

Huajun Zhou 926-9145<br />

Sana Ashraf 924-8217<br />

Yue Zhae 661-3536<br />

Bangbo Yan 924-0503<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

High temperature (150C – 1100C) syntheses using electrical furnaces. X-ray diffraction<br />

analysis using vacuum lines and inert gas systems to handle chemicals. Compressed gas<br />

cylinders are present, including argon, nitrogen, hydrogen, and oxygen. A hand torch<br />

<strong>for</strong> glass blowing, using both a hydrogen gas cylinder and benchtop natural gas, and<br />

an oxygen gas cylinder, is present in the back, right section <strong>of</strong> the room. Generally few<br />

chemicals (although a few toxic ones are present) with various types <strong>of</strong> ovens and heaters.<br />

A large glove box against the left wall contains mostly nontoxic chemicals, kept in there<br />

merely in order to be kept very dry.<br />

22


12. Dr. N<strong>of</strong>tle – Lab Room #117<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 117 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-4726<br />

Laboratory Instructor Dr. Ronald E. N<strong>of</strong>tle Office Phone 758-5520<br />

Office Room # 115B Home Phone 759-2441<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Jarrett Howell 724-7630<br />

Jeanette Sellers 922-5791<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

Synthetic organometallic, organ<strong>of</strong>luorine, and main group chemical lab, involving<br />

electrochemistry, toxic solvents, possibility <strong>of</strong> Hydrogen fluoride gas generated by<br />

hydrolysis <strong>of</strong> fluorine compounds, use <strong>of</strong> toxic gases, equipment under vacuum (glass),<br />

use <strong>of</strong> cryogenics (like liquid nitrogen and CO2, dry ice), electrochemical apparatus,<br />

danger <strong>of</strong> electrical shocks, and use <strong>of</strong> hazardous materials. Standard Operating<br />

Procedures dictated by general procedures listed in this manual.<br />

23


13. Dr. Sw<strong>of</strong><strong>for</strong>d – Lab Room #7<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 1 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-4542<br />

Laboratory Instructor Dr. Robert Sw<strong>of</strong><strong>for</strong>d Office Phone 758-4490<br />

Office Room # 209 Home Phone 766-0928<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

Laser laboratory devoted to the study <strong>of</strong> various properties <strong>of</strong> molecular structure.<br />

The main dangers present in this lab, which contains only a few chemical dyes and very<br />

Small amounts <strong>of</strong> various chemical samples, are due to eletrical shocks and possible eye<br />

Damage or skin burns from overexposure to lasers. The lab contains one or two normal<br />

Size compressed gas cylinders <strong>of</strong> nitrogen. Beware <strong>of</strong> walking into this lab while the<br />

Lasers are on.<br />

24


14. Dr. Tobey – Room # 2<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 2 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-4934<br />

Laboratory Instructor Dr. Suzanne Tobey Office Phone 758-5513<br />

Office Room # 4B Home Phone 922-3893<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

Research in this lab involves synthetic organic chemistry and the purification <strong>of</strong> organic molecules. The<br />

hazards include typical flammable laboratory solvents (ether, hexanes, tetrahydr<strong>of</strong>uran, benzene,<br />

dichloromethane) mineral acids, toxic and caustic chemicals in all phases, electrical appliances, and<br />

pressurized gas cylinders (argon, nitrogen). The flammable solvents are stored in cabinets under the hoods.<br />

The lab houses a solvent system located to the rear right wall intended <strong>for</strong> dispensing dry organic solvents.<br />

There are two vacuum pumps located in the lab under the hoods and the gas cylinders are secured in places<br />

using approved methods. Moisture and air sensitive chemicals (alkyl lithiums and Grignard reagents) are<br />

stored in the freezer located in the adjacent lab-room. Avoid spraying water towards the top shelf located<br />

above the benches as sodium and potassium metals will ignite. Hydrides (sodium hydride and lithium<br />

aluminum hydride) are located on the front bench so avoid use <strong>of</strong> water in this area. Base baths containing<br />

isopropanol and potassium hydroxide are stored in plastic containers under the hoods and can be casutic if<br />

spilled on the skin.<br />

25


15. Dr. Welker – Lab Room #s 13 and 18<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 13 and 18 Salem Hall, Reynolda Campus<br />

Laboratory phone #(or nearest building phone #) 758-5958 (or 5097)<br />

Laboratory Instructor Dr. Mark E. Welker Office Phone 758-5758<br />

Office Room # 15A Home Phone 778-1026<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Subbasis De 794-0051<br />

Kerry Pickin 922-9317<br />

Marion Franks 922-4677<br />

Brenden Quinn<br />

Anne Glenn 855-8767<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

This is an organic research laboratory containing mostly compressed gas<br />

cylinders,<br />

solvent stills, and various hazardous chemicals. It contains various organometallic<br />

compounds, some <strong>of</strong> which are moderately toxic and water reactive, but are present only<br />

in many small bottles. The gas cylinders tend to be mostly argon and nitrogen, and<br />

one each <strong>of</strong> carbon monoxide and air. Several smaller lecture bottles <strong>of</strong> fairly toxic gases<br />

are kept mostly in the left front hood as one enters the room, including HCl gas and<br />

ammonia.<br />

26


16. Undergraduate – Lab Room #s 7, 101, 102, 103, 104, 105, 106 and 111<br />

Lab Personnel Phone Numbers<br />

Laboratory Room Number 7,101,102,103,104,105,106,111 Salem Hall, Reynolda Campus<br />

Laboratory phone(or nearest building phone)758-4712, Chemistry Stockroom 110<br />

Laboratory Instructor Various Pr<strong>of</strong>essors Office Phone<br />

Students Assigned to this Laboratory, Name Home Phone Number<br />

including Graduate Students,<br />

Undergraduates and Post Doctorates<br />

Different Faculty members teach labs each semester, with rotating graduate students as<br />

Teaching Assistants.<br />

Brief Description <strong>of</strong> Research Conducted in This Lab<br />

INCLUDING POSSIBLE PROBLEMS FOR FIREFIGHTERS WITHIN:<br />

Room 111 generally contains 2 Nitrogen compressed gas cylinders, and one each<br />

<strong>of</strong> Nitrogen, Argon, Oxygen, and Helium compressed gas cylinders are kept in room 7.<br />

Generally nontoxic chemicals, with only a few flammable solvents (like acetone<br />

and ethanol) are used in 101 and 105. These freshman labs are seldom exposed to<br />

anything more harmful than the typical concentrated and dilute mineral acids in any lab,<br />

and more frquently make use <strong>of</strong> nontoxic dilute aqueous chemical solutions. Two<br />

nitrogen compressed gas cylinder are sometimes kept in back <strong>of</strong> room 103.<br />

The Organic undergraduate labs in rooms 102 and 106 make far more use <strong>of</strong><br />

mildly toxic to highly flammable organic solids and liquids, in reagent bottles on student<br />

benchtops. Room 7, the Physical Chem Lab, employs only small amounts <strong>of</strong> generally<br />

nontoxic compounds. The very toxic compounds are generally used in the Advanced<br />

Inorganic Lab in room 111, synthesizing heavy metal salts and organometallic complexes.<br />

27


B. General Safety Procedures<br />

1. BASIC SAFETY RULES FOR ALL UNDERGRADUATE LABORATORIES<br />

(prepared by Chemistry Department Faculty members)<br />

Read these safety regulations <strong>care</strong>fully, and be sure you understand them. Be<strong>for</strong>e each laboratory<br />

session, your instructor will discuss any safety hazards that might be associated with that day's experiment.<br />

1. Report all accidents to your instructor immediately. If you cut or burn yourself or accidentally<br />

inhale fumes, notify your instructor at once. The instructor will arrange immediate treatment.<br />

Learn the locations <strong>of</strong> the fire extinguishers, the safety showers, the fire blanket, eyewash, and<br />

phone, so that you can use them quickly in the case <strong>of</strong> an emergency. Your lab instructor will<br />

point out the emergency exits/routes out <strong>of</strong> Salem Hall in the case <strong>of</strong> an emergency.<br />

2. Wear safety goggles/glasses in the laboratory at all times. Always wear eye covering that will<br />

protect your eyes against both impact and splashes. (If you should get chemical in your eye, wash<br />

the eye with flowing water from the special eye-wash fountain <strong>for</strong> 15 to 20 minutes).<br />

3. Do not per<strong>for</strong>m any unauthorized experiments!<br />

4. Do not use mouth suction to fill pipettes with chemical reagents. (<strong>Use</strong> a suction bulb to fill<br />

pipettes).<br />

5. Exercise great <strong>care</strong> in noting the odor <strong>of</strong> fumes and avoid breathing fumes <strong>of</strong> any kind. Carry out<br />

experiments that produce noxious vapors in your fume hood. Arrange your apparatus setups so<br />

that the fume producing portion is inside the hood.<br />

6. Do not taste anything in the laboratory. (This applies to food as well as chemicals. Do not use the<br />

laboratory as an eating place; never eat or drink from laboratory glassware.)<br />

7. Confine long hair whenever you are in the laboratory.<br />

8. Place all hot glassware on a mat to cool; this will also signify to all laboratory personnel that the<br />

glassware is hot. Do not hand hot glassware to another person, because a person's natural instinct<br />

is to reach <strong>for</strong> it.<br />

9. Corrosive acids and bases are very soluble in water. If either a corrosive acid or base comes in<br />

contact with your skin, you can wash it <strong>of</strong> your skin be<strong>for</strong>e damage is done. Haste in washing the<br />

affected area is essential. Summon the laboratory instructor if you spill a corrosive acid or base<br />

on your skin. If strong acids are spilled on your skin, bathe the skin with dilute sodium<br />

bicarbonate after flooding with water <strong>for</strong> about 10 minutes. If strong bases are spilled on the skin,<br />

bathe the skin with a dilute solution <strong>of</strong> acetic acid or boric acid after flooding <strong>for</strong> about 10 minutes.<br />

If chemicals get into your eyes, immediately wash the eyes with a gentle stream <strong>of</strong> water from the<br />

eye wash <strong>for</strong> 15-20 minutes. Do not use dilute solutions <strong>of</strong> sodium bicarbonate, acetic acid, or<br />

boric acid in the eyes. After flushing with water, the student will be transported to the Student<br />

Health Service. If bromine or iodine is spilled on the skin, the skin should be immediately bathed<br />

with alcohol (ethanol) and then with glycerin.<br />

10. If you are preparing a dilute acid solution, never pour water into concentrated acid. Always pour<br />

the acid into the water while stirring the water constantly.<br />

28


11. Do not <strong>for</strong>ce glass tubing into rubber stoppers. Lubricate the tubing and introduce it gradually and<br />

gently. Protect your hands with a towel when you are inserting lubricated tubing into a stopper.<br />

Alternately, use the glass tube/stopper tool located in the stockroom In clamping glass tubing or<br />

glassware <strong>for</strong> apparatus setups, do not tighten the clamps any more than necessary to hold the glass<br />

in place (i.e. do not squeeze the glass).<br />

12. Do not wear open-toed shoes or shorts in the laboratory, since they do not <strong>of</strong>fer enough protection<br />

to the body.<br />

13. Never point a test tube containing a reacting mixture (especially when you are heating it) toward<br />

another person or toward yourself.<br />

14. Be extremely cautious when you are lighting a Bunsen Burner. Most laboratory fires can be<br />

smothered if handled at once. A cloth towel should be kept handy <strong>for</strong> this purpose. In the event <strong>of</strong><br />

a fire near your desk, immediately turn <strong>of</strong>f the gas cock that feeds your burner. If necessary, use<br />

the fire extinguisher (if your TA or instructor is nearby, let either one <strong>of</strong> them use the fire<br />

extinguisher).<br />

15. Never engage in horseplay in the laboratory.<br />

16. Read the label <strong>care</strong>fully be<strong>for</strong>e removing a chemical from its container.<br />

17. Never work in the laboratory alone.<br />

18. Do not wear contact lenses in any chemical laboratory, period.<br />

19. The areas where balances have been located are to remain clean. Anyone who spills any chemicals<br />

on the balance or on the table is responsible <strong>for</strong> the cleanup and the notification <strong>of</strong> the instructor.<br />

No weights are to remain on the balance and the balance doors are to be closed when you have<br />

finished.<br />

20. Everyone is responsible <strong>for</strong> keeping his/her own work area clean. All equipment is to be put away<br />

and the table top wiped clean. No trash is to be placed in the sinks.<br />

21. Many chemicals must be collected in proper containers <strong>for</strong> waste disposal. You will receive<br />

special instructions about disposing <strong>of</strong> any unusually dangerous chemicals. Otherwise, follow the<br />

instructions listed in your lab texts and manuals, or those given by your Teaching Assistant.<br />

22. Learn to estimate your chemical needs as closely as possible. Do not waste chemicals; other labs<br />

may need to use the same chemical.<br />

23. In using chemicals, be sure to replace all stoppers or droppers tightly; it is very hazardous to leave<br />

bottles open. Do not insert any medicine droppers into reagent bottles.<br />

24. The distilled water tap is located at the sink in the back <strong>of</strong> the lab. Be frugal in your use <strong>of</strong><br />

distilled water.<br />

25. Place all papers and match sticks in the waste crocks at your desk (not in the sink). Place all<br />

broken glass in the designated waste container in the back <strong>of</strong> the room.<br />

26. Never stop a centrifuge with your fingers.<br />

29


Please sign the <strong>for</strong>m below, tear this page <strong>of</strong>f and give it to the stockroom clerk upon check-in, and keep the<br />

previous two pages <strong>of</strong> safety rules <strong>for</strong> your reference throughout the semester.<br />

I, the undersigned, have read the Basic Safety Rules <strong>for</strong> All Laboratories, and I understand them.<br />

(Signature)<br />

(Date)<br />

WAKE FOREST UNIVERSITY<br />

CHEMISTRY DEPARTMENT<br />

30


2. Cleanliness in the Research Laboratory<br />

1. Clean up Research Lab benches occasionally. Wash your hands at the end <strong>of</strong> each lab session if you‟ve<br />

been working with chemicals at all. Check to make certain that any gloves you‟ve been wearing don‟t have<br />

pinhole leaks or tears. <strong>Use</strong> every means necessary to avoid ingesting chemicals in the lab or even touching<br />

them.<br />

2. If you must leave lab equipment, glassware, notebooks, etc., on the bench until the next day or work<br />

session, at least properly remove, store, and otherwise secure laboratory chemicals. Make a habit <strong>of</strong><br />

maintaining an orderly work bench area by removing unnecessary sheets <strong>of</strong> paper, soiled paper towels,<br />

broken glass, empty bottles, Pasteur pipets or anything else that doesn‟t belong there.<br />

3. Wear lab coats when working with chemicals if the possibility exits that you will contaminate your<br />

clothing. Outrageously Kaleidoscopic or unpleasantly odoriferous lab coats should be washed occasionally,<br />

although it probably isn‟t a good idea to mix them in with household laundry. Hang them up in your lab<br />

be<strong>for</strong>e lunch breaks in the graduate student lounge.<br />

4. It is <strong>for</strong>bidden to eat, drink or smoke in the lab or experimental work area. Such activities should occur<br />

outside the labs in designated areas. All research labs in Salem Hall have entranceway student desk areas,<br />

separated from the actual labs by walls. You may eat and drink there. However, it is preferable to make<br />

use <strong>of</strong> the graduate student lounge in room #112B. Even chewing gum in the lab should be avoided.<br />

5. Do not use laboratory refrigerators which contain any lab chemical whatsoever as repositories <strong>for</strong> food.<br />

Do not use ice from the undergraduate ice machine in room # 104 <strong>for</strong> any purpose other than experimental<br />

work. Since students tend to use laboratory containers, such as contaminated beakers, to scoop ice from<br />

this machine, you may end up with something unpleasant in your s<strong>of</strong>t drink!<br />

6. Laboratory glassware should be cleaned in laboratory sinks with soap and hot water. “Liqui-nox”<br />

(Fisher catalog # 04-322-158, gallon size) liquid soap concentrate and scouring soap powder, brand name<br />

“Sparkleen”(Fisher catalog # 04-320-4, 3lb. box), are located in the stockroom, room #110 if your research<br />

or teaching group has not purchased it already. Wear gloves while cleaning with properly chosen cleaning<br />

brushes. Check <strong>for</strong> tears and holes in the gloves. Don‟t allow dirty glassware to pile-up around sinks to an<br />

unmanageable level. This increases the likelihood <strong>of</strong> breakage and discourages the habit <strong>of</strong> examining each<br />

piece individually <strong>for</strong> degree <strong>of</strong> chemical contamination be<strong>for</strong>e washing. Rinse dirty glassware with labeled<br />

bottles <strong>of</strong> acetone if necessary. Highly contaminated, corrosive cleaning solutions, prepared from very<br />

acidic or alkaline chemicals, should in some cases be packaged in bottles when spent and taken to room<br />

#20, the solvent storage room, properly labeled <strong>for</strong> chemical waste company removal. In particular, spent<br />

chromerge (sulfuric acid and chromic acid combination cleaning solution) should be poured back into 2.5<br />

liter acid bottles and sent out with the waste company.<br />

7. The following cleaning solutions, as described in the Chemical Technician‟s Handbook (located in the<br />

stockroom, room # 110), can be used to clean glassware in research labs. Generally, undergraduate<br />

teaching labs will not require such strong cleaning solutions. Spent, highly acidic or alkaline cleaning<br />

solutions <strong>of</strong> common mineral acids or bases (e.g., nitric acid, sodium hydroxide, potassium hydroxide in<br />

ethanol, etc.) which have been used in research labs should be neutralized completely be<strong>for</strong>e disposal.<br />

Chromerge Cleaning Solutions: Obtain one 25ml bottle <strong>of</strong> chromerge from chemical storage room (room<br />

#19), composed <strong>of</strong> chromium trioxide, or chromic acid, and add contents directly to a standard 2.5 liter size<br />

bottle <strong>of</strong> concentrated sulfuric acid. Add approximately 5ml at a time, recap the acid bottle, and shake well.<br />

The precipitate which <strong>for</strong>ms after mixing is normal and indicates solution is saturated. Allow it to remain as<br />

it is a reservoir <strong>of</strong> additional chromate. The solution loses its effectiveness as it turns green with continued<br />

use.<br />

31


Concentrated solution <strong>of</strong> Dodycylbenzene sulphonic acid and potassium hydroxide(“Contrad-70”): This<br />

serves as a biodegradable, drain disposable alternative to chromerge. It is sold by Fisher Scientific Co.,<br />

Catalog # 04-3551. Prepare a 5% solution from the concentrate <strong>for</strong> lab use.<br />

“Dilute Nitric Acid Cleaning Solution: Films which adhere to the inside <strong>of</strong> flasks and<br />

bottles may <strong>of</strong>ten be removed by wetting the surface with dilute nitric acid, followed<br />

by multiple rinses with distilled water. Concentrated Nitric acid is good <strong>for</strong> tougher<br />

organic chemical stains.” <strong>Use</strong> in a hood only.<br />

“Aqua Regia Cleaning Solution: Aqua regia is made up <strong>of</strong> three parts <strong>of</strong> concentrated<br />

HCl and one part <strong>of</strong> concentrated HNO3. This is a very powerful, but extremely<br />

dangerous and corrosive, cleaning solution. <strong>Use</strong> in a hood with extreme <strong>care</strong>.”<br />

“Alcoholic Potassium Hydroxide or Sodium Hydroxide Cleaning Solution: Add<br />

about 1L ethanol (95%) to 120ml H20 containing 120g NaOH or 105g KOH. This is<br />

a very good cleaning solution. Avoid prolonged contact with ground-glass joints on<br />

interjoint glassware because the solution will etch glassware and damage will result.<br />

This solution is excellent <strong>for</strong> removing carbonaceous materials.”<br />

(Ballinger, Jack T. and Shugar, Gershon J. Chemical Technicians’ Ready Reference<br />

Handbook, 3rd edition. New York City: McGraw-Hill, Inc., 1990, pages 611-612).<br />

8. Broken Glassware Procedure: Waste containers stenciled with the label “Broken Glassware Only”<br />

have been placed in each laboratory. Broken glass should be placed in these containers, only, and only<br />

glass should be placed there. Glassware broken in the course <strong>of</strong> experimental work should be rinsed <strong>of</strong><br />

chemical contaminants, preferably with acetone, and the rinses deposited in lab chemical waste containers.<br />

Shards <strong>of</strong> broken glass found in common departmental waste containers are dangerous <strong>for</strong> housekeeping<br />

staff to handle. Glass should not there<strong>for</strong>e be mixed with paper and other common <strong>for</strong>ms <strong>of</strong> trash. Make<br />

sure that the top surface <strong>of</strong> broken glass within the Broken Glassware box does not overflow, resulting in<br />

dangerous situations <strong>for</strong> Housekeeping staff handling these boxes. It is requested that all research students<br />

and Teaching assistants within the undergraduate teaching labs occasionally check these boxes <strong>for</strong> overly<br />

jagged pieces <strong>of</strong> glass protruding through the side <strong>of</strong> the cardboard box or tearing up the plastic bag liner<br />

inside the box.<br />

9. Needles used <strong>for</strong> transferring chemical samples from one container to another or injection into<br />

instruments should be disposed <strong>of</strong> into red plastic containers marked “For Disposal <strong>of</strong> Non-reusable<br />

Needles, Only” placed in each research Lab requiring them. These containers will be collected when 80%<br />

full, stored in a large marked box in the <strong>Solvent</strong> Room # 20, and given to a biological Sharps (Needles, etc.)<br />

waste disposal company, such “Steri Cycle” Company, even though the Chemistry Department does not<br />

employ such needles in animal or human experiments. Replacement containers are located in room 20 or<br />

can be purchased from Fisher Scientific, catalog # 14-827-122 Needles which are meant to be reused<br />

should not be kept on counter tops without some provision to prevent accidental “sticking”. You can cap<br />

them, place them in holding packages or lab drawers, or request plastic holding containers from the<br />

department and gather them all into one holding container.<br />

Please do not overfill the Non-Reusable needle containers. Instead, leave 2 inches <strong>of</strong> "headspace"<br />

in each container at the top. Ins<strong>of</strong>ar as possible, do not place anything in these containers other than<br />

needles and the plastic sheathing associated with the needle. Large plastic and glass syringe tubes should be<br />

rinsed and disposed <strong>of</strong> in the garbage (glass syringe tubes go in with the broken glass boxes, <strong>of</strong> course). If<br />

you have the least bit <strong>of</strong> difficulty in removing smaller syringe tubes from the needle, then by all means<br />

drop the entire needle/tube assembly into the container <strong>for</strong> disposal.<br />

32


3. Housekeeping <strong>for</strong> All Labs<br />

Housekeeping services <strong>of</strong>fered by WFU Physical Facilities cannot automatically take <strong>care</strong> <strong>of</strong> all<br />

cleaning requirements encountered in fully functioning chemical labs, so be prepared to clean up such<br />

things as chemical spills on your own. Special requests <strong>for</strong> clean-up <strong>of</strong> non-routine nature should be<br />

called in at phone # 4255. Be cautious <strong>of</strong> such requests, however, if unattended housekeeping personnel<br />

must move unfamiliar lab equipment or disrupt normal lab activity while cleaning. Take steps to<br />

accommodate their time schedule and give them specific instructions. A COMMUNITY USE MOP AND<br />

BUCKET FOR CLEANING UP WATER SPILLS IS LOCATED IN CLOSET # J0, next to room 9E.<br />

In addition, observe the following general lab housekeeping rules:<br />

1. Chemical waste should be organized and kept in particular places in your lab, not scattered hither and<br />

yon.<br />

2. If your assigned bench-space work area generates chemical solvents which end up on the floor<br />

routinely, have your floor space cleaned and mopped more <strong>of</strong>ten. Consider getting a chemically<br />

resistant floor mat.<br />

3. If your work area is well <strong>care</strong>d <strong>for</strong> and your neighbor on an adjoining lab bench tends to be messy,<br />

don‟t allow bad habits <strong>of</strong> others to cramp your style. Report it to the lab manager, who will act as your<br />

subtle advocate.<br />

4. Both research students and teaching assistants should occasionally gather into communal clean-up<br />

teams and simply straighten up their research labs or assigned teaching labs. Chemistry stockroom<br />

personnel and the laboratory manager will help you.<br />

5. Don‟t allow overcrowded conditions to result in obstruction <strong>of</strong> safety equipment. Don‟t pile chemicals,<br />

tools, equipment, and towels randomly on lab bench tops or lab floors.<br />

6. Report overly dusty lab benches, dirty floors, leaves or cobwebs or dirt on windowsills to housekeeping<br />

personnel. Request housekeeping services whenever you see the need.<br />

7. Report damaged furniture to physical facilities <strong>for</strong> repair. Problems with plumbing, water fixtures or<br />

improper drainage should likewise be reported to maintenance.<br />

8. Teaching laboratory stockroom personnel housekeeping assignments are listed below. Chemistry<br />

stockroom personnel should be notified by TA‟s <strong>of</strong> anything which has not properly been completed<br />

be<strong>for</strong>e undergraduate teaching labs commence experimental activity.<br />

9. After lab check-out at the end <strong>of</strong> each semester, TA‟s should request that Housekeeping clean all<br />

undergraduate lab bench tops with the bottle <strong>of</strong> Servicemaster “Scrub „N‟ Shine” cleanser.<br />

Stockroom Personnel Housekeeping Assignments (Work/Study Undergrad employees):<br />

� Fill distilled water carboys.<br />

� Put paper towels at each third lab bench.<br />

� Fill metal acetone containers found under back sink with acetone from Rm. 20.<br />

� Make sure there is at least one bottle <strong>of</strong> Liqui-Nox soap concentrate in back <strong>of</strong> each lab, so that<br />

students can put ½ inch or so in their individual bench top soap bottles and dilute the rest <strong>of</strong> the<br />

container with water. Each lab only needs a dozen or so communal soap bottles.<br />

� Be sure to place gloves on stockroom counter: green gloves <strong>for</strong> General Chemistry labs and blue<br />

gloves <strong>for</strong> Organic Chemistry labs (only <strong>for</strong> experiments which require them).<br />

� Complete any other tasks <strong>for</strong> which the TA‟s may need assistance.<br />

33


4. Eyewash Fountains and Safety Showers<br />

Explicit instructions <strong>for</strong> using the eyewash fountains and safety showers located in Salem Hall are<br />

given in the safety film shown to all Chemistry Department freshmen during the first week <strong>of</strong> laboratory<br />

check-in. The film is entitled: “Starting with Safety.” Beginning graduate students serving as general<br />

chemistry lab teaching assistants will also be exposed to these instructions. TEACHING ASSISTANTS<br />

ARE FORMALLY REQUIRED TO SHOW ALL OF THEIR GENERAL CHEMISTRY LAB STUDENTS<br />

EXACTLY WHERE EMERGENCY EQUIPMENT IS LOCATED IN THEIR PARTICULAR ASSIGNED<br />

LABS. TA’s in all other undergraduate labs are expected to do the same.<br />

All eyewashes / safety showers in Salem Hall are located less than 75 feet from hazardous<br />

laboratory locations as required by the applicable standard cited by OSHA, referred to as ANSI Z358.1<br />

(American National Standards Institute). They are accessible from all work areas within undergraduate and<br />

graduate labs. Do not physically block access to these fountains with glassware, equipment, etc. Crowding<br />

equipment around infrequently used safety equipment will <strong>of</strong> course render them nonfunctional.<br />

Teaching assistants <strong>for</strong> undergraduate labs should activate the particular eyewash fountain or<br />

drench hose in their labs to demonstrate the flow <strong>of</strong> water available <strong>for</strong> chemical exposure to eyes. All<br />

research students should activate the eyewash fountain, drench hose, safety shower, and one or two fire<br />

extinguishers in their particular labs at least once to familiarize themselves with all safety equipment when<br />

beginning research during their first year <strong>of</strong> lab work.<br />

Contaminants in the eye frequently cause muscle contractions and an instinctive urge to close the<br />

eyelid making proper drenching difficult. It would not be unreasonable to practice trying to hold your<br />

eyelids open with your fingers while exposing your eyes to the discom<strong>for</strong>t <strong>of</strong> a good dousing. Eyewash<br />

fountains are constructed so as to remain flowing after they have initially been turned on. Ten or fifteen<br />

minutes <strong>of</strong> irrigation would not be unusual <strong>for</strong> a bad exposure. Drench hoses available in the newer<br />

undergraduate labs in Salem Hall do not automatically remain open, so you and your co-workers should be<br />

prepared to operate the hand-valve on the drench hose <strong>for</strong> injured students.<br />

Chemical injury to the eyes occur quickly and they need to be cleaned out rapidly, which means<br />

you need to be able to locate the eyewash fountain literally with your eyes closed. Practice this at least once<br />

in research labs.<br />

Other sections <strong>of</strong> this manual elaborate the necessity <strong>of</strong> wearing safety glasses while working with<br />

chemicals. The following eyewash fountain / lab drench hose directions will serve as your <strong>for</strong>mal guide <strong>for</strong><br />

using this equipment in the event you have not seen the a<strong>for</strong>ementioned general chemistry safety film<br />

entitled “Starting with Safety.”<br />

1. Memorize the location <strong>of</strong> eyewash fountains, lab drench hoses, and safety showers in your lab.<br />

2. Be prepared to help injured colleagues wash their eyes out properly. In other words, help them adjust<br />

to the discom<strong>for</strong>t <strong>of</strong> holding their faces in streams <strong>of</strong> cold water and <strong>for</strong>cing their eyelids open, thus<br />

avoiding the impulse to close eyes tightly after chemical exposure while attempting to irrigate them<br />

with water.<br />

3. Do not wear contact lenses in any lab while using chemicals.<br />

4. Know where to locate the emergency phone in your work area and how to call <strong>for</strong> medical help. Get<br />

medical help immediately after eye injuries.<br />

5. Wash out eyes <strong>for</strong> 10 to 15 minutes. Wash chemical spills on skin also. Don’t rub your eyes while<br />

washing them out.<br />

As <strong>for</strong> safety showers, make use <strong>of</strong> them by simply standing underneath and pulling the hand ring<br />

downwards. In most cases, heavy drenching with mineral acids or corrosive organic chemicals will require<br />

disrobing <strong>of</strong> at least the entire exposed clothing articles.<br />

The next page here lists physical locations <strong>of</strong> all eyewash fountains, fire blankets, and safety<br />

showers in Salem Hall.<br />

34


INVENTORY OF EYEWASH FOUNTAINS AND LAB EYEWASH<br />

DRENCH HOSES AND<br />

SAFETY SHOWERS / FIRE<br />

SALEM HALL<br />

BLANKETS<br />

Room # # <strong>of</strong> Safety Showers # <strong>of</strong> Drench Hoses # <strong>of</strong> Eyewash Fountains<br />

loading dock area 1 1<br />

7 1 1<br />

6 1 1<br />

2 1 1<br />

5 1 1<br />

13 1 1<br />

14 1 1<br />

17 1 1<br />

18 1 1<br />

101 1 8<br />

102 1 8<br />

103 1<br />

105 1 8<br />

106 1 8<br />

107 1 3<br />

108B 1 1<br />

109 1 4<br />

111 1 7<br />

112A 2<br />

113 1 1<br />

114 1 1<br />

117 1 1<br />

118 1 1<br />

Note: Fire Blankets are located in the hall in between the rooms specified below.<br />

Room #'s # <strong>of</strong> Fire Blankets<br />

101-103 1<br />

105-107 1<br />

111-113 1<br />

115-117 1<br />

1-3 1<br />

3-5 1<br />

11-13 1<br />

next to 12A 1<br />

15A-17 1<br />

35


5. Lab Fires and <strong>Use</strong> <strong>of</strong> Fire Extinguishers<br />

1. When graduate students are assigned to a particular research laboratory, they should look over the<br />

phone numbers on the “Telephone #s <strong>of</strong> Emergency Personnel / Emergency Facilities” sheet in this manual<br />

and take note <strong>of</strong> the location <strong>of</strong> all fire extinguishers within their lab and the nearest hallway fire blanket,<br />

dry powder fire extinguisher, fire alarm, and exit signs. Also, look at the Emergency Exit Plan map posted<br />

just outside your lab in the hallway. When a fire starts <strong>for</strong> any reason, consider the hazard to adjacent lab<br />

rooms, the hallway, and the building as a whole be<strong>for</strong>e activating the alarm. Decide yourself or from the<br />

assistance <strong>of</strong> others whether you can extinguish the fire with your laboratory safety equipment. Calling<br />

campus security (phone 5911) may be in order be<strong>for</strong>e calling the local fire station (phone 911), located a<br />

short distance away on Reynolda Road. Naturally, fires that have grown or show the potential <strong>of</strong> growing<br />

quickly into large-scale furniture or wall/ceiling fires call <strong>for</strong> a swift pull on the Fire Alarm.<br />

2. Bunsen burner flames should be allowed only in sections <strong>of</strong> the lab free from solvent vapors, organic<br />

solvents, or generally anything else which may accidentally combust while your back is turned. Clear the<br />

bench space around the burner be<strong>for</strong>e you light up. Do not leave glass-working torches or Bunsen burners<br />

on unless someone is in the lab.<br />

3. <strong>Use</strong> the designated fire extinguisher <strong>for</strong> the type <strong>of</strong> fire encountered. Extinguishers are marked with<br />

letters or descriptive pictographs corresponding to the following types <strong>of</strong> fires:<br />

A - common combustible solid material (wood, carpets, paper, etc.)<br />

B - flammable organic solvent liquids<br />

C - electrical equipment<br />

D - combustible chemical metals (e.g., sodium, phosphorus, lithium aluminum hydride,<br />

etc.)<br />

Each laboratory in Salem Hall is equipped with all needed types <strong>of</strong> fire extinguishers. Carbon<br />

dioxide (CO2) extinguishers are the most numerous, being located in all undergraduate and research<br />

laboratories. They are rated <strong>for</strong> type B and C fires.<br />

One multipurpose dry chemical powder extinguisher (containing an ammonium phosphate base<br />

inert material) is located in each hallway wing <strong>of</strong> the building outside <strong>of</strong> the laboratories. These are rated<br />

<strong>for</strong> A, B, and C type fires.<br />

Large type D extinguishers are located in particular research laboratories, those likely to deal with<br />

combustible metals.<br />

Most laboratory fires can be extinguished with CO2. Discharged extinguishers can be refilled by<br />

Physical Facilities, phone # 4255. Call them when you use more than half an extinguisher.<br />

4. Fire blankets <strong>for</strong> smothering clothing fires are located in each building hallway wing, on the wall in a<br />

vertical red metal container. <strong>Use</strong> them by grasping the rope loop on the right side and revolving your body<br />

leftward until you are tightly wrapped.<br />

5. Pull the retaining pin out <strong>of</strong> the extinguisher handle by TWISTING THE PIN LATERALLY TO<br />

BREAK THE PLASTIC TIE and then pulling out the pin, away from the cylinder. Aim the extinguisher<br />

spray at the base <strong>of</strong> the flame, not the flame itself. Organic solvent fires will spread if you spray the<br />

retardant directly on the liquid – aim just above the liquid.<br />

6. (The following in<strong>for</strong>mation was provided by Dave Brown, <strong>for</strong>mer WFU Safety Director).<br />

“The most common [fire safety] violations are listed below. Most are easily corrected and require<br />

minimal ef<strong>for</strong>t. Corrective action should be taken immediately if any <strong>of</strong> these situations exist.<br />

36


“COMMON FIRE CODE VIOLATIONS<br />

“Electrical<br />

a. Flat extension cords are not allowed. Power strips with built-in circuit breakers are<br />

acceptable. Don’t overload electrical circuits with too many appliances.<br />

b. Power strips cannot be plugged into other power strips (piggybacking).<br />

c. Faulty outlets (loose, broken, missing cover plates, ungrounded) must be repaired ASAP by<br />

Physical Facilities.<br />

d. Electrical panels must be fully accessible.<br />

e. Cords on appliances should not be frayed, spliced or cracked. If they are, have them<br />

repaired by Physical Facilities.<br />

“Exits<br />

a. Exits must be kept unlocked unless equipped with panic type hardware.<br />

b. Exit passages (stairways, hallways) are to be kept clear. No storage is allowed.<br />

c. Exits must be clearly indicated and equipped with functioning exit lights.<br />

d. Exit doors must be operable with no greater than 15 pounds <strong>of</strong> pressure and must not bind.<br />

“Housekeeping<br />

a. Areas must be clean, free <strong>of</strong> debris and combustibles (paper, rags, boxes).<br />

b. All containers must be clearly labeled to identify contents<br />

c. Flammable liquids must be stored in flammable liquids cabinets” [ or <strong>care</strong>fully stored in<br />

minimal amounts on laboratory shelves - MAT].<br />

7. Fire alarms are located in the following hallways:<br />

Ground Floor First Floor Second Floor<br />

1. Stairwell North 1. Left front door 1. Next to North Stairs<br />

2. Stairwell South 2. Right front door 2. Next to South Stairs<br />

3. Next to Rm. 7 3. Next to North door<br />

4. Next to Rm. 1 4. Next to South door<br />

5. Next to Rm. 17 5. Next to North Stairs<br />

6. Next to South Stairs<br />

Activating a fire alarm is a serious matter, not to be taken lightly. Most people realize this,<br />

perhaps even to such an extent as to render themselves reluctant to do so when it is clearly necessary. DO<br />

NOT hesitate to pull an alarm when a laboratory fire has grown out <strong>of</strong> control. Break the glass on the alarm<br />

with the attached breaking device and PULL! You should know the location <strong>of</strong> the nearest alarm to your<br />

lab and examine it at least once when you begin working in that area.<br />

Fire extinguisher inspections <strong>for</strong> Salem Hall are conducted periodically by Mr. Scott Frazier [WFU<br />

Assistant Environmental Health and Safety (EHS) Director]. Please call him at phone # 4329 to get<br />

extinguishers recharged if they are emptied during a fire in your lab. All Fire Extinguisher Inspection<br />

Records are kept with him, also.<br />

References <strong>for</strong> General Safety Procedures:<br />

Safety in Academic Laboratories, 6 th edition. American Chemical Society, Washington D.C.:<br />

1995, pages 3-8, 32.<br />

Chemical Safety Manual <strong>for</strong> Small Businesses, 2 nd edition. American Chemical Society,<br />

Washington D.C.: 1992, pages 4-11, 25-31, 53-59.<br />

37


C. Procedures <strong>for</strong> Handling Hazardous Chemical Waste<br />

1. HAZARDOUS WASTE COLLECTION: GENERAL GUIDELINES<br />

Please collect chemical waste in well-labeled containers (with labels headed with the wording<br />

“HAZARDOUS WASTE, Date______”) and store in your research or work area, fully enclosed and<br />

preferably kept in a hood or in the vented cabinets beneath the hood. Keep aqueous solutions separated<br />

from organic solvents. Do not mix liquids with large amounts <strong>of</strong> solids. Consolidate chemically compatible<br />

inorganic solids in one bottle, and organic solids in another. Incompatible or mutually reactive<br />

compounds should not be placed in the same bottle. (See Prudent Practices, 2nd edition, table 3.9 on<br />

page 52 and table 3.10 on page 54). When in doubt whether you are mixing incompatible chemicals,<br />

consult the laboratory manager or a pr<strong>of</strong>essor. The safest course is to keep each particular compound in a<br />

different container if you have the slightest suspicion that one <strong>of</strong> the waste chemicals may react with the<br />

other.<br />

Aqueous solutions or mixed Organic <strong>Solvent</strong>s should be labeled with the solvent name(s) and<br />

approximate weight or volume percentage <strong>of</strong> each listed dissolved solid chemical component (i.e., 10%,<br />

1%, 0.01%, less than 1%, etc.).<br />

When you are ready to dispose <strong>of</strong> waste, take it to the metal surface table in the solvent room #20,<br />

located next to the acetone drum, in the loading dock area <strong>of</strong> Salem Hall. Chemical solids, in appropriate<br />

labeled containers, and small one to four liter size bottles <strong>of</strong> labeled organic solvents and aqueous inorganic<br />

solutions can also be placed here.<br />

Extremely reactive and very toxic waste can be stored in the hood in the chemical storage room<br />

#19 (i.e., sodium metal, osmium tetroxide, phosphorus, sodium cyanide, barium cyanide, reactive metal<br />

hydrides, etc.) LABEL WITH A HEADING OF “HAZARDOUS WASTE”, AND THEN LIST<br />

BELOW IT A SPECIFIC SPELLED-OUT CHEMICAL NAME OR NAMES AND DATE IT WITH<br />

THE DAY OF THE MONTH AND YEAR THE WASTE WAS COLLECTED. Waste companies will<br />

not accept unidentified waste. Labels such as "aromatic waste" or "inorganic salts" are inappropriate and<br />

will be returned to you. AGAIN, LABEL WITH SPECIFIC FULLY SPELLED OUT CHEMICAL<br />

NAMES. Place organic peroxides on the bottom shelf <strong>of</strong> this hood and keep away from organic or<br />

inorganic acids.<br />

A designated Graduate Student or teaching assistant <strong>for</strong> your work area will maintain a Micros<strong>of</strong>t<br />

Word document listing <strong>of</strong> typical waste generated in your lab, which will be emailed to the Laboratory<br />

manager at mathomps@wfu.edu in your department when the waste is ready <strong>for</strong> removal to the <strong>Solvent</strong><br />

room # 20. <strong>Example</strong>s <strong>of</strong> labels include:<br />

HAZARDOUS WASTE, Date 02-22-07 (This date refers to the date that the waste<br />

) One white plastic container <strong>of</strong> filter paper and Organic solids: is actually taken downstairs to the<br />

� N-Acetyl-2-aminobenzoic acid Chemical waste “Accumulation”<br />

� 9-Fluorenol area in the <strong>Solvent</strong> room)<br />

� Methoxychalcone<br />

� Naphthalene<br />

HAZARDOUS WASTE, Date 02-22-07<br />

) Water with:<br />

� Sodium iodide, approximately 5%<br />

� Ammonium chloride, 2-5%<br />

� Sodium sulfate, less than 1%<br />

� Sodium thiosulfate, less than 1%<br />

HAZARDOUS WASTE, Date 02-03-06<br />

38


) 4-Bromodimethylaniline<br />

HAZARDOUS WASTE, Date 03-15-02<br />

) Two bottles <strong>of</strong> Water (acidic) with:<br />

� Bis(salicylaldehydato)nickel (II) dehydrate<br />

� Bis(salicylaldiminato)nickel (II)<br />

� Bis(N-2’-butylsalicylaldiminato)nickel (II)<br />

HAZARDOUS WASTE, Date 11-19-06<br />

) Two bottles <strong>of</strong> Acetone, Hexane, and Ethyl ether with:<br />

� Acetophenone<br />

� Anisole<br />

� Benzaldehyde<br />

� Benzyl alcohol<br />

� Benzoic acid<br />

� Naphthalene<br />

Aqueous solutions should be checked with (blue) litmus paper and labeled acidic (see above<br />

example) if necessary, although the presence <strong>of</strong> a compound named as an acid (e.g., Acetic acid) will<br />

ordinarily be sufficient to indicate that the material inside is acidic.<br />

Each research laboratory should maintain its own supply <strong>of</strong> spent reagent bottles to be used as<br />

waste containers. Please take extras to the small marked cart or under the metal table <strong>of</strong> room #20 <strong>for</strong><br />

community use. You may take containers from this area when you need them. If necessary, get clean<br />

bottles from the stockroom, #110, or the general chemistry preparation room, #103. Gallon sized glass jars<br />

are located in room #103, and empty 5 gallon blue Fisher metal cans are located in the solvent room, #20.<br />

White five gallon polyethylene jugs are also in room #103.<br />

The waste chemicals will eventually be "lab-packed" or enclosed in safe transportation packages<br />

and taken out by waste treatment firms.<br />

Wake Forest University's hazardous waste is currently removed by a national company with a<br />

branch in North Carolina:<br />

ONYX ENVIRONMENTAL SERVICES Carolina Environ Associates American Envr. Services.<br />

2176 Pressley Road P.O. Box 963 9741 Suite I<br />

Charlotte, NC 28217 or, alternately: Burlington, NC 28216-0963 Southern Pine Blvd<br />

Tel.No. (800) 626-1461 336-229-0058 Charlotte, NC 28273<br />

Phone 704-527-4777<br />

These companies maintain treatment and storage facilities in North Carolina and disposal facilities in other<br />

states, like New Jersey.<br />

39


2. Common Organic Waste <strong>Solvent</strong>s<br />

The following common laboratory organic solvents can be poured into one <strong>of</strong> the two 55 gallon<br />

waste drums located in the solvent room, #20, labeled HAZARDOUS WASTE, Non-Sulfur, Non-<br />

Halogenated Organic <strong>Solvent</strong>s, meant <strong>for</strong> the following highly flammable, generally non-reactive<br />

hydrocarbons, commonly used in most academic research and teaching Labs. Do not add water or acidic<br />

material to these drums:<br />

acetone methyl ethyl ketone pump oil<br />

benzaldehyde mineral spirits tetrahydr<strong>of</strong>uran<br />

benzene motor oil toluene<br />

cyclohexane naphtha xylenes<br />

ethyl ether paint thinner ethyl alcohol, (and,<br />

ethyl acetate petroleum ether low-molecular weight alcohols,<br />

heptane propanol (1 or 2-propanol) cyclohexanol, methanol )<br />

hexane propyl acetate ethylene glycol<br />

Dimethyl<strong>for</strong>mamide<br />

You must list each chemical by name and approximate amount (liters) in logbooks kept near each<br />

drum. DO NOT OVERFILL THESE DRUMS! Leave about 4 to 6 inches from the top. Don't empty<br />

mineral acids, organic acids, or aqueous solutions into these drums. Oxidizers in the presence <strong>of</strong> mixed<br />

organic solvents may cause a fire. Waste companies do not appreciate receiving organic solvent drums with<br />

a water layer on the bottom.<br />

All other organic solvents not on the list above must be poured into separate glass or metal<br />

containers, labeled, and placed on the metal table. This includes any potentially reactive or unstable<br />

liquid organic chemical. <strong>Example</strong>s would be sulfur-containing compounds, complex heterocyclics,<br />

corrosives, organic acids, lachrymators, etc. - i.e., bromine, acetic anhydride, acetyl chloride,<br />

chlorosulfonic acid, pyridine, acetonitrile, alanine, 1,4-dioxane, tert-butyl chloride, etc.<br />

The two common halogenated organic solvents (methylene chloride and chloro<strong>for</strong>m, only) must<br />

be separated from other solvents and poured into labeled, 20 liter empty white polyethylene containers kept<br />

next to the large 55 gallon steel drums, on the floor in the wide yellow spill tray. When a waste company is<br />

called to take out waste (about once every three months) these halogenated solvents will be consolidated<br />

into one 55 gallon drum - to do so earlier would cause buildup <strong>of</strong> rust within the larger drums. Methylene<br />

chloride hydrolyzes and produces HCl which causes metal cans to rust. Do not deposit these two solvents<br />

in metal cans.<br />

3. SAFETY PRECAUTIONS IN SOLVENT ROOM<br />

Note that an eyewash station and safety shower are located just outside the door, in the loading<br />

dock area. Wear safety glasses and chemically resistant gloves. Absorbent material <strong>for</strong> chemical spills is<br />

located on the second metal table located next to the large 55 gallon drums. Follow the chemical spill<br />

procedure in section III.J.3 <strong>of</strong> this manual. There is a rear emergency exit door. Please keep this door<br />

unlocked from inside and locked from outside the room.<br />

In the event <strong>of</strong> a fire, the automatic fire extinguisher system in the ceiling will trigger. Additional<br />

fire extinguishers are located by the entrance doorway. Report any spills or corroded waste containers.<br />

Static electricity discharge cables are located on the large 55 gallon drums. Connect these to metal waste<br />

containers be<strong>for</strong>e you pour waste from them into the drum. Please note that the newly installed independent<br />

ventilation systems in both the solvent room and the chemical storage room were designed to maintain<br />

concentrations <strong>of</strong> chemical fumes below the Permissible Exposure Limit (PEL). Report any malfunction <strong>of</strong><br />

the ventilation system to Physical Facilities (phone x-4255).<br />

Some Fisher organic solvents in 20 liter blue-metal cans, placed in this room <strong>for</strong> community use,<br />

are capable <strong>of</strong> peroxide <strong>for</strong>mation once opened and exposed to air <strong>for</strong> long periods. If half emptied and left<br />

<strong>for</strong> 5 or 6 months, these solvents may become explosive. DO NOT OPEN NEW CANS OF THIS<br />

MATERIAL UNTIL CANS THAT HAVE ALREADY BEEN OPENED ARE USED UP ENTIRELY:<br />

Diethyl ether, Tetrahydr<strong>of</strong>uran, 1,4-Dioxane<br />

Date the label <strong>of</strong> these chemicals with the date on which the container was first opened. If the above cans<br />

are not labeled, the laboratory manager will begin ordering these solvents individually, rather than in-bulk,<br />

until students learn to properly date them. Be sure to tighten the black plastic spout cap after dispensing<br />

any solvents kept in this room. The hazardous waste storage area is checked weekly by the laboratory<br />

40


manager and stockroom personnel using a standard <strong>for</strong>m located on the second metal table. Do not move<br />

the logbook from this area.<br />

4. MERCURY SPILLS<br />

At present, there is no legal method <strong>for</strong> disposing <strong>of</strong> metallic mercury. Take broken<br />

thermometers and place in the white plastic pail located in the hood <strong>of</strong> the chemical storage room,<br />

#19, across from the solvent room. These are recycled with the chemical waste company serving Salem<br />

Hall.. Mercury spills should be collected with a vacuum hand pump (“Hg Vac”, Lab Supply Company<br />

Catalog # YB-20754, refill pack catalog # YB-16613). Empty the collection tube into a wide mouth glass<br />

bottle and take it to the plastic holding tray located beneath the hood in room # 19, underneath the broken<br />

thermometer white plastic pail. Every ef<strong>for</strong>t should be made to collect mercury droplets with this device,<br />

instead <strong>of</strong> sweeping them up, since the mercury must be recycled and sold. Dirt and trash collected along<br />

with the mercury will contaminate it. Containers holding more trash than mercury will be returned to you<br />

<strong>for</strong> proper cleanup.<br />

Don‟t use commercially available mercury absorbent material, such as Lab Safety brand Mercury<br />

Vapor Absorbent and Hg Absorb (a zinc amalgam material) which are located in the stockroom, unless<br />

absolutely necessary, i.e., <strong>for</strong> very large spills <strong>of</strong> mercury which cannot be collected with the hand pump.<br />

This material will be extremely difficult to dispose <strong>of</strong>, since no waste company will take it. Charges<br />

incurred by the department in disposing <strong>of</strong> it will be reimbursed by the research group responsible <strong>for</strong> the<br />

spill.<br />

The mercury will eventually be poured into metal canisters, located on the floor next to the hood, and sold<br />

to the following mercury recycling center:<br />

Bethlehem Apparatus Company, Inc.<br />

890 Front Street; P.O. Box Y<br />

Hellertown, PA 18055<br />

Tel. No. (610)-838-7034<br />

An alternate company would be:<br />

D. F. Goldsmith, Chemical and Metal corp.<br />

909 Pitner Ave.<br />

Evanston, IL 60202<br />

Tel.No. (708) 869-7800<br />

5. WASTE FROM UNDERGRADUATE LABORATORIES, FIRST FLOOR<br />

Persons working as Teaching Assistants are responsible <strong>for</strong> handling waste generated by<br />

undergraduate students and transporting it to the solvent room. Chemical preparation persons are<br />

responsible <strong>for</strong> a) dispensing reagent and prepared chemicals to each lab bench and b) labeling empty waste<br />

containers and placing them in appropriate waste-holding areas in each lab be<strong>for</strong>e the experiment actually<br />

begins. Give T.A.'s only the number <strong>of</strong> waste containers actually needed <strong>for</strong> a particular week's experiment.<br />

Aqueous solutions <strong>of</strong> inorganic salts generated in the freshman lab classes will be poured into<br />

open, white or gray plastic pails located in the general chemistry prep room, #103, and left in the hood in<br />

that room to evaporate. The residue will be consolidated into one or two pails and taken to the solvent<br />

room when full. Label each pail with the full name (or <strong>for</strong>mula) <strong>of</strong> the component involved - i.e., Barium<br />

Chloride (or BaCl 2 ), Cadmium nitrate [or Cd(NO 3 ) 2 ], Silver nitrate (or AgNO 3 ), etc.<br />

Generally, these common inorganic salts should be placed in two different storage categories and<br />

not mixed together in the same white or gray plastic pail. One category is composed <strong>of</strong> higher toxic<br />

potential cations and anions, as specifically listed on pages 167 and 168 <strong>of</strong> Prudent Practices, 2nd Edition.<br />

The other category consists <strong>of</strong> very low toxic cations/anions, listed here as well. Do Not, however, place<br />

41


any aqueous solutions whatsoever <strong>of</strong> mercuric salts in any <strong>of</strong> these storage containers (i.e. mercuric<br />

chloride, mercurous nitrate, etc.) Mercuric salts, either Hg 1+ or Hg 2+ , cannot presently be taken<br />

by waste companies. We will have to store the evaporated remnants <strong>of</strong> these solutions in a labeled<br />

container, kept in the solvent room #20, until we can either recycle them or receive clear instructions from<br />

higher waste authorities. Be sure to read the Forsyth County/City <strong>of</strong> Winston-Salem ordinance disallowing<br />

drain disposal <strong>of</strong> metal cations above specific concentration levels, located in subchapter # 11, below. You<br />

should also read section 7.D.3.8, “Inorganic Ions”, <strong>of</strong> Prudent Practices, 2nd edition., pages 166-171.<br />

For all other waste handling and disposal involving freshman student labs please follow the<br />

guidelines listed under the “Chemical Handling” section <strong>of</strong> the modular laboratory student handouts,<br />

instruction‟s in<strong>for</strong>mation section. The teacher will give this in<strong>for</strong>mation to you.<br />

Organic chemistry Teaching Assistants will gather student waste containers located in the rear <strong>of</strong><br />

their assigned teaching laboratory rooms and take them to the solvent room, #20, <strong>for</strong> storage on the metal<br />

table. If each container is properly labeled be<strong>for</strong>e the experiment starts, you will not have to sort out the<br />

waste into new containers afterwards. Remember, the prep persons are responsible <strong>for</strong> dispensing<br />

chemicals and waste containers to your assigned area, but you are responsible <strong>for</strong> removing the waste to the<br />

solvent room, room #20, downstairs. Generally, most benign organic solids used in the undergrad Organic<br />

Labs can be mixed in the same container. When in doubt, check with your instructor or the laboratory<br />

manager.<br />

DO NOT MIX (OR ALLOW UNDERGRADS TO MIX) AQUEOUS SOLUTIONS WITH<br />

ORGANIC SOLVENTS, SOLIDS WITH LIQUIDS, OR OTHERWISE INCOMPATIBLE CHEMICALS<br />

IN THE SAME CONTAINER. These organic lab is equipped with a large, 2-liter, separatory funnel. If<br />

students have trouble separating aqueous and organic waste, have them pour their liquid waste into these<br />

funnels. At the end <strong>of</strong> the experiment, pour out the bottom layer <strong>of</strong> water and, if the aqueous ingredients are<br />

non-hazardous, non-regulated and chemically benign, neutralize it with sodium bicarbonate or baking soda,<br />

and pour them down the lab drains with copious amounts <strong>of</strong> water.<br />

In addition to the above guidelines, have the students read the “Cleaning Up” section at the end <strong>of</strong><br />

each particular experimental procedure in the class textbook, Williamson, Kenneth. Macroscale and<br />

Microscale Organic Experiments, 2nd edition. Lexington, MA: D.C. Heath and Company, 1994 and<br />

follow these instructions.<br />

Be<strong>for</strong>e taking the waste downstairs, you can store it temporarily in the hood <strong>of</strong> room #107, a<br />

general chemistry lab room. Keep a couple <strong>of</strong> 5 gallon metal solvent cans <strong>for</strong> common organic solvent<br />

waste (see list <strong>of</strong> common organic solvent list in previous section B, Waste Organic <strong>Solvent</strong>s). Place a<br />

separate paper label with the name <strong>of</strong> the solvent or solvents <strong>for</strong> each and every solvent poured into the<br />

drum. This drum should be labeled overall as the acidic organic solvent waste drum and should not be<br />

poured into the 55 gallon waste drum downstairs, since most organic experiments will involve some use <strong>of</strong><br />

mineral acids and will no doubt contaminate this organic solvent waste can. If the solvents are overly<br />

acidic, pour them into the large 2 liter separatory funnels in the back hoods <strong>of</strong> your lab, add some sodium<br />

bicarbonate aqueous solution, shake it out <strong>care</strong>fully, pour organic solvent back into the can and discard the<br />

water. By the time you fill the can, you should have at least a dozen labels on it. If this is not taken <strong>care</strong> <strong>of</strong><br />

by community ef<strong>for</strong>t among the TA‟s, THE LAB MANAGER WILL ASSIGN THIS TASK TO ONE<br />

PARTICULAR T.A. PER SEMESTER.<br />

Reactive solvents, like acetic anhydride or bromine, <strong>for</strong> example, should go into separate smaller<br />

containers, as should halogenated solvents, like methylene chloride or chloro<strong>for</strong>m.<br />

Solid organic compounds which are compatible (i.e., most organic solids used in undergraduate<br />

organic labs) can go into one communal wide-mouth glass or plastic jar, naturally, with named labels<br />

attached. Any overly reactive solid, like lithium aluminum hydride or sodium metal, etc., should go into<br />

separate containers. <strong>Use</strong> your judgment or ask <strong>for</strong> advice. Acidic or basic aqueous layers with trace<br />

amounts <strong>of</strong> non-toxic inorganic salt components can be neutralized with sodium bicarbonate or dilute<br />

mineral acids and dispensed into the lab sink drain, as per instructions in the above CRC procedure.<br />

42


Mineral acids (HCl, HNO 3 and H 2 SO 4 ), ammonium hydroxide (NH 4 OH), and Phosphoric Acid<br />

(H3PO4) can legally be disposed <strong>of</strong> as instructed in Armour, M.A., Hazardous Laboratory Chemicals<br />

Disposal Guide, 2nd edition. Boston: CRC Press, 1996, under the following conditions:<br />

a. The acids must be completely neutralized and this must occur as a definite part <strong>of</strong> the<br />

experimental procedure, preferably at the end.<br />

b. Dilute with at least 1:10 dilution <strong>of</strong> acid to H 2 O be<strong>for</strong>e neutralizing<br />

c. Contaminants present in the acid must be less than 1% total<br />

(A copy <strong>of</strong> this book is kept in the stockroom #110.)<br />

Do not dispose <strong>of</strong> hydr<strong>of</strong>luoric acid or perchloric acid in this manner. It should be given to the<br />

waste companies, as should spent chromerge (chromic acid/H 2 SO 4 ) cleaning mixtures.<br />

The listed procedures <strong>for</strong> all four mineral acids are basically as follows:<br />

Wear suitable gloves, such as nitrile rubber gloves (i.e., the blue, green, or yellow gloves located in<br />

the stockroom, room #110), a laboratory coat, and eye protection while slowly diluting the concentrated<br />

acid or further diluting less concentrated acids in a suitable container, such as a large beaker or a lab sink<br />

with a drain plug, or a large standard heavy-duty polyethlene pan.<br />

Add baking soda (sodium bicarbonate), sodium carbonate, calcium carbonate, or soda ash slowly<br />

into the diluted solution until neutralization is complete, i.e., until vapors <strong>of</strong> CO2 don‟t rise from the<br />

mixture. Pour the resulting solution down the drain with at least 50 times its volume in H20. All <strong>of</strong> this<br />

should preferably be done in a fume hood.<br />

Reaction equations <strong>for</strong> Neutralizations <strong>of</strong> Acids:<br />

2 HCl + Na2CO3 � 2NaCl + CO2 + H2O<br />

2HNO3 + Na2CO3 � 2NaNO3 + H2O + CO2<br />

H2SO4 + Na2CO3 � Na2SO4 + H2O + CO2<br />

Ammonia can similarly be disposed <strong>of</strong> using dilute hydrochloric acid as the neutralizing agent.<br />

Reaction equations <strong>for</strong> neutralizations <strong>of</strong> ammonium hydroxide and phosphoric acid:<br />

NH4OH + HCl � NH2Cl + H2O<br />

2 H3PO4 + 3 Na2CO3 � 2 Na3PO4 + 3 H2O + 3 CO2<br />

43


6. ALUMINA/SILICA-GEL CHROMATOGRAPHY WASTE<br />

label:<br />

This material should be packaged in 30 gallon blue polyethylene containers with the following<br />

HAZARDOUS WASTE,<br />

Date________<br />

Alumina/Silica-Gel<br />

a) Silica-gel 30 %<br />

b) Sand 30 %<br />

c) Alumina 30 %<br />

d) Florisil 10 %<br />

When full, take to the solvent room # 20 <strong>for</strong> storage.<br />

7. SPENT LECTURE-BOTTLE COMPRESSED GAS CYLINDERS<br />

These metal cylinders, when completely empty, can be legally disposed <strong>of</strong> via the local landfill by<br />

labeling "EMPTY" with clearly visible markings and depositing in the loading dock garbage bins. This<br />

would apply to inert or non-air sensitive gases which are spent, entirely. However, it is not advisable to do<br />

this. Naturally, it would be better to return the cylinders to the original vender.<br />

Lecture bottles bought from Sigma-Aldrich Chemical Company are especially easy to return.<br />

Their cylinder return service instructions can be obtained by calling 1-800-558-9160, the customer service<br />

department. The cost is about $27.00. Most lecture bottles are best purchased from this company, anyway,<br />

if not National Welders. Twenty-seven dollars is much less than the $200 to $300 that most waste<br />

companies would charge. Give them the in<strong>for</strong>mation they need (our account # with Sigma-Aldrich, the<br />

catalog # <strong>of</strong> the cylinder, and the chemical name) and they will send you shipping labels so that we can send<br />

back empty lecture bottles in cardboard boxes, properly labeled with the DOT chemical warning labels that<br />

were shipped to you with the cylinder when you received it. SAVE THE SHIPPING BOX AND THE<br />

WARNING LABELS THAT YOU RECEIVED WITH THE LECTURE BOTTLE. The lab manager will<br />

make arrangements to send the cylinders back via Roadway transportation services, phone # 993-4811 in<br />

Kernersville, NC. They must be sent by truck. UPS will not take them.<br />

The following Matheson Gas Company lecture bottle gases are sold by Fisher Scientific Co.:<br />

Gas Catalog #<br />

Ammonia 10-599A<br />

Carbon Dioxide 10-599E<br />

Chlorine 10-599F<br />

Ethylene 10-599I<br />

Helium 10-599J<br />

Hydrogen 10-599K<br />

Hydrogen Sulfide 10-599L<br />

Methane 10-599N<br />

Nitrogen 10-599P<br />

Oxygen 10-599R<br />

SO2 Anhydrous 10-599W<br />

This is generally the least expensive source <strong>of</strong> such lecture bottle size gas cylinders, and you can<br />

return them by mail to Matheson via the following procedure:<br />

Call Matheson Gas Products at phone # (770) 961-7891, Morrow, GA, and follow these steps, as<br />

stipulated by the company:<br />

44


1. “Lecture Bottles must be Matheson Lecture Bottles.<br />

2. Bottles must be properly labeled (original).<br />

3. Valves must be operable and in good condition.<br />

4. Product must be from existing product line or will not be accepted.<br />

5. Accepting location must have capability to drain cylinders. (It does, at least in Morrow, GA)<br />

6. Lecture Bottles must be in generally good condition.<br />

7. A flat return charge <strong>of</strong> $40.00 per Lecture Bottle will be assessed to cover processing costs.<br />

8. Prior arrangements must be made be<strong>for</strong>e making returns.<br />

(Call above phone number and send to:<br />

Matheson Gas Products<br />

6874 South Main Street<br />

Morrow, Ga 30260)<br />

“See DOT Shipment <strong>of</strong> Chemicals section in the laboratory manager’s copy <strong>of</strong> this manual<br />

<strong>for</strong> proper labels to add to the box. The laboratory manager will have proper DOT warning<br />

labels you can add to the shipping container. It is a good idea to keep the original shipping<br />

box, with the labels already affixed, somewhere in your lab or in the storage room #8A, <strong>for</strong><br />

future shipment <strong>of</strong> the empty cylinder. Remember, no gas cylinder should be completely<br />

drained, so you will have trace amounts <strong>of</strong> gas in the bottle, enough <strong>for</strong> justification <strong>of</strong><br />

warning labels.<br />

9. Any bottles received not meeting these criteria will be returned to the customer.<br />

10. Matheson reserves the right to refuse all lecture bottles.<br />

“The company regrets any inconvenience this may cause, however, Matheson cannot continue to<br />

absorb the increasing costs <strong>of</strong> cylinder reclamation (due to unidentifiable, non-labeled lecture<br />

bottles").<br />

National Welders, Inc., a local company which supplies our large-size gas cylinders, is also a<br />

dealer <strong>for</strong> Matheson lecture bottles. This company will collect most empty cylinders when requested.<br />

Please contact them by phone (744-0010) and take the cylinders to the "Empty Cylinder" area in the outer<br />

loading dock area <strong>of</strong> Salem Hall. NEVER COMPLETELY EXPEND CORROSIVE, AIR-SENSITIVE,<br />

MOISTURE-SENSITIVE OR STRONG OXIDIZER GASES FROM LECTURE BOTTLES. Outside air<br />

will be drawn into the cylinder and an explosion may occur after contact with oxygen, water vapor or<br />

oxidizable material (like organic lubricants or grease). Return the cylinder to the vendor with about 20-25<br />

psi remaining in the tank. Consult your research advisor if you have any uncertainties as to the safety <strong>of</strong><br />

emptying a particular cylinder.<br />

8. Lab Procedures <strong>for</strong> “In-Process” disposal <strong>of</strong> Highly Reactive Chemicals<br />

Occasionally a chemical encountered in research laboratories is so corrosive or reactive that it must be<br />

destroyed as part <strong>of</strong> the experimental procedure when it is spent or no longer in a useable <strong>for</strong>m. If it is to be<br />

used in an experiment and is clearly in need <strong>of</strong> “in-process” destruction, consult with your research advisor<br />

and obtain such in<strong>for</strong>mation from the chemical literature or one <strong>of</strong> the following sources:<br />

Armour, M.A. Hazardous Laboratory Chemicals Disposal Guide, 2nd edition. Boston: CRC Press, 1996,<br />

located in the chemistry stockroom, Room # 110.<br />

Lunn, George and Sansone, Eric B. Destruction <strong>of</strong> Hazardous Chemicals in the Laboratory, 2nd edition.<br />

New York: John Wiley and Sons, Inc., 1994.<br />

Prudent Practices, 2nd edition, especially Chapter 7.<br />

9. Responsibilities <strong>of</strong> Laboratory Personnel<br />

Persons working as teaching assistants, laboratory chemical preparation persons or stockroom<br />

workers cleaning up in various undergraduate laboratories will begin to include the handling <strong>of</strong> chemical<br />

waste in their repertoire <strong>of</strong> privileges and responsibilities associated with being students <strong>of</strong> science.<br />

As <strong>for</strong> research laboratories, please note that you are responsible <strong>for</strong> your own chemical waste.<br />

Label all containers, list all components with approximate percentages <strong>of</strong> each, bottle or can up all chemical<br />

waste, and move it out to the solvent room, #20. Please try not to clutter this area. Report any infractions<br />

<strong>of</strong> safety rules, spills, accidents, etc. occurring in this room to the laboratory manager.<br />

45


YOU ARE REQUESTED TO READ SECTION 5.C.6 OF Prudent Practices, 2nd edition, pages 84-85,<br />

FOR A GOOD SUMMARY OF THE CHEMICAL WASTE PROCEDURES LISTED IN THIS<br />

MANUAL.<br />

It is hereby stipulated that each research laboratory group designate one graduate student to<br />

oversee the collection and transportation <strong>of</strong> chemical waste from the group‟s work area to the metal table or<br />

55 gallon solvent waste drum in room #20. In particular, this designated person has the responsibility <strong>of</strong><br />

visually checking the contents <strong>of</strong> each waste container be<strong>for</strong>e it is take by other students within the group to<br />

the waste holding area, to make certain incompatible chemicals have not been placed in the same container.<br />

This should be a permanent or rotating assignment, based on research priorities and faculty dictate.<br />

10. Laboratory Manager Responsibilities<br />

As the designated “Hazardous Substance Officer” <strong>for</strong> the Chemistry Department, the laboratory manager is<br />

responsible <strong>for</strong>:<br />

1. Coordination <strong>of</strong> the Chemistry Department‟s compliance with local fire department, state, and<br />

federal laws on hazardous substances.<br />

2. Inventory <strong>of</strong> all chemicals <strong>for</strong> the Chemistry Department.<br />

3. Securing Material Safety Data Sheets <strong>for</strong> all chemicals <strong>for</strong> the Chemistry Department.<br />

4. Preparing a written Standard Operating Procedure <strong>for</strong> handling chemical waste <strong>for</strong> the<br />

Chemistry Department.<br />

All hazardous waste in Salem Hall must be contained, cataloged, recorded, manifested and sent out<br />

to waste companies. The laboratory manager will be more than happy to describe the regulatory<br />

requirements <strong>of</strong> chemical waste with you and supervise the manner in which it is handled by you.<br />

11. Conversation with Ms. Crystall Couch on 4/1/93 (As per instructions from Dr. Antony Shoaf,<br />

<strong>for</strong>mer Chemical/Biohazard Officer, Bowman Gray School <strong>of</strong> Medicine, WFU):<br />

“On March 8, 1993, the City/County Utilities Commission passed ordinances which required that<br />

all businesses in Winston-Salem and Forsyth County to not dump concentrations <strong>of</strong> metal ions and certain<br />

pollutants into the city sewage which are greater than the concentrations listed below. If the<br />

concentrations <strong>of</strong> any <strong>of</strong> the constituents listed below are greater than the listed maximum in the effluents<br />

leading from a facility, then that facility will require a special permit.<br />

“Pollutant Maximum Permitted Level in Effluents, ppm (mg/l)<br />

Ag (Silver) < .002 Note: These concentrations are<br />

As(Arsenic) < .005 incredibly dilute. This section generally<br />

Cd (Cadmium) < .005 applies to trace amounts <strong>of</strong> material left in<br />

Cr (Chromium) < .03 dirty lab glassware which is cleaned in lab<br />

Hg (Mercury) < .0002 sinks and does not imply permission to<br />

Cu (Copper) < .2 dump toxic inorganic salts down the drain.<br />

Pb (Lead) < .05 See Prudent Practices, 2nd edition, page 166,<br />

Ni (Nickel) < .05 <strong>for</strong> a discussion <strong>of</strong> how to distinguish<br />

Zn (Zinc) < .005 between toxic and nontoxic inorganic salts.<br />

BOD 500<br />

Susp. Solids 500<br />

pH between 5 and 10<br />

Hydrocarbons, oil,<br />

and grease < 100<br />

Cn - (Cyanide) < .005”<br />

12. Chemical Waste listed by the EPA as “Acute Hazardous Waste” (P-Listed Waste)<br />

Certain chemicals are considered so hazardous as chemical waste, either because <strong>of</strong> their toxicity<br />

or reactivity, that research laboratory generation <strong>of</strong> them must remain below a certain amount per month<br />

46


(one kilogram per month, total amount <strong>for</strong> the Reynolda campus). Otherwise the university could lose its<br />

EPA “Small Quantity Generator” status [meaning small quantity generator <strong>of</strong> hazardous waste]. In the<br />

event this status is lost, much more regulatory paperwork is required <strong>for</strong> what will then be a “Large Quantity<br />

Generator”.<br />

It is advisable that you consult the list <strong>of</strong> such chemicals (referred to by the EPA and “P-list waste”<br />

because the waste codes begin with the letter P) at least once to become familiar with it. It is listed in the<br />

appendix <strong>of</strong> this manual.<br />

As an example <strong>of</strong> precautions to use, consider the following suggestion. Suppose your research<br />

lab generates Osmium tetroxide. This is a P-list waste and you should either end up with only a very small<br />

amount to dispose <strong>of</strong> (say 1 to 200 grams, or 500 mL <strong>of</strong> solution) or set in place a procedure to detoxify or<br />

decontaminate the material, though chemical decomposition, as the last step in your overall reaction<br />

process. Be sure to add this procedure to your reaction process while in progress. Do not treat hazardous<br />

waste after the reaction process has been stopped or disassembled. In house treatment <strong>of</strong> stored hazardous<br />

waste, other than simple neutralization, is not presently permitted by the EPA.<br />

13. Hazardous Waste Record-Keeping <strong>for</strong> WFU and the Chemistry Department<br />

All hazardous chemical waste generated by the university must be properly “manifested”. That is,<br />

shipping papers, prepared by waste companies, must be kept on campus <strong>for</strong> future reference - as required by<br />

RCRA (the Resource Conservation and Recovery Act) and explained on pages 146 and section 9.D, page<br />

205, <strong>of</strong> Prudent Practices, 2nd edition, if you wish to read it (not required reading). All such manifests are<br />

now kept by the Assistant Environmental Health and Safety (EHS) Director, Scott Frazier, at Physical<br />

Facilities. Copies <strong>of</strong> the Waste Company‟s Packing Slip listing <strong>of</strong> all waste chemicals collected from the<br />

Chemistry Department are kept by the Chemistry Department laboratory manager in the top drawer <strong>of</strong><br />

OSHA file cabinet, Chemistry Department Stockroom # 110.<br />

47


Summary <strong>of</strong> Rules <strong>for</strong> Chemical Waste Collection and Labeling<br />

Nearly all spent chemicals generated in teaching and research laboratories should be securely bottled or packaged, labeled,<br />

and stored in or near a laboratory hood, the solvent room # 20 (Loading Dock area), or other safe, secure areas within your Laboratory<br />

stipulated by your research or teaching advisor. Some chemicals are regarded as non-hazardous, non-regulated chemicals and may be<br />

safely deposited in the normal garbage, but the identity <strong>of</strong> these chemicals is not usually something students would be expected to<br />

readily recognize (e.g., “paper, corks, sand, alumina [used in chromatography experiments], silica gel, sodium sulfate, magnesium<br />

sulfate, and so on….”, as explained in the Organic teaching lab CHEM 122L textbook The Organic Chem Lab Survival Manual,<br />

Chapter one, “Disposing <strong>of</strong> Waste”. There<strong>for</strong>e, since most <strong>of</strong> our waste is ultimately given to a Chemical Waste company <strong>for</strong> pickup,<br />

it is advised that nearly all <strong>of</strong> the waste in your work area be handled as follows:<br />

Be sure that the wording “HAZARDOUS WASTE, Date _______” appears as a heading on the label and the begin identifying each<br />

<strong>of</strong> the chemical components with its fully spelled out name, not its chemical <strong>for</strong>mula. For example:<br />

HAZARDOUS WASTE, Date 11-19-06 DO NOT WRITE Na Write out the word “Sodium”<br />

) One bottle <strong>of</strong> Sodium metal in Mineral oil<br />

HAZARDOUS WASTE, Date 03-31-02<br />

) One bottle <strong>of</strong> Organic solids: DO NOT WRITE THE CHEMICAL SYMBOLS OR FORMULAS ONLY<br />

� 1-Naphthol<br />

� Glucose pentaacetate<br />

� Nitrotyrosine (in glass vials)<br />

� 4-Aminobenzenesulfonic acid<br />

� 8-Anilino-1-naphthalenesulfonic acid, ammonium salt hydrate<br />

1. Keep aqueous solutions separated from organic solvents, ins<strong>of</strong>ar as possible. If you do mix the two together, make sure<br />

that in<strong>for</strong>mation is on the label, although it is better to separate the layers (organic and aqueous phases) and place them in<br />

separate containers.<br />

2. Do not mix liquids with large amounts <strong>of</strong> solids.<br />

3. Consolidate chemically compatible inorganic solids in one bottle, and organic solids in another. Incompatible or<br />

mutually reactive compounds should not be placed in the same bottle.<br />

4. Keep each particular compound in a different container if you have the slightest suspicion that one <strong>of</strong> the waste chemicals<br />

may react with the other.<br />

5. Aqueous solutions or mixed Organic <strong>Solvent</strong>s should be labeled with the solvent name(s) and approximate weight or<br />

volume percentage <strong>of</strong> each listed dissolved solid chemical component (i.e., 10%, 1%, 0.01%, less than 1%, etc.) if at all<br />

possible. For example:<br />

HAZARDOUS WASTE, Date 02-22-07<br />

) Water with:<br />

� Sodium iodide, approximately 5%<br />

� Ammonium chloride, 2-5%<br />

� Sodium sulfate, less than 1%<br />

� Sodium thiosulfate, less than 1%<br />

HAZARDOUS WASTE, Date 11-19-06<br />

) Two bottles <strong>of</strong> Acetone, Hexane, and Ethyl ether with:<br />

� Acetophenone, less than 1%<br />

� Anisole, less than 1%<br />

� Benzaldehyde, 10 %<br />

� Benzyl alcohol, trace amount<br />

� Benzoic acid, 20 %<br />

� Naphthalene, 2 to 5%<br />

The following common laboratory organic solvents can be poured into one <strong>of</strong> the two 55 gallon waste drums located in the solvent<br />

room, #20, labeled HAZARDOUS WASTE, Non-Sulfur, Non-Halogenated Organic <strong>Solvent</strong>s, meant <strong>for</strong> the following highly<br />

flammable, generally non-reactive hydrocarbons, commonly used in most academic research and teaching Labs:<br />

acetone methyl ethyl ketone pump oil<br />

benzaldehyde mineral spirits tetrahydr<strong>of</strong>uran<br />

benzene motor oil toluene<br />

cyclohexane naphtha xylenes<br />

ethyl ether paint thinner ethyl alcohol, (and,<br />

ethyl acetate petroleum ether low-molecular weight alcohols,<br />

heptane propanol (1 or 2-propanol) cyclohexanol, methanol )<br />

hexane propyl acetate ethylene glycol<br />

Dimethyl<strong>for</strong>mamide<br />

The two common halogenated organic solvents (methylene chloride and chloro<strong>for</strong>m, only) must be separated from other solvents<br />

and poured into labeled, 20 liter empty white polyethylene containers kept next to the large 55 gallon steel drums, on the floor in the<br />

wide yellow spill tray.<br />

48


All other organic solvents not on the list above must be poured into separate glass or metal containers, labeled, and placed on<br />

the metal table. This includes any potentially reactive or unstable liquid organic chemical. <strong>Example</strong>s would be sulfurcontaining<br />

compounds, complex heterocyclics, corrosives, organic acids, lachrymators, etc. - i.e., bromine, acetic anhydride,<br />

acetyl chloride, chlorosulfonic acid, pyridine, acetonitrile, alanine, 1,4-dioxane, tert-butyl chloride, etc.<br />

Common mineral acids used in Academic laboratories (Hydrochloric, Nitric, Sulfuric acids, including Acetic and Phosphoric acids)<br />

can be completely neutralized with Sodium carbonate or bicarbonate and flushed down the drain with plenty <strong>of</strong> cold water, unless<br />

other harmful chemical components are mixed in with them, in which case they should be securely bottled, capped, labeled, and sent<br />

out with the waste company.<br />

Research students in each research lab making use <strong>of</strong> chemicals and generating chemical waste are responsible <strong>for</strong> identifying and<br />

gathering chemical waste, putting them in appropriate empty glass or plastic containers (depending on the reactivity or lack there<strong>of</strong> <strong>of</strong><br />

the chemical with the type <strong>of</strong> container you‟re using), labeling them as described above, making sure there is no evidence <strong>of</strong> spillage<br />

on the container surface, storing the chemical waste temporarily in a designated storage area within your lab (ideally in a hood, or<br />

underneath a hood, or in a flammable storage cabinet), capping or otherwise closing the container tightly, making absolutely certain<br />

that different chemicals stored within the same container are chemically compatible (that is, do not react with each other), and finally<br />

that each bottle is dated when full and taken to the Hazardous Chemical Waste holding (Accumulation) area in the <strong>Solvent</strong> room # 20<br />

<strong>for</strong> eventual removal by the Chemical Waste Company. Faculty Research Directors and Faculty teaching Lab instructors are<br />

responsible <strong>for</strong> identifying chemical waste if Graduate students are unclear as to what constitutes chemical waste generated in their<br />

research or teaching laboratory work areas. Any other questions regarding chemical waste should be directed to Scott Frazier [WFU<br />

Assistant Environmental Health and Safety (EHS) Director], phone # 4255.<br />

It is hereby stipulated that each research laboratory group designate one graduate student to oversee the collection and transportation<br />

<strong>of</strong> chemical waste from the group‟s work area to the Accumulation area on the metal table or 55 gallon solvent waste drum in room<br />

#20. In particular, this designated person has the responsibility <strong>of</strong> visually checking the contents <strong>of</strong> each waste container be<strong>for</strong>e it is<br />

taken by other students within the group to the waste holding area, to make certain incompatible chemicals have not been placed in<br />

the same container, and dating each waste container when it is taken to the Accumulation area. This should be a permanent or<br />

rotating assignment, based on research priorities and faculty dictate.<br />

The designated Graduate Student or teaching assistant <strong>for</strong> your work area will maintain a Micros<strong>of</strong>t Word document listing <strong>of</strong> typical<br />

waste generated in your lab, which will be emailed to the Laboratory manager at mathomps@wfu.edu in your department when the<br />

waste is ready <strong>for</strong> removal to the <strong>Solvent</strong> room # 20.<br />

49


D. Protective Devices, Equipment, and Apparel<br />

1. Personal Protective Equipment: Eyewear<br />

1. All laboratory workers are required to wear safety glasses or goggles at all times in research and<br />

undergraduate laboratories. Departmentally available “Wraparound” safety glasses must be worn over<br />

prescription eyeglasses. Alternatively, you can purchase your own prescription-lens safety goggles, but be<br />

prepared to prove that they are actually fully rated as safety glasses.<br />

Contact lenses are not acceptable in most laboratory situations, especially around chemicals which<br />

readily generate vapors <strong>of</strong> any sort, i.e. volatile organic liquids or solids, corrosive mineral acids,<br />

lachrymators, solids with dust-like consistencies. These vapors easily become lodged underneath the<br />

contacts rendering removal difficult. Also, one cannot flush the eyes with water until they are physically<br />

removed. After accidentally splashing chemicals into the eyes, one cannot expect to remain panic-free<br />

while groping about <strong>for</strong> the eye-wash fountain and struggling with contact lenses. If contact lenses must be<br />

worn <strong>for</strong> some reason, cover your face with tight-fitting safety goggles. More elaborate eye protection,<br />

including full face shields, may be obtained from the chemistry stockroom (room #110).<br />

2. All undergraduate laboratory students are required to obtain safety glasses, goggles, or “Wraparound”<br />

goggles from the chemistry department stockroom (room #110) during check-in procedures. These must be<br />

kept and worn through each and every laboratory session. They should be returned at the end <strong>of</strong> the<br />

semester, during lab check-out procedures.<br />

Graduate students may obtain eyewear from the same room to be kept until graduation. In the<br />

event other types are desired, they may be purchased from Fisher Scientific Company (or anywhere else) by<br />

their Faculty research directors. Graduate students must obtain one com<strong>for</strong>table pair <strong>of</strong> safety glasses and<br />

one pair <strong>of</strong> tight-fitting safety goggles <strong>for</strong> use in more hazardous research lab operations.<br />

The standard safety glasses kept in the stockroom are AO Safety or Aerosite Fisher Brand (Fisher<br />

Catalog #17-981-9B or 10B, large or small size). These are safety spectacles, with permanently attached<br />

side shields, all in accordance with the relevant OSHA standard, 29 CFR 1910.133, which employs the same<br />

criteria <strong>for</strong> safety glasses stipulated by the American National Standards Institute (ANSI), referred to as<br />

standard Z87.1-1989. The goggles kept in the stockroom are UVEX Classic (Fisher Catalog #17-253 <strong>for</strong> one<br />

size) or UVEX Futura chemical splash goggles (Fisher catalog #17-260-1 small, and catalog #17-982-587<br />

large), all <strong>of</strong> which meet the Standard <strong>for</strong> Occupational and Educational Eye and Face Protection listed under<br />

29 CFR 1910.133. Cynmar Corporation makes catalog # 180-11090 Wraparound goggles.<br />

Specific in<strong>for</strong>mation regarding UV light protection in both the standard Departmental safety<br />

glasses and the safety googles can be obtained from the manufacturer by calling Fisher Scientific.<br />

50


2. Personal Protective Equipment: Lab Coats and Gloves<br />

1. The chemical laboratory is not the place <strong>for</strong> fashionable or impractical clothing. Wear sturdy cotton<br />

trousers or long skirts and thick, well-worn shirts with long sleeves. Some other resilient material may be<br />

just as good, but synthetic fabrics tend to melt when burned and adhere to skin. It is generally easy to end up<br />

with chemical stains on clothes during any serious lab work. Don your old blue jeans, wear lab coats when<br />

necessary, and keep your feet completely covered with leather or thick canvas shoes. Cotton lab coats are<br />

preferable, although other fabrics sold by Fisher Scientific Company are acceptable. Disposable aprons are<br />

available in the Chemistry Department Stockroom (room #110).<br />

2. Gloves: Wear disposable laboratory gloves when working with hazardous chemicals. Which type you<br />

choose to wear should be dictated by the general class <strong>of</strong> chemical you will be exposed to in the lab.<br />

Research lab gloves should be purchased by your research advisor. If your research advisor does not<br />

stipulate which type you should obtain or provide them <strong>for</strong> you then please procure them from the<br />

stockroom (room #110). They are described as follows:<br />

a) Lightweight Purple nitrile gloves (brand name Kimberly-Clark “Safeskin”, Fisher catalog # 19-149-<br />

863A through D, <strong>for</strong> sizes extra-small through extra-Large, $74.90 per case <strong>of</strong> 1000 as <strong>of</strong> 10-18-06)<br />

meant generally <strong>for</strong> organic solvents and solids and to a lesser extent, mineral acids. These gloves are<br />

also used <strong>for</strong> undergraduate Organic Chemistry, Chem 221-221L labs and are 4 "mils" thick (a "mil" is<br />

equal to 0.001 inch). A good substitute <strong>for</strong> these would be VWR, Inc., Microgrip Ambi-nitrile gloves<br />

(purple), catalog # 40101-344 (small) through 40101-346 (large). All <strong>of</strong> these are disposable gloves.<br />

b) Light-weight latex rubber <strong>of</strong>f-white and green gloves (Kimberly-Clark “Safeskin”, Fisher catalog #<br />

11-390-1A through D, <strong>for</strong> sizes extra-Small through extra-Large, $53.00 per case <strong>of</strong> 1000 as <strong>of</strong> 10-18-06)<br />

are best <strong>for</strong> mineral acids and inorganic salts and are used by undergraduate students in general<br />

chemistry labs, Chem 111-116L labs. They are 6 mils thick (again, 0.006 <strong>of</strong> an inch thick). THEY DO<br />

NOT STAND UP WELL TO ORGANIC SOLVENTS. A good substitute <strong>for</strong> these would be VWR, Inc.,<br />

Microgrip Latex gloves (blue-green, or teal), catalog # 40101-414 (small) through 40101-418 (large).<br />

Again, these are disposable. We also have SAFESKIN latex gloves (<strong>of</strong>f white), Fisher # 11-390-1A<br />

through 1E, which are 6 mils thick (again, 0.006 <strong>of</strong> an inch thick).<br />

c) Yellow, heavy-duty, universal, thick, cotton lined rubber gloves (ANSELL EDMONT Natural<br />

Rubber, Fisher catalog #11-394-7A through E, size 7-10). These are good overall protection <strong>for</strong> both<br />

graduate and undergraduates. They are more cumbersome than the lighter gloves described above. Do<br />

not use them if your skin is overly sensitive to cotton. These are meant to be reusable gloves. We also<br />

have slightly heavier duty orange ANSELL EDMONT Natural Rubber gloves, Fisher catalog # 11-391-<br />

145 [size 7], then 11-394-6B through 11-394-6D (<strong>for</strong> sizes small through large).<br />

d) Heavyweight, non-cotton lined, dark-green nitrile gloves (MAPA Pr<strong>of</strong>essional Stansolv Nitrile gloves,<br />

Fisher catalog #11-391-1A through E, size 7-11) are <strong>for</strong> people who may be allergic to cotton-lined<br />

gloves.<br />

e) "Multi-flex" powder-lined heavyweight green vinyl gloves, VWR Scientific Products (Baxter) catalog<br />

# G7235-3 or 4, <strong>for</strong> large or extra large sizes. Vinyl(or PVC) material stands up well to acids and<br />

alcohols, but not most organic solvents.<br />

f) "Zetex" brand temperature resistant gloves (non-asbestos material), Fisher catalog #11-392-15one size<br />

only.<br />

g) Neoprene Gloves <strong>for</strong> handling Hydr<strong>of</strong>luoric acid will be supplied by Scott Frazier [WFU Assistant<br />

Environmental Health and Safety (EHS) Director]. His phone # is 4329 (or 4224)<br />

Please read the section entitled "Hand Protection" on pages 132-3 <strong>of</strong> Prudent Practices, 2nd<br />

edition, and consult the glove selection charts kept in the Stockroom (room # 110) copy <strong>of</strong> The Chemical<br />

51


Hygiene Plan when choosing the appropriate gloves to wear in you laboratory situation. Choose the type <strong>of</strong><br />

gloves you need based on the kinds <strong>of</strong> chemicals with which you work. Some <strong>of</strong> the gloves described above<br />

are headed with a handwritten asterisk on the chart columns corresponding to the glove brand name or<br />

glove material.<br />

An extended glove compatibility chart is contained in the booklet entitled "Quick Selection Guide<br />

to Chemical Protective Clothing," 2nd edition, by Krister Forsberg and S.Z. Mansdorf, Van Nostrand<br />

Reinhold Publishers, kept by the laboratory manager.<br />

The "Calendar Guide to Chemical Resistant Best Gloves," 7th edition, lists chemical<br />

compatabilities <strong>for</strong> thicker, heavier-duty gloves than anything we have in stock above and are made <strong>of</strong> more<br />

chemically resistant material. You will find all pertinent in<strong>for</strong>mation <strong>for</strong> them in the Fisher Catalog or in<br />

the "Calendar Guide" chart by Best company.<br />

The Glove compatibility charts from Best Company can also be accessed from their Web site,<br />

http://www.bestglove.com/, go to the “industrial” glove sidebar, then to “chemical resistent”, then scroll<br />

down and download the red disk icon labeled “download chemrest Guide”, fill in and complete the required<br />

name and address fields (apparently <strong>for</strong> future guide update info), and the download the Windows 95<br />

option.<br />

For the Ansell heavy-duty yellow gloves chemical compatibility chart, go to<br />

http://www.ansellpro.com/<br />

For the MAPA Stansolv heavy-duty cotton-less, green nitrile gloves, go to<br />

http://www.mapaglove.com/<br />

The Safeskin (purple nitrile SHIELDMASTER) glove compatibility chart is also available on the<br />

Web. Go to:<br />

http://www.shieldmaster.com/ and then to:<br />

http://www.safeskin.com/chemresist/<br />

The following useful in<strong>for</strong>mation on gloves was obtained from Dartmouth College, Environmental<br />

Health and Safety, 6216 Clement West, Hanover, NH 03755, phone # 603-646-1762:<br />

“Glove materials:<br />

Viton� - Excellent resistance to chlorinated and aromatic solvents. (Expensive)<br />

Butyl - Good choice <strong>for</strong> aldehydes, ketones and esters. (Expensive)<br />

Neoprene - Wide range <strong>of</strong> resistance to solvents, acids, caustics and alcohols.<br />

Nitrile - Wide range <strong>of</strong> applications along with puncture and abrasion resistance.<br />

Natural rubber (latex) - resists acids and caustics. Often combined with other polymers <strong>for</strong> a broader range<br />

<strong>of</strong> applications.<br />

PVC - resists acids but not petroleum solvents.”<br />

52


3. VENTILATION AND PROPER USE OF HOODS<br />

1. Ventilation System<br />

Laboratory hoods serve as very convenient “designated areas” <strong>for</strong> working with dangerous<br />

chemicals and you should take advantage <strong>of</strong> them whenever you feel it necessary.<br />

The hoods in the Salem Hall are designed to keep the concentration <strong>of</strong> all airborne chemicals<br />

below the Threshold Limit Values (TLVs) or Permissible Exposure Limits (PELs) as defined by<br />

OSHA and explained in the subchapter <strong>of</strong> this manual titled “A Guide to OSHA Air Concentration<br />

Acronyms”. Active laboratory areas are constantly provided with 100% fresh air from the ventilation<br />

system, with the exception <strong>of</strong> laboratories in room #s 101, 103, 105, 107 and 109. The room #s 19 and 20<br />

have been given an entirely separate air-control system with 8 air changes per hour, again <strong>of</strong> 100% fresh air.<br />

The exhaust system <strong>for</strong> the building as a whole provides <strong>for</strong> complete separation <strong>of</strong> intake air from<br />

exhaust air. The two enormous fans on the ro<strong>of</strong> drive the exhaust air through the exit stacks approximately<br />

fifty feet upward, away from intake air openings.<br />

2. Supply air <strong>for</strong> all Laboratory Hoods<br />

The hoods located in all research laboratories <strong>of</strong> Salem Hall are “Kewaunee Hoodaire Airflow”<br />

fume hoods, <strong>of</strong> the Variable-volume non-bypass type. This means that the hoods are constructed to<br />

maintain a constant velocity air flow at the opening <strong>of</strong> the hood (face velocity) as one opens or closes the<br />

horizontal window-sashes. In a non-bypass hood, air is fed into the hood through the sash opening and<br />

through the air-foil only. Since the hoods empty air from the room at differing rates, as one opens or closes<br />

the sashes, air must be fed into the room at matching rates, or one cannot maintain even air flows.<br />

One make-up air valve is located above the ceiling tile in each research and newly renovated<br />

undergraduate lab. These “Phoenix Control” air valves track the exhaust valves above each hood and<br />

automatically adjust the make-up supply air <strong>for</strong> the room as the exhaust valve air volume changes.<br />

If you do not notice changes in the noise level <strong>of</strong> these valves when a majority <strong>of</strong> the sashes in the<br />

lab are closed or opened, the valve is functioning abnormally. Another indication, <strong>of</strong> course, is whether the<br />

air flow in the room is normal and unchanging as one opens and closes the sashes or whether the air<br />

pressure in the room feels normal as one opens or closes the door to the room. If the valves are obviously<br />

malfunctioning, call maintenance at Physical Facilities (phone # 4255). Call this number if any problem<br />

with the ventilation arises in research labs, undergraduate labs, or storage rooms.<br />

The Kewaunee hoods with vertical sashes, made from standard Kewaunee sash plate glass, are<br />

located in the back bench areas <strong>of</strong> the newly renovated undergraduate labs in room #s 102, 106 and 111<br />

(and soon to be in rooms 101 and 105). They are Kewaunee “Visionaire” brand by-pass hoods. They have<br />

face velocities <strong>of</strong> 60 feet per minute. These hoods are used <strong>for</strong> dispensing reagents to undergraduate labs<br />

and storage <strong>of</strong> hazardous waste.<br />

The small bench top hoods in the newly renovated undergraduate labs are Kewaunee “Visionaire<br />

View 2010” hoods, with polycarbonate safety shields, sidewall slots on the outer wall rims to reduce air<br />

turbulence at the face opening, and clear tops and sides to allow maximum visibility which working, thus<br />

encouraging the student to work inside the hood. The safety shield in front provides added protection.<br />

These constant volume individual station hoods were designed by Wake Forest University Chemistry<br />

Department faculty members and Kewaunee representatives. They have face velocities <strong>of</strong> about 30 to 40<br />

feet per minute.<br />

TLVs and PELs are safe air concentration levels based on 8 hour average workdays, 5 days a<br />

week. Since undergraduate students work an average <strong>of</strong> 4 hours one afternoon per week, their exposures<br />

are not likely in any case to exceed the PELs or TLVs <strong>of</strong> common laboratory chemicals. If one can smell a<br />

chemical, one has in most cases just reached the boundary line <strong>of</strong> concern and one should seek to make<br />

more efficient use <strong>of</strong> the nearest laboratory fume hood. Take the chemical you are working with and place<br />

it closer to or further back into the hood. Proper planning <strong>for</strong> lab experiments be<strong>for</strong>ehand, however, will<br />

take into consideration the need <strong>for</strong> working in a hood. You should not rely on smell as a safeguard against<br />

potential hazards. Some chemicals with low PELs can be hazardous at levels below the odor threshold.<br />

53


It cannot be overemphasized that the hoods in Salem Hall were designed to maintain all<br />

chemical exposures at levels below the permissible exposure limits (PELs) established by OSHA.<br />

When used properly, only accidents and spills will result in overexposures to chemicals.<br />

All research hood sashes have been replaced with “safety glass”. This glass will break into<br />

literally hundreds <strong>of</strong> relatively small round non-lacerating bits <strong>of</strong> glass when cracked during use. If<br />

explosions occur, the glass will actually partially absorb the shock in the process <strong>of</strong> breaking. When any<br />

breakage occurs, replacements are kept in room #8A. Please call Physical Facilities (phone #4255) <strong>for</strong><br />

installation.<br />

The research hoods have been physically placed in the room so as to minimize the effects <strong>of</strong><br />

traffic, i.e., walking in front <strong>of</strong> the hoods. Laboratory workers should nevertheless recognize that this<br />

causes a certain amount <strong>of</strong> turbulence in front <strong>of</strong> the hoods and disrupts the flow <strong>of</strong> air. Fumes will<br />

momentarily stretch outward from the hood if such traffic is severe. The air flow through the open sash is<br />

maintained at 100 feet per minute while the speed <strong>of</strong> walking is about 3 miles per hour (or 250 feet per<br />

minute). There is no law stipulating a certain air flow rate in the hoods, but it required that we adhere to<br />

published standard recommendations, as follows (As advised by Dr. Haugen, we will adhere to NFPA 45<br />

and ANSI/AIHA Z9.5 standard recommendations, <strong>for</strong> flow rates between 80 and 120 feet per minute – We<br />

keep the research lab hoods set at 100 feet per minute):<br />

PUBLISHED FACE VELOCITY RECOMMENDATIONS<br />

Compiled by Dr. Bob Haugen, (Kewaunee Scientific Corporation, Laboratory Division, PO Box 5400,<br />

Statesville, NC 28687, phone # 704-871-3214):<br />

Organization Citation Face Velocity<br />

1) ACGIH Industrial Ventilation 19 th edition p.5.24 60-100 FPM<br />

2) ASHRAE 1999 ASHRAE Handbook, 13.5 20%-50% <strong>of</strong> exterior<br />

disturbance velocities. (60-<br />

175 FPM) if 300 FPM<br />

walkby used to calculate)<br />

3) ANSI/AIHA ANSI/AIHA Z9.5, Sect 5.7 80-120 FPM<br />

4) CALOSHA CCR Title VIII, Subchapter 7.5454.1 Min 100 FPM<br />

5) Nat. Rsrch.Cnc. Prudent Practices, p.178 80-100 FPM<br />

6) NFPA NFPA 45: 6-4.5 & A6-4.5 "Sufficient to prevent<br />

escape from hood; 80-120<br />

FPM;<br />

40 CFM/lin foot min<br />

7) NIOSH Recommended Indust. Ventil. Gudelines p166 100-150 FPM<br />

8) NRC NRC Guide, 6.3 100 FPM <strong>for</strong> hospital<br />

radioactives<br />

9) OSHA 29 CFR 1910 Appendix A Sec. A.C.4.g 60-100 FPM<br />

10) SEFA SEFA 1.2: 5.2 75-100 FPM<br />

54


3. Preliminary Considerations <strong>for</strong> Safe Operation <strong>of</strong> Hoods<br />

All hoods in Salem Hall have air slots in the back (bottom, mid, and top) to allow passage <strong>of</strong> air<br />

from the “face” <strong>of</strong> the hood straight through to the back surface and out. The larger hoods have airfoils,<br />

which prevent vertical displacement and guide the air horizontally. Air flow is much smoother if the slots<br />

are not blocked by packing the hoods with everything imaginable. Do not overcrowd these hoods. Air<br />

flows will be much smoother if equipment is raised 2 or 3 inches with support racks, lab jacks, or makeshift<br />

raised plat<strong>for</strong>ms. The degree <strong>of</strong> air flow (referred to as “face velocity”) is not in itself an adequate measure<br />

<strong>of</strong> hood efficiency. High flow rates <strong>of</strong> 100 - 150 feet per minute through hoods which are packed with<br />

extraneous equipment, bottles, unnecessary chemicals, etc., only create high air turbulence and do not<br />

operate as hoods, but rather as “expensive fans.”<br />

The cabinets upon which these hoods rest contain venting holes leading to the hood. There<strong>for</strong>e,<br />

THESE CABINETS ARE IDEAL FOR STORAGE OF TOXIC OR OTHERWISE ODORIFEROUS<br />

CHEMICALS. They also are lined with firepro<strong>of</strong> material. The hoods are in continual operation - they are<br />

never turned <strong>of</strong>f, unless there is a building ventilation shutdown, in which case you should evacuate your lab<br />

if you are working with chemicals in the hoods or storing toxic chemicals below them in the storage<br />

cabinets.<br />

OSHA recommends 2.5 linear feet <strong>of</strong> hood space per worker if they spend most <strong>of</strong> their time<br />

working with chemicals. Our research hoods have 3.5 linear feet per research student. The newly<br />

renovated undergraduate laboratory hoods have 2 linear feet <strong>of</strong> hood space per student, each <strong>of</strong> whom will<br />

spend at most 6 hours per week working with a hood. These undergraduate hoods are built much better<br />

than most academic undergraduate hoods in other universities.<br />

All electrical outlets, light switches, water and gas valves are located just outside <strong>of</strong> the research<br />

hood chamber. The hood sashes SHOULD BE CLOSED when not in use, to save energy and cut down on<br />

the expense <strong>of</strong> air maintenance. All hoods in Salem Hall will be inspected periodically and certified when<br />

possible.<br />

4. Hood Air Flow Monitors<br />

All research laboratories, including one undergraduate teaching laboratory in room #7, the physical<br />

chemistry lab, contain Phoenix Control Corporation Fume Hood Monitors. These monitors electronically<br />

monitor the flow rate through your hoods and sound alarms when the flow rate falls below 70 feet per<br />

minute. This indicates that you should evacuate the lab, unless there is merely a temporary malfunction <strong>of</strong><br />

the monitoring device itself. Read and follow the operating procedure <strong>for</strong> these monitors which follows this<br />

section.<br />

The monitor also regulates the air flow as sash doors are opened and closed during use. Horizontal<br />

bar magnet sensors, located on top <strong>of</strong> the sashes and electrically connected to the Phoenix monitors,<br />

increase the flow rate through the sash opening as the sash opening widens to a maximum flow rate <strong>of</strong> 100<br />

linear feet per minute. As the door closes, the rate decreases to a minimum <strong>of</strong> 70 feet per minute. During<br />

an emergency requiring a much higher air flow, such as a runaway reaction generating clouds <strong>of</strong> toxic<br />

vapors, an emergency button can be depressed on the monitor to activate a sudden increase to 120 feet per<br />

minute flow, simultaneously sounding an alarm. The mute button can then be depressed to silence the alarm<br />

while maintaining the higher flow rate. Press the red emergency button again to return the flow to its<br />

normal rate.<br />

The large Kewaunee “Visionaire” hoods, located in back <strong>of</strong> the newly renovated undergraduate<br />

hoods, also contain air flow monitors. The air-flow rate is 60 feet per minute. When the air flow falls<br />

below this level, the Kewaunee “Air Alert 300” fume hood monitor will sound an alarm, indicating that<br />

the flow rate will no longer maintain concentrations below the permissible exposure limits <strong>for</strong> hazardous<br />

chemicals in the hood.<br />

The green light on the monitor indicates normal air flow. When the air flow falls to a lower level,<br />

a red alarm indicator light will flash and the alarm will sound. Please see the following diagram and<br />

accompanying directions <strong>for</strong> use. IF ANY PROBLEM IS ENCOUNTERED WITH HOOD<br />

MONITORING EQUIPMENT, WIRING, SASH SENSORS, OR HOOD AIR FLOW IN GENERAL,<br />

STOP WORKING AND CONTACT THE LAB MANAGER AND CALL PHYSICAL FACILITIES<br />

(PHONE #4255).<br />

55


For repairs <strong>of</strong> Phoenix Control Monitors, call Mr. Dean Dray <strong>of</strong> Hahn-Mason Air Systems, Inc.,<br />

Service Division, 410 Oberlin Road, Suite 350, P.O. Box 10465, Raleigh, NC 27605, phone # 1-919-834-<br />

9230. Air-flows can be recalibrated by Mr. Tommy York, or other WFU Physical Facilities personnel.<br />

5. Hoodaire Airflow Fume Hoods Operating Instructions, posted as labeled instructions on each research<br />

hood as follows (Kewaunee Scientific Corporation, Laboratory Division, PO Box 5400, Statesville, NC<br />

28687, phone # 704-871-3214):<br />

a. “Prior to using hood, check to make sure that exhaust fan is operating and that air is entering<br />

the hood<br />

b. Never use perchloric acid in a hood not specifically designed <strong>for</strong> perchloric acid use. Also,<br />

never use a perchloric acid hood <strong>for</strong> other purposes.<br />

c. Avoid placing head inside hood. Keep hands outside <strong>of</strong> hood as much as possible.<br />

d. Always work as far back in hood as possible. In particular avoid fume emission in front 6” <strong>of</strong><br />

hand opening area.<br />

e. Normally, rear baffle adjustment strips should be set with bottom slot full open and top slot<br />

approximately 1/2 open. However, <strong>for</strong> special conditions, slots should be adjusted to provide<br />

the flow <strong>of</strong> air desired. <strong>Example</strong>: <strong>for</strong> high heat loads at hood working surfaces, bottom slot<br />

should be closed and top slot should be fully open.<br />

f. <strong>Use</strong> good housekeeping in hood at all times. Clean up spills immediately. Periodically clean<br />

hood interior including fluorescent light glass panel. Replace burned out light bulbs to<br />

maintain maximum illumination.<br />

g. If corrosive or volatile materials are stored inside hood, hood exhaust system must be in<br />

operation.<br />

h. Avoid blocking <strong>of</strong>f baffle exhaust slots in any manner.<br />

i. Where possible, maintain sash position at lowest practicable working level.<br />

j. Avoid cross drafts and excessive personnel passage in front <strong>of</strong> hoods. Air disturbances so<br />

created may draw fumes out <strong>of</strong> hood.<br />

k. Periodically check air flow velocity through hood using a source <strong>of</strong> visible smoke. If air flow<br />

has decreased in velocity, check exhaust fan, ductwork, etc., to determine cause.<br />

l. Do not place large, bulky objects directly on hood working surface, block up 2” to 3” to allow<br />

a flow <strong>of</strong> air under the object and into lower rear baffle exhaust slot <strong>of</strong> hood.<br />

m. Do not remove deflector vane nor block <strong>of</strong>f the opening between the underside <strong>of</strong> the vane and<br />

the work top.”<br />

56


OPERATING INFORMATION FOR FHM 400 FUME HOOD MONITORS<br />

LOCATED ON RESEARCH LAB HOODS AND TWO UNDERGRADUATE<br />

HOODS IN THE PHYSICAL CHEMISTRY LAB IN ROOM #7<br />

- Green light indicates hood is safe to use<br />

- Red lights indicate danger - hood is not safe.<br />

Call Maintenance at phone #4255, ask <strong>for</strong> Donnie Adams, building zone<br />

supervisor<br />

- No lights indicate loss <strong>of</strong> power. Call maintenance at phone #4255<br />

- For malfunctions <strong>of</strong> monitor or hood sash sensor bar magnets, located on top <strong>of</strong> the<br />

glass sash doors, and crimped or broken sash sensor wires leading to the monitor, call<br />

Mr. Dean Dray, monitor service engineer, Hahn-Mason Air Systems, Inc., 612 West<br />

Lane Street, Raleigh NC, phone # 919-834-9230<br />

CAUTION-LOW FACE VELOCITY<br />

ALARM LIGHT (RED)<br />

Indicates unsafe airflow condition.<br />

An alarm will sound and red light<br />

will come on and blink. Immediately<br />

close sash and call maintenance at<br />

phone #4255. DO NOT USE HOOD<br />

CAUTION-HIGH FACE VELOCITY<br />

ALARM LIGHT (RED)<br />

Indicates the emergency high face<br />

velocity exhaust mode is activated.<br />

The red light is on and blinking.<br />

EMERGENCY EXHAUST<br />

BUTTON (RED)<br />

USE WHEN A HAZARDOUS<br />

MATERIAL SPILL OCCURS IN<br />

HOOD OR NEARBY LAB AREA..<br />

Push this button to activate the<br />

emergency exhaust mode. An alarm<br />

will sound. In this mode exhaust air<br />

is at its maximum flow to rapidly<br />

evacuate the hood. (The red light in<br />

the switch indicates the switch is<br />

turned on). Push the button again to<br />

turn <strong>of</strong>f the emergency exhaust<br />

mode.<br />

FUME HOOD MONITOR<br />

CLOSE SASH DOORS TO SAVE ENERGY<br />

AND IMPROVE SAFETY<br />

EMERGENCY<br />

EXHAUST<br />

SYSTEM NORMAL<br />

CAUTION* Low Face Velocity<br />

CAUTION High Face Velocity<br />

RESET MUTE<br />

*Indicates Majority <strong>of</strong> Low Flow Conditions<br />

Automatic Constant Face Velocity <strong>for</strong> Safety<br />

PHOENIX CONTROLS CORPORATION<br />

FHM 400 Model<br />

SYSTEM NORMAL LIGHT<br />

(GREEN)<br />

Indicates normal operation <strong>of</strong> fume<br />

hood. This light must be on <strong>for</strong><br />

safe use <strong>of</strong> the hood<br />

MUTE SWITCH(GRAY)<br />

Audible alarms are energized on any<br />

<strong>of</strong> the following conditions:<br />

- CAUTION ALARM<br />

- EMERGENCY EXHAUST<br />

Push the button to silence alarm.<br />

Alarm status lights will remain lit.<br />

The mute mode is reset<br />

automatically after alarm conditions<br />

clear<br />

57


OPERATING INFORMATION FOR FHM 410 FUME HOOD MONITORS<br />

LOCATED ON RESEARCH LAB HOODS<br />

- Green lights indicate hood is safe to use.<br />

- Red lights indicate danger -- hood is not safe. Call maintenance at phone<br />

#4255, ask <strong>for</strong> Donnie Adams, Building Zone Supervisor.<br />

- No lights indicate loss <strong>of</strong> power. Call maintenance at phone #4255.<br />

EMERGENCY EXHAUST<br />

LIGHT (RED)<br />

Indicates the emergency exhaust<br />

mode is activated. See Emergency<br />

Button below <strong>for</strong> an explanation <strong>of</strong><br />

the Emergency Exhaust Mode.<br />

EMERGENCY BUTTON (RED)<br />

USE WHEN A HAZARDOUS<br />

MATERIAL SPILL OCCURS IN<br />

HOOD OR NEARBY LAB<br />

AREA.<br />

Push this button to activate the<br />

emergency exhaust mode. An<br />

alarm will sound. In this mode<br />

exhaust air is at its maximum flow<br />

to rapidly evacuate the hood. (The<br />

red light in the switch indicates the<br />

switch is turned on). Push the<br />

button again to turn <strong>of</strong>f the<br />

emergency exhaust mode.<br />

FUME HOOD MONITOR<br />

SYSTEM STATUS<br />

STANDBY OPERATION<br />

-NORMAL-<br />

STANDARD OPERATION<br />

EMERGENCY EXHAUST<br />

CAUTION - FLOW ALARM<br />

EMERGENCY MUTE<br />

Automatic constant Face Velocity <strong>for</strong> Safety<br />

PHOENIX CONTROLS CORPORATION<br />

FHM 410 Model<br />

NORMAL LIGHTS (GREEN)<br />

Indicates normal operation <strong>of</strong><br />

fume hood. One <strong>of</strong> these lights<br />

must be on <strong>for</strong> the hood to be safe<br />

to use.<br />

Standard Operation: system<br />

operating at standard face<br />

velocity<br />

Standby Operation: system<br />

operating at a lower face velocity<br />

(active only with Zone Presence<br />

Sensor, which are not presently<br />

installed).<br />

CAUTION FLOW ALARM<br />

LIGHT (RED)<br />

Indicates unsafe airflow<br />

condition. An alarm will sound.<br />

Immediately close sash and call<br />

maintenance at phone #4255.<br />

DO NOT USE THE HOOD.<br />

MUTE SWITCH (GRAY)<br />

Audible alarms are energized on<br />

any <strong>of</strong> the following conditions:<br />

- CAUTION - FLOW ALARM or<br />

- EMERGENCY EXHAUST<br />

Push the button to silence alarm.<br />

Alarm status lights will remain<br />

lit. The mute mode is reset<br />

automatically after alarm<br />

conditions clear.<br />

58


6. Visionaire or Supreme Air hood operating instructions, located in the rear <strong>of</strong> undergraduate<br />

laboratories on the first floor, room #s 102, 106 and 111, posted as a black label on the front <strong>of</strong> the<br />

hood by Kewaunee Scientific Corporation.<br />

“CAUTION: VISIONAIRE OR SUPREME AIR KEWAUNEE HOOD.<br />

BEFORE USING THIS HOOD, READ KEWAUNEE’S “RECOMMENDED WORK PRACTICES FOR<br />

LABORATORY FUME HOODS,” [Summarized below on the label, although the full text is available in the<br />

Departmental Chemical Hygiene Plan.]<br />

“Failure to follow these procedures may result in overexposure to contaminants or other injury.<br />

1. “Do not use Perchloric Acid in this hood. Perchloric Acid may create an explosion hazard<br />

2. Prior to using hood, verify that the exhaust fan is operating and sufficient air is being exhausted from<br />

hood.<br />

3. Never put head into hood while contaminants are being generated.<br />

4. Set up all apparatus and sources <strong>of</strong> contaminants at least 6” back from sash opening and in recessed<br />

portion <strong>of</strong> work surface.<br />

5. Do not place electrical receptacles or other sources <strong>of</strong> ignition in hood when flammables are present.<br />

6. <strong>Use</strong> a safety shield if there is a possibility <strong>of</strong> a small explosion or runaway reaction. This hood is not<br />

designed <strong>for</strong> explosion protection.<br />

7. Do not obstruct slots in rear baffle.<br />

8. Do not remove bottom deflector vane nor block <strong>of</strong>f opening between the underside <strong>of</strong> deflector vane<br />

and the worktop.<br />

9. Place equipment with large flat surfaces parallel to hood face on legs 2” to 3” high.<br />

10. While working at hood, keep sash lowered to minimum opening required <strong>for</strong> access to working area.<br />

During other times, keep sash closed.<br />

11. Wear gloves and other protective clothing if skin contact with airborne contaminants is a hazard.<br />

Other important data:<br />

A. Remove all materials from hood which are not needed <strong>for</strong> the immediate work.<br />

B. Do not store chemicals in hood.<br />

C. Avoid making rapid movements while working at hood.<br />

D. Minimize personnel traffic past hood.<br />

E. Avoid creating air currents in the laboratory which affect the air flow patterns into the hood.<br />

F. <strong>Use</strong> good housekeeping in hood at all times. Clean up spills immediately.<br />

G. Test the per<strong>for</strong>mance <strong>of</strong> hood at least once every six months.<br />

H. In models with removable sash, always replace sash be<strong>for</strong>e operating.”<br />

59


“GENERAL DESCRIPTION OF AIR ALERT 300 KEWAUNEE HOOD MONITOR FOR KEWAUNEE<br />

“VISIONAIRE” HOODS”<br />

(from Kewaunee's Air Alert Technical Note, Kewaunee Scientific Corporation, Laboratory Division, PO<br />

Box 5400, Statesville, NC 28687)<br />

“The Kewaunee AIR ALERT 300 alarm is designed to continuously monitor air flow through fume hoods.<br />

This permanently installed device provides both visual and audible alarms to alert the user <strong>of</strong> abnormal air<br />

flow conditions, after the instrument is calibrated <strong>for</strong> the particular installation. A green light on the front<br />

<strong>of</strong> the monitor indicates normal flow conditions <strong>of</strong> 60 fpm. When flow conditions lower than 60 fpm are<br />

encountered, a red light is activated along with an audible alarm. A test button is provided at the front <strong>of</strong><br />

the monitor to allow the user to check the operation <strong>of</strong> the alarm. See the following description <strong>of</strong> each key<br />

function located on the front <strong>of</strong> the monitor.”<br />

3<br />

4 AIR ALERT 300 1<br />

TEST 5<br />

RESET<br />

6 2<br />

Description <strong>of</strong> Features on Front <strong>of</strong> Monitor<br />

KEWANEE<br />

1. Air Inlet A portion <strong>of</strong> the air coming into the hood passes through the air inlet and across<br />

sensors.<br />

2. Adjustment <strong>for</strong> This potentiometer is used to set the low flow indicators.<br />

alarm set point<br />

3. Normal flow This green light indicates normal flow conditions.<br />

indicator<br />

4. Alarm Indicator This red light is activated approximately six seconds after the low flow set point<br />

is reached.<br />

5. Test/Reset If no alarm is present, this button will cause the read lamp to light, and the<br />

button audible alarm to sound. If an alarm is present, this button will silence the<br />

audible alarm.<br />

6. Power on This light stays on to indicate power is on.<br />

indicator<br />

60


4. Chemical Storage in Research Labs<br />

Make an ef<strong>for</strong>t to use up bottles <strong>of</strong> a particular chemical you already have in your lab be<strong>for</strong>e<br />

buying a new one, or be prepared to deal with old chemicals which have a short shelf life or decompose<br />

slowly upon prolonged standing. Some, such as deliquescent compounds, tend to absorb large amounts <strong>of</strong><br />

water after prolonged storage. Several organic liquids tend to polymerize, becoming useless as laboratory<br />

reagents. See the “Standard Operating Procedure <strong>for</strong> All Labs <strong>of</strong> Salem Hall” section <strong>of</strong> this manual <strong>for</strong><br />

dealing with ancient material which may have <strong>for</strong>med harmful peroxides.<br />

* Take the trouble to periodically examine old chemical containers <strong>for</strong> cracks or other signs <strong>of</strong> wear<br />

and tear. The original manufacturers label should remain intact, with rein<strong>for</strong>cing tape applied if necessary.<br />

Graduate students and undergraduate chemical preparation personnel should make an attempt to print the<br />

receiving date <strong>for</strong> each chemical which arrives in Salem Hall.<br />

* See Prudent Practices, 2nd Edition, Table 4.1, Page 73, <strong>for</strong> guidance in storing chemicals in<br />

compatible groups based on their mutual reactivity. PLEASE MAKE AN ATTEMPT TO SHELVE YOUR<br />

LABORATORY CHEMICALS ACCORDING TO THIS SCHEME. ALSO, CONSULT TABLE 3.9,<br />

PAGE 52 OF Prudent Practices, 2nd Edition, AND USE THIS AS YOUR GUIDE FOR KEEPING<br />

INCOMPATIBLE CHEMICALS SEPARATED FROM EACH OTHER ON STORAGE SHELVES. Note<br />

also the excellent advice appearing beneath this table, i.e., that “separation <strong>of</strong> chemical groups can be by<br />

different shelves within the same cabinet” and “Do Not store chemicals alphabetically as a general group.<br />

This may result in incompatibles appearing together on a shelf. Rather, store alphabetically within<br />

compatible groups.”<br />

Research laboratory shelves in Salem Hall have been embellished with transparent lexan sideguard<br />

strips to prevent accidental spillage <strong>of</strong> bottles when reaching <strong>for</strong> them.<br />

Large amounts (over one liter) <strong>of</strong> flammable organic solvents should be kept in yellow metal<br />

storage cabinets or in designated wooden cabinets lined with firepro<strong>of</strong> material in the research laboratories.<br />

These cabinets should not be vented. Remember that open containers <strong>of</strong> such liquids are very dangerous<br />

around sources <strong>of</strong> heat. The vapors <strong>of</strong> these liquids tend to be heavier than air, gathering in concentrated<br />

levels on bench tops, corners, and recesses in the lab work area. Operating electrical equipment, spark<br />

generating electrical switches, open flames, and warm heating mantels are potential sources <strong>of</strong> solvent fume<br />

generated fires. There<strong>for</strong>e, make every ef<strong>for</strong>t to keep such containers tightly capped. Open them, in so far<br />

as is possible, in hoods. Keep them away from any sources <strong>of</strong> ignition.<br />

The fifty-five gallon acetone drum in the solvent room # 20 is fitted with a grounding cable. If you<br />

have metallic acetone containers which you use <strong>for</strong> acetone storage, be sure to attach one end <strong>of</strong> the wire to<br />

the can be<strong>for</strong>e pouring out liquid from the 55 gallon drum into the can, thus equalizing the static electrical<br />

charge between the storage can and the drum. This will prevent a spark from starting a solvent fire. Cold<br />

winter days with low humidity content favor conditions <strong>of</strong> such discharge <strong>of</strong> static electricity.<br />

Instead <strong>of</strong> metallic cans <strong>for</strong> organic solvents, non-metallic polyethylene safety storage containers<br />

<strong>of</strong> one or two liter size ,such as “Justrite” brand, can be obtained from Fisher Scientific Co. (Fisher Catalog<br />

# 17-177B). See page 96 <strong>of</strong> Prudent Practices, 2nd edition, <strong>for</strong> more elaboration. Such containers have<br />

the advantage <strong>of</strong> less breakage potential.<br />

61


In addition to the guidance listed above, the following storage rules should be followed in all labs:<br />

� Water reactive chemicals (i.e. sodium metal, lithium aluminum hydride, etc.) should not be stored<br />

near a source <strong>of</strong> water, such as faucets, sinks, fire sprinklers, safety showers, etc.<br />

� Corrosive chemicals (i.e., mineral acids) should not be stored above shoulder level on lab benches. It<br />

is not a good idea to store any chemical on high shelves, out <strong>of</strong> com<strong>for</strong>table reach.<br />

� Make certain that all bottles <strong>of</strong> chemicals are labeled<br />

� Attempt to segregate chemicals into definite areas <strong>of</strong> storage as outlined above and return them there<br />

when finished with them.<br />

� When tempted to store chemicals in hoods, remember that the cabinets beneath are vented and will<br />

serve just as well, leaving you with a safer work area in the hood.<br />

� Do not store highly volatile, flammable chemicals in a refrigerator unless it contains a spark pro<strong>of</strong><br />

thermostat (i.e., unless it is an explosion pro<strong>of</strong> refrigerator!)<br />

� Periodically check the chemicals in your laboratory to make certain they are tightly capped! Prolonged<br />

storage <strong>of</strong>ten results in caps gradually working loose. Parafilm can be used in some cases to further airlock<br />

the container.<br />

� Store lecture bottles <strong>of</strong> compressed gases in the bottom vented cabinets <strong>of</strong> research lab hoods.<br />

62


E. Laboratory Operations which require prior approval from Chemistry<br />

Department Instructors<br />

Certain laboratory operations or chemicals are so dangerous that it is unwise to allow<br />

inexperienced personnel access to them unless subjected to constant scrutiny and direct supervision. Prior<br />

approval to proceed with a laboratory task shall be obtained by research and undergraduate students from<br />

their particular research directors or teachers under the following circumstances. Please note that specific<br />

instructions by teachers to engage in these activities while under their guidance in teaching laboratories<br />

constitutes such approval.<br />

Obtain approval be<strong>for</strong>e any use or synthesis whatsoever <strong>of</strong> perchlorate salts. These compounds<br />

tend occasionally to spontaneously detonate. Every ef<strong>for</strong>t must be made to obtain as much in<strong>for</strong>mation<br />

regarding their stability as possible by the research director be<strong>for</strong>e work begins.<br />

Obtain approval be<strong>for</strong>e ever using Hydr<strong>of</strong>luoric acid. Laboratories using this material should have<br />

access to a supply <strong>of</strong> a commercial HF skin treatment, a 0.13% solution <strong>of</strong> ZEPHIRAN CHLORIDE, the<br />

systematic name <strong>of</strong> which is Benzalkonium chloride, and must have multiple tubes <strong>of</strong> 2.5% Calcium<br />

gluconate gel in the work area and approved Neoprene gloves <strong>for</strong> both lab workers and emergency<br />

personnel in well marked and easily noticed storage. They must also have access to the Air Products<br />

publication Safetygram 29 titled “Treatment Protocol <strong>for</strong> Hydr<strong>of</strong>luoric Acid Burns.” One is kept near<br />

the departmental copy <strong>of</strong> the Chemical Hygiene Plan in the stockroom, room # 110, along with ordering<br />

in<strong>for</strong>mation <strong>for</strong> Calcium gluconate. All this material is also kept in Research Lab room 117.<br />

Obtain approval be<strong>for</strong>e use <strong>of</strong>:<br />

1. Peroxides <strong>of</strong> any kind<br />

2. Metallic mercury<br />

3. Picric acid<br />

4. Water reactive chemicals (see Prudent Practices, 2nd edition, page 51, and the table on the<br />

next page <strong>of</strong> this manual).<br />

5. Pyrophoric chemicals (see Prudent Practices, 2nd edition, page 51, and the table on the next<br />

page <strong>of</strong> this manual. Also see the Standard Operating Procedures <strong>for</strong> working with<br />

Pyrophorics on page 98 <strong>of</strong> this manual)<br />

6. Any <strong>of</strong> the following gasses, during installation <strong>of</strong> regulators or actual use: (listed in Prudent<br />

Practices, 2 nd edition, page 105).<br />

Boron halides chlorine<br />

Chlorine trifluoride Bromine<br />

Hydrogen selenide Phosphine<br />

Methyl chloride Phosgene<br />

Silane Ammonia<br />

Silyl halides Hydrogen chloride<br />

Fluorine<br />

7. Hydrogenation reaction apparatus, X-Ray crystallography defractometers, atomic absorption<br />

spectrometers, pressurized glove boxes.<br />

8. Fuming Nitric or Sulfuric acid 9. Potassium cyanide<br />

63


“This table lists some chemicals that react violently with water. They should be handled and<br />

stored away from both water and water vapor.<br />

Water Reactive Chemicals and Compounds<br />

“Alkali metals, such as Sodium (Na), Potassium, (K), Lithium (Li)<br />

Alkali metal hydrides and alkali metal amides, like Lithium aluminum hydride (LiAlH4) or sodium amide<br />

(NaNH2)<br />

Metal alkyls, such as lithium alkyls, aluminum alkyls, and magnesium alkyls (Grignard reagents)<br />

such as butyllithium, triethylaluminum, phenylmagnesium bromide in ethyl ether, etc.<br />

Acid halides <strong>of</strong> nonmetals, such as Boron trichloride (BCl3), Boron trifluoride (BF3), Phosphorus<br />

trichloride (PCl3), Phosphorus pentachloride (PCl5), Sulfur chloride (S2Cl2), Tetrachlorosilane, or Silicon<br />

tetrachloride (SiCl4)<br />

Inorganic acid halides, such as Phosphorus oxychloride (POCl3), Thionyl chloride (SOCl2), Sulfuryl<br />

chloride, or Sulfur oxychloride (SO2Cl2), and Phosphorus pentoxide, or Phosphoric anhydride (P2O5)<br />

Calcium carbide (CaC2)<br />

Organic acid halides and anhydrides <strong>of</strong> low molecular weight, like acetyl chloride and acetic anhydride<br />

Anhydrous metal halides <strong>of</strong> Aluminum (Al), Arsenic (As), Iron (Fe), Phosphorus (P), Sulfur (S), Antimony<br />

(Sb), Silicon (Si), Tin (Sn), Titanium (Ti), Zirconium (Zr) such as Aluminum Chloride (AlCl3), Titanium<br />

trichloride (TiCl3) (very reactive), Titanium dichloride (TiCl2) (much less reactive), Zirconium<br />

tetrachloride (ZrCl4), Stannic chloride (SnCl4)<br />

Metal hydrides <strong>of</strong> Aluminum (Al), Boron (B), Calcium (Ca), Potassium (K), Lithium (Li), Sodium (Na), like<br />

Sodium Hydride (NaH), Lithium Hydride (LiH), Aluminum Hydride (AlH3)”<br />

“This table lists some chemicals that oxidize readily and ignite spontaneously in air. These<br />

materials should be stored in tightly closed containers under an inert atmosphere or liquid.<br />

Pyrophoric Chemicals<br />

“Alkali metals, such as Sodium (Na), Potassium (K), Lithium (Li)<br />

Grignard reagents (RMgX), R=alkyl, X=Halides, like phenylmagnesium bromide<br />

Metal alkyls and aryls, such as alkyl Lithium (RLi), alkyl Sodium (RNa), alkyl Aluminum (R3Al), alkyl Zinc<br />

(R2Zn), (ie., tributylaluminum, butyllithium, etc.)<br />

Metal powders, such as Aluminum (Al), Cobalt (Co), Iron (Fe), Magnesium (Mg), Manganese (Mn),<br />

Palladium (Pd), Platinum (Pt), Titanium (Ti), Tin (Sn), Zinc (Zn), Zirconium (Zr)<br />

Metal hydrides, such as Sodium hydride (NaH), Lithium aluminum hydride (LiAlH4)<br />

Non-metal hydrides, such as Diborane (B2H6) and other boranes, Phosphene (PH3), Arsine (AsH3)<br />

Non-metal alkyls, such as alkyl Boron (R3B), alkyl Phophorus (R3P), alkyl Silver (R3Ag)<br />

Phosphorus (white)”<br />

(Both tables from Bowman Gray School <strong>of</strong> Medicine’s Chemical Waste Disposal: Policies and Procedures, 1985, pages IV 3-4)<br />

64


F. Provisions <strong>for</strong> Additional Protection When Working with Particularly<br />

Hazardous Chemicals<br />

The OSHA Laboratory Standard, besides stipulating that a Chemical Hygiene Plan be written <strong>for</strong> each lab,<br />

requires you to be particularly <strong>care</strong>ful in handling what are referred to as "particularly hazardous<br />

chemicals." These include "select" carcinogens, reproductive toxins, and substances which have a high<br />

degree <strong>of</strong> acute toxicity.<br />

"Select" carcinogens are defined in 29 CFR 1910.1450(b), as indicated on page 221 <strong>of</strong> Prudent<br />

Practices, 2nd edition. See also page 203 <strong>of</strong> that monograph, section 9.C.4, <strong>for</strong> a more elaborate<br />

description <strong>of</strong> regulated reproductive toxins and highly toxic substances. Please note that newly synthesized<br />

chemicals in research laboratories are considered highly toxic until proven otherwise.<br />

Each particularly hazardous chemical will be identified as such <strong>for</strong> you within the Chemistry<br />

Department’s MSDS sheet Inventory, on the sheet itself, written by the manufacturer <strong>of</strong> the chemical in<br />

question.<br />

It is advisable to gather all "select" carcinogens which are present in your laboratory, label them<br />

with yellow tape marked "Danger: Chemical Carcinogen" (commercially available), and store them in a<br />

designated storage area <strong>for</strong> carcinogens in your lab, preferably a hood or a safe storage cabinet.<br />

All reproductive toxins in your inventory should be labeled with commercially available orange<br />

tape marked "Danger: Mutagen or Teratogen.” You would be well advised to store these in the same<br />

storage area <strong>for</strong> carcinogens, although it may not always be possible to identify all <strong>of</strong> your teratogens since<br />

published lists <strong>of</strong> these compounds are less specific than lists <strong>of</strong> carcinogens.<br />

Highly Acute Toxic Chemicals have been listed <strong>for</strong> you in your inventory, via HMIS/NFPA<br />

toxicity ratings <strong>of</strong> 3 or 4, usually by the manufacturer. Also, they can generally be identified by the<br />

manufacturer’s warning labels (danger! - Highly Toxic, Poison, etc.) While no specific secondary labeling<br />

will be attached to chemical containers <strong>for</strong> highly acute toxic chemicals, you will be expected to adhere to<br />

the special handling provisions listed below when working with them. There is no need to store them in a<br />

designated storage area, although you should work with them only in a designated work area (in other<br />

words, a hood).<br />

See the Training section <strong>of</strong> this manual <strong>for</strong> an explanation <strong>of</strong> the Hazard Communication<br />

Standard’s Hazard Material Identification System (HMIS) or National Fire Protection Association (NFPA)<br />

hazard rating system. Under these systems, both hazard ratings are pretty much the same.<br />

Most chemical manufacturers rate their chemicals. The Hazard Communication Standard requires<br />

manufacturers to provide hazard evaluations in the <strong>for</strong>m <strong>of</strong> MSDS sheets. All supply MSDS sheets with<br />

hazard evaluations, but not all supply HMIS hazard ratings.<br />

The present regulatory standard applicable to the Chemistry Department, which superseded the<br />

Haz-Comm Standard, is called the “Laboratory Standard” and requires only that “particularly hazardous<br />

chemicals” be worked with in designated areas. It only requires carcinogens and mutagens/teratogens to be<br />

labeled.<br />

Acute toxicity is rated from 0 to 4 in the HMIS/NFPA systems (0 less dangerous, 4 most<br />

dangerous). One could regard those rated as 3 and 4 as chemicals with a “high degree <strong>of</strong> acute toxicity,”<br />

thus combining the regulatory requirements <strong>for</strong> hazard assessment present in the Haz-Com standard and the<br />

Laboratory standard, into one rating system, that is, the HMIS system.<br />

Teratogens and mutagens are listed as chronically toxic chemicals, designated as the letter “T” <strong>for</strong><br />

known teratogens and “t” <strong>for</strong> suspected teratogens. Known mutagens are “M”, suspected mutagens are<br />

“m”. Allergens are “A” and substances which cause silicosis are “S”. Carcinogens are labeled as<br />

65


chronically toxic chemicals, with letter designation <strong>of</strong> “C” <strong>for</strong> known carcinogens and “c” <strong>for</strong> suspected<br />

carcinogens. This system is in place so that you will be able to immediately recognize all carcinogens,<br />

teratogens / mutagens, and extremely hazardous chemicals in your lab when you review your MSDS<br />

inventory<br />

The procedures <strong>for</strong> working with these three types <strong>of</strong> particularly hazardous chemicals are<br />

described below.<br />

2. INIMICAL CHEMICALS: RULES OF ENGAGEMENT<br />

* Work only in a "designated area" when handling carcinogens, reproductive toxins, or extremely<br />

hazardous chemicals. The "designated area" may be an undergraduate lab fume hood, a research lab hood,<br />

a glove box, or, at the very minimum, any well ventilated area judged to be appropriate to the severity <strong>of</strong><br />

danger by your teacher or research director. An alternative strategy would be to refer to the entire area or<br />

laboratory as the designated area, if such substances are constantly moved back and <strong>for</strong>th throughout the<br />

room.<br />

* Label the designated area. Do not allow access to the area by anyone other than authorized personnel.<br />

Storage areas should also be labeled specifically <strong>for</strong> storage <strong>of</strong> carcinogens and reproductive toxins. When<br />

possible, store such chemicals in hood cabinets. Extremely hazardous chemicals can be stored on lab<br />

shelves, but should be handled only in designated areas.<br />

* <strong>Use</strong> the smallest amount <strong>of</strong> the chemical necessary <strong>for</strong> completion <strong>of</strong> your work. Do not leave bottles<br />

or other containers open. Close them immediately after use.<br />

* Always wear safety glasses and always wear gloves when the slightest possibility exists that these<br />

chemicals may come into skin contact. Heavier protection such as face-shields or safety shields should be<br />

available if needed.<br />

* Cease all activity with these chemicals when hoods malfunction entirely. Make every ef<strong>for</strong>t to avoid<br />

breathing fumes from these chemicals<br />

* Wash hands be<strong>for</strong>e leaving laboratory.<br />

* Do not place bottles <strong>of</strong> chemicals in harm’s way in congested work areas without adequate room to<br />

maneuver.<br />

* Read pages 90-93 <strong>of</strong> Prudent Practices, 2nd edition <strong>for</strong> further elaboration.<br />

* Also, you must list procedures <strong>for</strong> safely removing highly toxic waste, such as EPA acute P-<br />

Listed waste (http://www.epa.gov/docs/epacfr40/chapt-I.info/subch-I/40P0261.pdf – go to Part 261.33)<br />

or any other broad category <strong>of</strong> frequently encountered classes <strong>of</strong> very toxic waste generated in your<br />

work area or hood. An example would be how to package spent mercury from an organometallic<br />

reaction or how to dispose <strong>of</strong> contaminated Silica-gel from a column chromatography experiment.<br />

<strong>Use</strong> the entire chapter <strong>of</strong> the “Procedures <strong>for</strong> Handling Hazardous Chemical Waste” beginning in<br />

section III.C <strong>of</strong> this manual as your basic guide.<br />

* Lastly, you must also state how you would de-contaminate used equipment and bench top<br />

surfaces which have come in contact with very toxic waste spilled and/or used with the equipment,<br />

(See Dr. Fishbein’s following example procedure <strong>for</strong> decontamination <strong>of</strong> carcinogenic diazoate and<br />

nitrosamine residues). You should indicate how you will remove traces <strong>of</strong> it from bench tops if<br />

spilled, how to place it in containers without endangering yourself or others, etc.<br />

66


G. Specific Procedures <strong>for</strong> Safe Removal <strong>of</strong> Highly Toxic Waste<br />

PROCEDURE FOR LAB ROOM #<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

67


1. Dr. Alexander – Lab Room #108<br />

SPECIFIC PROCEDURE FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE#108<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Two categories <strong>of</strong> hazardous waste are generated in room 108. The first is radioactive waste, which will<br />

be disposed <strong>of</strong> according to the requirements <strong>of</strong> the <strong>of</strong>fice <strong>of</strong> radiation safety as outlined in the user’s<br />

license. Briefly, short half-life ( 32 P and 35 S) will be stored separately ( 32 P in a shielded container) from<br />

longer half-life waste such as 3 H and 14 C. These will be collected at regular intervals by employees <strong>of</strong> the<br />

<strong>of</strong>fice <strong>of</strong> radiation safety.<br />

The second category is ethidium bromide used to detect nucleic acids by gel electrophoresis. The<br />

quantities used (except <strong>for</strong> stock quantities) are on the order <strong>of</strong> 0.05% in water or gel. Low concentration<br />

liquid waste will be decontaminated by household bleach and disposed <strong>of</strong> in the drain after<br />

decontamination. Low concentration gel waste will be collected and disposed <strong>of</strong> on a quarterly basis<br />

(approximately 1 ft 3 per quarter).<br />

Every two weeks we autoclave (steam sterilize) pipets, tilps, and petri dishes that contain small amounts <strong>of</strong><br />

non-patogenic E. Coli bacteria. We autoclave to mininize the smell <strong>of</strong> this waste and to minimize possible<br />

autibiotic resistance from developing. The nonhazardous, nonregulated waste material from this operation<br />

is deposited directly in the garbage containers in the lab.<br />

68


2. Dr. Bierbach – Lab Room #107<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Two categories <strong>of</strong> hazardous waste are generated in room 107. The first is radioactive waste, which will<br />

be disposed <strong>of</strong> according to the requirements <strong>of</strong> the <strong>of</strong>fice <strong>of</strong> radiation safety as outlined in the user’s<br />

license. Briefly, short half-life ( 32 P ) will be stored in a shielded container. This will be collected at<br />

regular intervals by employees <strong>of</strong> the <strong>of</strong>fice <strong>of</strong> radiation safety.<br />

The second category is ethidium bromide used to detect nucleic acids by gel electrophoresis. The<br />

quantities used (except <strong>for</strong> stock quantities) are on the order <strong>of</strong> 0.05% in water or gel. Low concentration<br />

liquid waste will be decontaminated by household bleach and disposed <strong>of</strong> in the drain after<br />

decontamination.<br />

Beirbach‟s chemical waste, taken to the waste storage area in room # 20<br />

Dr. Beirbach’s chemical waste<br />

HAZARDOUS WASTE, DATE_________<br />

� Dichloromethane<br />

� Chloro<strong>for</strong>m<br />

� 9-Aminoacridine (1 – 3%)<br />

� Dimethyl<strong>for</strong>mamide (1 – 5%)<br />

HAZARDOUS WASTE, DATE_________<br />

� 1,4-Dioxane<br />

� Tetrahydr<strong>of</strong>uran<br />

� Diethyl ether<br />

� 9-Aminoacridine (1 – 3%)<br />

� Dimethyl<strong>for</strong>mamide (1 – 5%)<br />

HAZARDOUS WASTE, DATE__________<br />

� Ethanol<br />

� Acetone<br />

� Methanol<br />

� 9-Aminoacridine (1 – 3%)<br />

� Dimethyl<strong>for</strong>mamide (1 – 5%)<br />

HAZARDOUS WASTE, DATE__________<br />

Water with 1 to 5% <strong>of</strong> each <strong>of</strong>:<br />

� Cobalt chloride<br />

� Chromium chloride<br />

� Sodium sulfate<br />

� Calcium chloride<br />

� Magnesium sulfate<br />

� Sodium chloride<br />

� 9-Aminoacridine<br />

69


HAZARDOUS WASTE, DATE__________<br />

) Non-halogenated Organic solvents:<br />

� Ethyl acetate<br />

� Hexane<br />

� Methanol<br />

� Ethanol<br />

� Acetone<br />

� Petroleum ether<br />

� Benzene<br />

� Toluene<br />

HAZARDOUS WASTE, DATE_________<br />

) Water with:<br />

� Acridine<br />

� Sodium hydroxide<br />

HAZARDOUS WASTE, DATE_________<br />

) Ethanol and water with:<br />

� Mercuric chloride<br />

� Mercury metal<br />

� Aluminum metal<br />

HAZARDOUS WASTE, DATE_________<br />

) Vacuum pump oil and cyclohexane<br />

HAZARDOUS WASTE, DATE___________<br />

) Halogenated Organic solvents:<br />

� Methylene chloride<br />

� Chloro<strong>for</strong>m<br />

70


3. Dr. Brown – Lab Room #14<br />

SPECIFIC PROCEDURE FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE#14<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Four broad categories <strong>of</strong> hazardous wastes are generated by this laboratory. Each category is listed below,<br />

followed by typical examples. Specific handling precautions, waste disposal, and decontamination<br />

procedures are given <strong>for</strong> each class <strong>of</strong> waste.<br />

1. Biohazards/recombinant organisms (antibiotic-resistant E. coli and Pichia pastoris)<br />

2. Mutagenic/carcinogenic/teratogenic chemicals (ethidium bromide, dimethyl <strong>for</strong>mamide)<br />

3. Toxic heavy-metals (lead, mercury, gold, platinum, osmium, iridium, samarium, uranium)<br />

4. Radioactive isotopes ( 32 P, 33 P, 35 S)<br />

BIOHAZARDOUS WASTE<br />

Protective Equipment.<br />

Gloves and a lab coat should be worn at all times when working with recombinant organisms or handling<br />

potentially infectious or biohazardous material. Further details can be sought at the CDC‟s web page<br />

”Biosafety in Microbiological and Biomedical Laboratories” (BMBL) 4th Edition<br />

http://www.cdc.gov/od/ohs/biosfty/bmbl4/bmbl4toc.htm.<br />

Liquid waste. Liquid bacteria or yeast cultures or used media should be decontaminated prior to disposal.<br />

Dilute cultures with an appropriate germicidal agent, i.e., 20 % Wescodyne in 50% ethanol or 10 % sodium<br />

hypochlorite (Chlorox bleach) and allow to stand <strong>for</strong> 10-20 minutes. Dispose <strong>of</strong> solution by pouring down<br />

drain followed by copious amount <strong>of</strong> water. Flush sink with germicide and rinse with water.<br />

Solid waste. Any tubes, pipets, pipet tips, Petri dishes, or solid medium (agar) which has<br />

come in contact with microorganisms should be disposed <strong>of</strong> in an appropriate biohazardous waste bag, and<br />

subsequently autoclaved. Sharp items such as needles, tips or broken glassware should be placed in a<br />

sharps container and autoclaved separately from other solid-waste items.<br />

CARCINOGENIC, MUTAGENIC OR TERATOGENIC WASTE<br />

Protective Equipment.<br />

Safety goggles, gloves and a lab coat should be worn at all times when working with carcinogenic,<br />

mutagenic or teratogenic compounds. The most typical carcinogenic compound encountered in our<br />

laboratory is ethidium bromide.<br />

Liquid waste. Liquid containing low concentrations <strong>of</strong> ethidium bromide should be deactivated by the<br />

addition <strong>of</strong> sodium hypochlorate and poured down the drain. Solutions containing high concentrations <strong>of</strong><br />

ethidium bromide should filtered through activated-charcoal,. The filtrate can be deactivated with bleach<br />

and poured down the drain and the charcoal disposed <strong>of</strong> as solid waste.<br />

Solid waste. Any tubes, pipets, pipet tips, or gel medium (agarose) which has come in contact with<br />

ethidium bromide should be disposed <strong>of</strong> in an appropriate waste container and labeled. Solid waste will be<br />

disposed <strong>of</strong> on a quarterly period.<br />

71


HEAVY-METAL WASTE<br />

Protective Equipment.<br />

Safety goggles, gloves and a lab coat should be worn at all times when working with heavy metal-containing<br />

compounds. Volatile compounds, such as mercury-containing chemicals, should be used only in the fume<br />

hood.<br />

Heavy Metal Safety Rules<br />

In protein crystallography we use many heavy metal compounds. Toxicity in<strong>for</strong>mation is available <strong>for</strong> just<br />

a few <strong>of</strong> them. There<strong>for</strong>e, assume that all <strong>of</strong> them are insidious toxins and treat them with great respect.<br />

These rules are very similar to radioisotope rules. You must be introduced to these chemicals; you may not<br />

spontaneously start using them.<br />

1. Research is done by humans. The skill <strong>of</strong> humans depends on emotional state. Please think about how<br />

coherent you are feeling be<strong>for</strong>e doing heavy atom work. Don't rush through a heavy metal experiment<br />

to get somewhere else. Completely focus your attention on the heavy metal experiment.<br />

2. All the heavy atom compounds must be handled with gloves. Wear gloves even to look at the bottles. If<br />

you must touch doorknobs while handling heavy metals, take <strong>of</strong>f the gloves, or get somebody to open<br />

the doors <strong>for</strong> you. You should also wear a lab coat and closed-toe shoes.<br />

3. Glassware and spatulas used <strong>for</strong> heavy metal experiments are contaminated <strong>for</strong>ever: Do not return them<br />

to general circulation. <strong>Use</strong> our dedicated heavy metal spatulas <strong>for</strong> heavy metals. Clean heavy metal<br />

spatulas with a wet kimwipe. The contaminated kimwipe goes to dry waste (see item 7). Please do<br />

heavy atom experiments in well labelled crystallization trays, whenever possible. If you must use<br />

glassware, clearly label it, and keep it completely separate from non-heavy metal glassware.<br />

4.Weigh heavy metal compounds on weighing paper, or into centrifuge tubes on top <strong>of</strong> weighing paper.<br />

<strong>Use</strong> the analytical balances (the ones with enclosures), not the top-loaders. Many <strong>of</strong> these compounds<br />

are corrosive to the balances, in addition to poisoning all subsequent experiments and experimentalists.<br />

If you spill any, clean up immediately. A spray decontaminant, and a roll <strong>of</strong> hazardous spill towel are in<br />

room 219A. All clean-up materials go to heavy metal dry waste (see item 7).<br />

5. <strong>Use</strong> only minimal amounts <strong>of</strong> heavy atom compounds. Try to keep heavy metal experiments below<br />

1ml, using at most a few milligrams <strong>of</strong> heavy metal compound. The volume <strong>of</strong> toxic solution and<br />

disposal bulk may be minimized by soaking the crystals on the tops <strong>of</strong> Micro Bridges.<br />

6. Special handling: Moderately volatile mercury compounds such as methyl mercuric chloride are stored<br />

in a sealed box. Open that box in the hood and handle these compounds in the hood as much as<br />

possible. We have separate documentation <strong>for</strong> dimethyl-mercury and tetraethyllead:<br />

http://www.doe-mbi.ucla.edu/People/Recipes/DMM.html<br />

Osmium tetroxide is also volatile, and should be stored in the same kind <strong>of</strong> vials as dimethylmercury.<br />

Uranium and thorium compounds are radioactive, not just toxic. Document their use on the inventory<br />

sheet stored with the compounds, just as you would any other isotope.<br />

7. Disposal <strong>of</strong> and planning <strong>for</strong> disposal <strong>of</strong> heavy metal wastes: Segregate heavy metals to ease disposal:<br />

Keep mercury compounds in one crystallization tray, platinum reagents in another. Keep track <strong>of</strong> how<br />

much heavy metal reagent is in each tray. At disposal time, fill in the blanks on a “Hardous Waste ID<br />

Tag”.<br />

Wet and dry trays: Collect liquid heavy metal wastes into screw-cap bottles to take to hazardous waste<br />

disposal. There should be one metal type per bottle (all Hg or all Pt, etc.). Fill in the blanks, and attach<br />

a ``Hazardous Waste ID Tag" to each bottle. After flushing the trays with at least 1 M HNO3, or if the<br />

trays have already dried out at the time <strong>of</strong> disposal, the contaminated trays qualify as “dry waste” (see<br />

below), so put them into a clear plastic bag (Put the bag inside a box, if there are a lot <strong>of</strong> trays).<br />

72


<strong>Dry</strong> s<strong>of</strong>t things: Weighing paper, paper towels, gloves, and other dry non-sharp wastes contaminated by<br />

heavy metals should be left in the heavy metal dry waste container near the hood.<br />

<strong>Dry</strong> sharp things: Contaminated sharp things should be left in the heavy metal sharps container, in the<br />

hood.<br />

Uranium and Thorium compounds are radioactive and very toxic. They should be packaged <strong>for</strong> disposal<br />

as <strong>for</strong> the other metals, but their contents identified with chemical and isotope tags, and given to the<br />

Radiation Safety Office, not to the usual hazardous waste disposal people.<br />

Liquid waste.<br />

Liquid waste containing heavy metal compounds should be placed in a labeled container and<br />

stored <strong>for</strong> chemical waste pick-up.<br />

Solid waste.<br />

Solid waste containing heavy metals should be left in the heavy metal dry waste container near the<br />

hood.<br />

RADIOACTIVE WASTE<br />

Protective Equipment.<br />

Safety goggles, gloves and a lab coat should be worn at all times when working with radioactive<br />

compounds.<br />

Liquid waste.<br />

Liquid waste containing heavy atoms should be placed in a labeled container.<br />

Radioactive waste will be disposed <strong>of</strong> according to the requirements <strong>of</strong> the <strong>of</strong>fice <strong>of</strong> radiation safety as<br />

outlined in the user’s license. Briefly, short half-life ( 32 P and 35 S) will be stored separately ( 32 P in a shielded<br />

container) from longer half-life waste such as 3 H and 14 C. These will be collected at regular intervals by<br />

employees <strong>of</strong> the <strong>of</strong>fice <strong>of</strong> radiation safety.<br />

73


4. Dr. Buchmueller – Lab Room #1<br />

SPECIFIC PROCEDURE FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE #1<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Three categories <strong>of</strong> hazardous waste are generated in room 1. The first is radioactive waste, which will be<br />

disposed <strong>of</strong> according to the requirements <strong>of</strong> the <strong>of</strong>fice <strong>of</strong> radiation safety as outlined in the user’s license.<br />

Briefly, short half-life ( 32 P and 35 S) will be stored separately ( 32 P in a shielded container). These will be<br />

collected at regular intervals by employees <strong>of</strong> the <strong>of</strong>fice <strong>of</strong> radiation safety.<br />

The second category is ethidium bromide used to detect nucleic acids by gel electrophoresis. The<br />

quantities used (except <strong>for</strong> stock quantities) are on the order <strong>of</strong> 0.05% in water or gel. Low concentration<br />

liquid waste will be decontaminated by household bleach and disposed <strong>of</strong> in the drain after<br />

decontamination. Low concentration gel waste will be collected and disposed <strong>of</strong> on a quarterly basis<br />

(approximately 1 ft 3 per quarter).<br />

We rarely work with E. Coli, but when we do we autoclave (steam sterilize) pipets, tilps, and petri dishes<br />

that contain small amounts <strong>of</strong> non-patogenic E. Coli bacteria. We autoclave to mininize the smell <strong>of</strong> this<br />

waste and to minimize possible autibiotic resistance from developing. The nonhazardous, nonregulated<br />

waste material from this operation is deposited directly in the garbage containers in the lab.<br />

Small amounts <strong>of</strong> phenol, Chloro<strong>for</strong>m, and Isoamyl alcohol waste are generated (estimated amount less<br />

than 500 milliliters per year). This waste is clearly labeled and stored a 55 ml bottle kept in the hood in<br />

room # 1 until it is taken to the waste containment area in room # 20 <strong>of</strong> Salem Hall <strong>for</strong> removal.<br />

74


5. Dr. Colyer – Lab Room # 114<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

The Colyer lab (Salem 114) binds organic dyes to proteins and then separates them using capillary<br />

electrophoresis. The organic dyes are typically prepared in methanol, DMSO, or DMF and later diluted in<br />

water, or aqueous buffers. Extremely small amounts <strong>of</strong> waste are produced at any given time, due to the<br />

total <strong>of</strong> 3-10 mL <strong>of</strong> buffer used by a researcher on any given day. Due to the basic fuctioning <strong>of</strong> the system,<br />

small amounts <strong>of</strong> protein will be disposed <strong>of</strong> with the buffer waste. The final concentrations <strong>of</strong> protein tend<br />

to be in the pico-femtomolar concentration in the buffer or organic hazardous waste systems. The pure<br />

proteins are prepared in water, stored in the refrigerator or freezer, and disposed <strong>of</strong> by neutralization in<br />

50% bleach solution.<br />

Typical chemical waste generated in this lab is as follows. It will be labeled as Hazardous Waste, the<br />

contents <strong>of</strong> each properly bottle sealed, and all will be taken downstairs to the solvent room # 20 to await<br />

removal by a chemical waste company:<br />

HAZARDOUS WASTE<br />

1) Methanol and Ethanol with organic dyes, as follows:<br />

� DIMETHYL-SULFOXIDE (DMSO), less than 1%<br />

� N,N-DIMETHYLFORMAMIDE (DMF), less than 1%<br />

� SQUARYLIUM RED-1C, ORGANIC DYE, less than 1%<br />

� SQUARYLIUM RED-3, ORGANIC DYE, less than 1%<br />

� NN-127, ORGANIC DYE, less than 1%<br />

� CALCAFLUOR, ORGANIC DYE, less than 1%<br />

� FQ, ORGANIC DYE, less than 1%<br />

� FLUORESCAMINE, ORGANIC DYE, less than 1%<br />

HAZARDOUS WASTE<br />

2) Aqueous with organic dyes, as follows:<br />

� METHANOL, less than 1%<br />

� DIMETHYL-SULFOXIDE (DMSO), less than 1%<br />

� N,N-DIMETHYLFORMAMIDE (DMF), less than 1%<br />

� SQUARYLIUM RED-1C, ORGANIC DYE, less than 1%<br />

� SQUARYLIUM RED-3, ORGANIC DYE, less than 1%<br />

� NN-127, ORGANIC DYE, less than 1%<br />

� CALCAFLUOR, ORGANIC DYE, less than 1%<br />

� FQ, ORGANIC DYE, less than 1%<br />

� FLUORESCAMINE, ORGANIC DYE, less than 1%<br />

HAZARDOUS WASTE<br />

3) Methanol and Ethanol with organic dyes and proteins, as follows:<br />

� DIMETHYL-SULFOXIDE (DMSO), less than 1%<br />

� N,N-DIMETHYLFORMAMIDE (DMF), less than 1%<br />

� SQUARYLIUM RED-1C, ORGANIC DYE, less than 1%<br />

75


� SQUARYLIUM RED-3, ORGANIC DYE, less than 1%<br />

� NN-127, ORGANIC DYE, less than 1%<br />

� CALCAFLUOR, ORGANIC DYE, less than 1%<br />

� FQ, ORGANIC DYE, less than 1%<br />

� FLUORESCAMINE, ORGANIC DYE, less than 1%<br />

� SERUM ALBUMINS (HSA AND BSA), PROTEIN, less than 1%<br />

� BETA LACTOGLOBULIN A & B, PROTEIN, less than 1%<br />

� GLUTATHIONE, TRIPEPTIDE, less than 1%<br />

� ALLOPHYCOCYANINE, PROTEIN, less than 1%<br />

� B-PHYCOERYTHRIN, PROTEIN, less than 1%<br />

� C-PHYCOCYANIN, PROTEIN, less than 1%<br />

HAZARDOUS WASTE<br />

4) Aqueous with:<br />

� METHANOL, 10%<br />

� THALLOUS NITRATE, less than 1%<br />

HAZARDOUS WASTE<br />

5) Aqueous based with organic dyes, protein, and buffer salts, as follows:<br />

� DIMETHYL-SULFOXIDE (DMSO), less than 1%<br />

� N,N-DIMETHYLFORMAMIDE (DMF), less than 1%<br />

� METHANOL, less than 1%<br />

� SQUARYLIUM RED-1C, ORGANIC DYE, less than 1%<br />

� SQUARYLIUM RED-3, ORGANIC DYE, less than 1%<br />

� NN-127, ORGANIC DYE, less than 1%<br />

� CALCAFLUOR, ORGANIC DYE, less than 1%<br />

� FQ, ORGANIC DYE, less than 1%<br />

� FLUORESCAMINE, ORGANIC DYE, less than 1%<br />

� SERUM ALBUMINS (HSA AND BSA), PROTEIN, less than 1%<br />

� BETA LACTOGLOBULIN A & B, PROTEIN, less than 1%<br />

� GLUTATHIONE, TRIPEPTIDE, less than 1%<br />

� ALLOPHYCOCYANINE, PROTEIN, less than 1%<br />

� B-PHYCOERYTHRIN, PROTEIN, less than 1%<br />

� C-PHYCOCYANIN, PROTEIN, less than 1%<br />

� PHYTIC ACID, BUFFER, less than 1%<br />

� BORIC ACID, BUFFER, less than 1%<br />

� TRISMA (TRIS), BUFFER, less than 1%<br />

� SODIUM DODECYL SULFATE (SDS), SURFACTANT, less than 1%<br />

� AMMONIUM BICARBONATE, BUFFER, less than 1%<br />

� AMMONIUM ACETATE, BUFFER, less than 1%<br />

HAZARDOUS WASTE<br />

6) Aqueous with:<br />

� POTASSIUM CYANIDE, less than 1%<br />

� BORIC ACID, 25mM<br />

HAZARDOUS WASTE<br />

7) THALLOUS NITRATE<br />

76


6. Dr. Hinze – Lab Room # 109<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Common wastes from this laboratory include used mobile phase and extraction solvents which<br />

generally contain only trace amounts <strong>of</strong> more toxic chemicals. Most should be stored in glass containers<br />

in a hood until a volume <strong>of</strong> 1L or greater has been collected at which time the container should be taken to<br />

the metal solvent waste table in room 20, provided it has been labeled with the full name and approximate<br />

amount <strong>of</strong> each component.<br />

77


7. Dr. Brad Jones – Lab Room # 118<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Trace and ultra trace metal standards are prepared at concentration well below the toxic level.<br />

For example, Ca, Zn, Ba at the ppb and sub-ppb level. Standards containing HNO3 are neutralized prior<br />

to disposal. They are then safely disposed <strong>of</strong> with plenty <strong>of</strong> water down the sink.<br />

Typical relatively benign chemical waste generated in this lab is described as follows:<br />

Water (Acidic) with:<br />

(Color varies with component concentration - e.g., when Copper predominates, the color will<br />

be bluish, but all components are still less than 1%)<br />

� Cadmium Chloride, less than 1%<br />

� Cadmium Bromide, less than 1%<br />

� Lead Nitrate, less than 1%<br />

� Copper nitrate, less than 1%<br />

� Lanthanum nitrate, less than 1%<br />

� Thulium nitrate, less than 1%<br />

� Yetterbium nitrate, less than 1%<br />

� Europium nitrate, less than 1%<br />

� Lutetium nitrate, less than 1%<br />

� Gadolinium nitrate, less than 1%<br />

� Samarium nitrate, less than 1%<br />

� Promethium nitrate, less than 1%<br />

� Lutetium nitrate, less than 1%<br />

78


8. Dr. Paul Jones – Lab Room # 14<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

In addition to safe handling and disposal <strong>of</strong> routine chemicals described elsewhere in this document (i.e.,<br />

Section III.C, Procedures <strong>for</strong> Handling Hazardous Waste,) , the following in<strong>for</strong>mation applies specifically<br />

to this Lab. Please consult this safety manual <strong>for</strong> general guidelines and MSDS sheets <strong>for</strong> detailed<br />

guidelines <strong>for</strong> particular chemicals.<br />

Occasionally, Osmium/Chromium oxidations <strong>of</strong> alkenes to carboxylic acids are carried out in this lab.<br />

Osmium and Chromium reagents must be handled extremely <strong>care</strong>fully as both are highly toxic metals.<br />

Always wear gloves when working with these reagents and <strong>for</strong> any neat Osmium or Chromium compound,<br />

handle the material only in a fume hood. Any waste generated from the reaction that contains either metal<br />

must be placed in a sealed container and clearly marked as containing the metals. Prior to this, reduce<br />

any remaining Chromium(VI) by adding a large excess <strong>of</strong> 2-propanol. Once the waste container is 3/4 full,<br />

seal it securely, be sure the identification is still clear (along with your name, lab, lab phone number, and<br />

date), and place the container in the solvent disposal room (Salem 20).<br />

Under no circumstances should waste containing Osmium or Chromium be placed in routine solvent<br />

waste or go down the drain.<br />

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9. Dr. Bruce King – Lab Room # 17<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Room 17: General Activity - Synthetic Organic Chemistry. Room 17 contains flammable organic<br />

solvents, halogenated and non-halogenated, organic chemicals, concentrated acids, sodium metal,<br />

compressed gas cylinders, and silica gel. These materials are stored in labeled containers in an explosion<br />

pro<strong>of</strong> refrigerator, under various fume hoods and on shelving around the laboratory. Waste organic<br />

solvents and chemicals are separated as non-sulfur and non-halogen containing organic compounds and<br />

stored in labeled containers under a fume hood. Sulfur and halogen containing organic waste is placed in<br />

separate labeled containers. <strong>Use</strong>d silica gel is stored in a labeled plastic container in a fume hood. When<br />

full, these waste containers are transferred to the large waste containers in room # 20.<br />

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10. Dr. Kondepudi – Lab Room # 5<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Remove chemicals from lab via labeling, temporary storage in back <strong>of</strong> hoods, and transport to<br />

room #20 via "Procedures <strong>for</strong> Handling Chemical Waste" section already listed in this manual. Only<br />

occasional toxic metal salts and sodium chlorate, etc., will be used in this lab.<br />

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11. Dr. Lachgar – Lab Room # 6<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Solid wastes are to be collected into labeled waste bottles and then transferred to waste storage<br />

areas. The liquids used are usually aqueous acid and base solutions. They are to be disposed after being<br />

neutralized. Aqueous solutions(usually acidic) <strong>of</strong> inorganic saltsare kept in typical glass waste jars,<br />

labeled with all components, and taken to the waste storage area in room # 20. Typical waste streams<br />

generated in this lab are as follows:<br />

1) Water, methanol, acetonitrile and ethanol (acidic) with:<br />

� Niobium chloride<br />

� Potassium cyanide<br />

� Silver nitrate<br />

� Copper chloride<br />

� Ethylenediamine<br />

� Vanadium acetylacetonate<br />

� salicylaldehyde<br />

� Tetramethylammonium chloride<br />

� Manganese acetate<br />

2) Water and ethanol (acidic) with:<br />

� Niobium chloride<br />

� Potassium cyanide<br />

� Cadmium chloride<br />

� Iron chloride<br />

� Tetramethylammonium chloride<br />

� Sodium chloride<br />

� Potassium chloride<br />

3) Hydrochloric acid (dilute) with:<br />

� Niobium chloride, trace amount<br />

� Tantalum chloride, trace amount<br />

4) Two jars <strong>of</strong> Water (acidic) with:<br />

� Hydrochloric acid<br />

� Nitric acid<br />

� Niobium chloride (trace amounts)<br />

� Tantalum chloride (trace amounts)<br />

5) One container <strong>of</strong>:<br />

� Acetone<br />

� Water<br />

� Dimethyl <strong>for</strong>mamide<br />

� Iron cyanide<br />

� 4,4’-Dipyridyl<br />

� Methylammonium chloride<br />

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� Ammonium hydroxide<br />

� Ammonium nitrate<br />

� Iron(III) chloride<br />

� Ethylenediamine<br />

� Acetonitrile<br />

� Ethanol<br />

� Niobium chloride<br />

� Salicylaldehyde<br />

83


12. Dr. N<strong>of</strong>tle – Lab Room # 118<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

The following common laboratory organic solvents can be collected in a waste container, labeled<br />

NON- SULFUR, NON-HALOGENATED ORGANIC SOLVENTS and be poured into one <strong>of</strong> the two 55<br />

gallon waste drums located in the solvent room, #20, assuming they are not overly contaminated with acids<br />

or large amounts <strong>of</strong> toxic or odoriferous sulfur compounds. Each chemical should be recorded by name<br />

and amount.<br />

acetone methyl ethyl ketone pump oil<br />

benzaldehyde mineral spirits tetrahydr<strong>of</strong>uran<br />

benzene motor oil toluene<br />

cyclohexane naphtha xylenes<br />

ethyl ether paint thinner ethyl alcohol, (and,<br />

ethyl acetate petroleum ether low-molecular weight alcohols,<br />

The methylene chloride and chloro<strong>for</strong>m must be collected in a well-labeled waste bottle and can be poured<br />

into labeled 20 liter empty white polyethylene containers kept next to the large 55 gallon steel drum on the<br />

floor in the wide yellow spill tray in the solvent room, #20. Sulfur containing compounds, complex<br />

heterocyclics, corrosives, organic acids, lachrymators, etc. (i.e. thiophene, pyrrole, acetonitrile, etc.)<br />

should be collected into well-labeled waste bottles and taken to the metal surface in the solvent room, #20.<br />

Consolidate compatible inorganic solids in a well-labeled waste container, organic solids in another.<br />

These can be placed on the metal surface table in the solvent room #20. Non-compatible solids should<br />

naturally be packaged separately.<br />

Typical waste streams originating from Dr. N<strong>of</strong>tle’s research lab are as follows:<br />

Organic <strong>Solvent</strong>s (Non-Halogenated)<br />

Ethyl Acetate, Hexanes, Acetone<br />

Diethyl Ether, Methanol, Ethanol<br />

Tetrahydr<strong>of</strong>uran, Toluene, Pentane<br />

Cyclohexane, Benzene, Acetonitrile, and occasionally Nitrobenzene<br />

Halogenated <strong>Solvent</strong>s<br />

Methylene chloride, chloro<strong>for</strong>m<br />

Acetone, with:<br />

tetrabutylammonium perchlorate tetrabutylammonium hexafluorophosphate<br />

tetrabutylammonium trifluoromethanesulfonate<br />

copper(II) perchlorate hexahydrate copper(II) trifluoromethanesulfonate<br />

copper(II) acetate monohydrate copper(II) chloride<br />

zinc(II) perchlorate hexahydrate zinc(II) trifluoromethanesulfonate<br />

N2-(2-pyridylmethyl)-3-thienyl carboxamide<br />

N2-(2-pyridylmethyl)-3-thenyl carboxamide<br />

N2-(2-pyridylmethyl)-5-(3-thienyl)-butyl carboxamide<br />

N2-(2-pyridylmethyl)-trans-3-(3-thienyl) acrylamide<br />

84


13. Dr. Sw<strong>of</strong><strong>for</strong>d – Lab Room # 1<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Practically no highly toxic waste is generated in this lab. Only benign organic dyes and other<br />

small amounts <strong>of</strong> analytical samples (<strong>for</strong> example, polyaromatic hydrocarbons). Typical bottles <strong>of</strong><br />

chemical waste (usually one or three one gallon jars collected over a period <strong>of</strong> 6 to 12 months) contain the<br />

following: methanol, ethanol, ethylene glycol, acetone, heptane, benzene, hexane, toluene, octane, and<br />

dyes, such as Rhodamine 590 and 61 and Keton red dye.<br />

85


14. Dr. Tobey – Lab Room # 2<br />

For the routine disposal <strong>of</strong> common chemicals please refer to Section III. C <strong>of</strong> this manual <strong>for</strong> standard<br />

handling <strong>of</strong> hazardous waste. The guidelines specific to this lab are outlined below.<br />

Palladium complexes are routinely used in this lab <strong>for</strong> cross-coupling reactions. Gloves should be worn in<br />

handling palladium waste and the waste is placed in a separate and clearly labeled container. Occasionally<br />

hydrazine is used in this lab and this is known to be carcinogenic so any waste containing hydrazine should<br />

be placed in a separate waste container and clearly labeled <strong>for</strong> disposal.<br />

Under no circumstances should hydrazine or palladium waste be placed in routine solvent containers<br />

or poured down the drain.<br />

Typical waste streams originating from this lab include:<br />

1) Clear Glass Bottle labeled “Liquid Palladium Waste”<br />

� Ethyl Ether<br />

� Tetrahydr<strong>of</strong>uran<br />

� Ethanol<br />

� Sulfuric acid<br />

� Palladium triphenylphosphine<br />

� Palladium acetate<br />

� Palladium metal<br />

� Trace amounts <strong>of</strong> Dimethyl sulfoxide, Hydrazine Hydrate, Hydrazine, water, Ethyl acetate, and<br />

Acetone<br />

2) Brown solvent bottle labeled “mixed palladium waste” (acidic)<br />

� Diluted acetic acid<br />

� Palladium triphenylphosphine<br />

� Palladium acetate,<br />

� Palladium metal<br />

� Palladium chloride<br />

� Filter paper<br />

� Triphenylphosphine<br />

� Ethyl Ether<br />

� Tetrahydr<strong>of</strong>uran<br />

� Ethanol,<br />

� Trace amounts <strong>of</strong> DMSO, Hydrazine Hydrate, Hydrazine, water, Ethyl Acetate,<br />

and Acetone<br />

3) wide mouth plastic bottle labeled “solid palladium waste”<br />

� Palladium metal<br />

� Palladium triphenylphosphine<br />

� Palladium acetate,<br />

� Palladium metal<br />

� Palladium chloride<br />

� Filter paper<br />

� Triphenylphosphine<br />

� Trace amounts <strong>of</strong> Dimethylsulfoxide, Hydrazine Hydrate, and Hydrazine<br />

4) Brown solvent bottle filled with acidic aqueous waste<br />

86


� Hydrochloric acid<br />

� Acetic acid,<br />

� Ammonium Chloride,<br />

� Potassium Carbonate,<br />

� triethylamine,<br />

� NaCl,<br />

� Sulfuric Acid,<br />

� triphenylphosphine oxide,<br />

� magnesium oxide,<br />

� diethylene glycol,<br />

� methanol,<br />

� ethanol,<br />

� less than 5mL <strong>of</strong> bis[2-(N,N-dimethylaminio)ethyl]etherAmmonium chloride<br />

5) Brown solvent bottle filled with acid aqueous waste (acidic)<br />

� Hydrochloric acid,<br />

� Acetic acid,<br />

� Ammonium Chloride,<br />

� Potassium Carbonate,<br />

� triethylamine,<br />

� NaCl,<br />

� Sulfuric Acid,<br />

� triphenylphosphine oxide,<br />

� magnesium oxide,<br />

� diethylene glycol,<br />

� methanol,<br />

� ethanol,<br />

� less than 5mL <strong>of</strong> bis[2-(N,N-dimethylaminio)ethyl]etherAmmonium chloride<br />

6) Brown solvent bottle filled with acidic aqueous waste:<br />

� Hydrochloric acid,<br />

� Acetic acid,<br />

� Ammonium Chloride,<br />

� Potassium Carbonate,<br />

� triethylamine,<br />

� Sodium chloride,<br />

� Sulfuric Acid,<br />

� triphenylphosphine oxide,<br />

� magnesium oxide,<br />

� diethylene glycol,<br />

� methanol,<br />

� ethanol,<br />

� Benzene<br />

� Magnesium oxide<br />

� Magnesium hydroxide<br />

� Magnesium bromide<br />

� Magnesium sulfate<br />

7) Large Red Can Organic <strong>Solvent</strong> Waste (February 2006)<br />

� Ethyl Acetate<br />

� Hexanes<br />

� Acetone<br />

� Isopropanol<br />

87


8) Brown solvent bottle filled with aqueous waste (30 March 2006)<br />

� Diluted acetic acid<br />

� Diluted HCl<br />

� VERY Diluted KOH<br />

� Carbonate salts<br />

� NaCl<br />

� Copper salts<br />

� Ammonium salts<br />

9) Brown solvent bottle filled with acidic aqueous waste (06 June 2006)<br />

� acetic acid<br />

� hydrochloric acid<br />

� potassium hydroxide<br />

� Sodium Carbonate<br />

� Sodium chloride<br />

� Ammonium hydroxide<br />

� Ammonium chloride<br />

� Cupric cyanide<br />

10) Water, very acidic (and small amount <strong>of</strong> Tetrahydr<strong>of</strong>uran) with:<br />

� Potassium carbonate<br />

� Ammonium chloride<br />

� Sodium bicarbonate<br />

� Acetic acid<br />

� Hydrochloric acid<br />

88


15. Dr. Welker – Lab Room # 13<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Handling, Storing and Removal <strong>of</strong> Gases: This lab uses chlorine gas, ammonia, carbon<br />

monoxide (toxic), sulfur dioxide (toxic), and carbonyl sulfide (always work in fume hood). Always label<br />

cylinders, secure strap or chain cylinders to wall. When cylinders are not in use, shut the valves and<br />

relieve the regulator and cap the cylinders. Segregate gas cylinder storage from the storage <strong>of</strong> other<br />

chemicals. Keep in compatible classes <strong>of</strong> gases stored separately and keep flammable reactives, which<br />

include oxidizers and corrosives, away from cylinders. Segregate empty and full cylinders. To remove<br />

empty cylinders, place cylinder in its original shipping box, sealed with packing tape, and ship back to<br />

manufacturer (or give them to a local company).<br />

Preparation <strong>of</strong> Mercury (<strong>Use</strong>d) <strong>for</strong> Reclamation:<br />

Mercury must be clean and free <strong>of</strong> any salts or solvents be<strong>for</strong>e it can be sent <strong>for</strong> reclamati Work in a fume<br />

hood, wearing gloves and safety glasses. Obtain a large pan and two large beakers. Fill one beaker about<br />

1/4 full with water. Place some waste mercury * into the beaker containing water. Swirl contents <strong>of</strong><br />

beaker and <strong>care</strong>fully decant water into the other beaker. Repeat until mercury appears clean and free <strong>of</strong><br />

salts. Store mercury in appropriate container in well-ventilated area. Water may be poured down drain.<br />

* If mercury has been used in an amalgam with sodium, when reaction is complete, open the flask<br />

to the air <strong>for</strong> at least one day in a fume hood. Stir mercury with some isopropanol <strong>for</strong> a few hours to<br />

quench any sodium remaining. Decant the isopropanol. Mercury is ready to be cleaned and stored <strong>for</strong><br />

reclamation.<br />

89


16. Undergraduate – Lab Rooms # 7, 101, 102, 103, 104, 105, 106, 111<br />

SPECIFIC PROCEDURES FOR SAFE REMOVAL OF HIGHLY TOXIC WASTE<br />

Consult with your research advisor concerning proper methods <strong>for</strong> packaging and storing extremely<br />

hazardous waste. Research usually involves working with selective types or classes <strong>of</strong> chemicals. Prepare<br />

brief summaries in this section <strong>for</strong> handling spent chemicals peculiar to your lab.<br />

Highly toxic waste, as defined in section III.F.2 <strong>of</strong> this manual, is very seldom if ever generated in<br />

undergraduate teaching laboratories. When it is, specific procedures <strong>for</strong> removing it will be elaborated by<br />

the lab manager and instructors <strong>for</strong> the particular teaching lab in question. When working with highly<br />

toxic waste, one must work with it under a hood, pack it separately from other waste material, label it with<br />

specific names, collect it in a container (all as a last step in the student’s reaction or experimental<br />

procedure), and take it downstairs to the waste holding area in room #21.<br />

All other waste materials are covered under procedures listed elsewhere in this manual. (consult<br />

subchapter # 5, entitled "Waste from Undergraduate Labs", in section III.C). General Chemistry<br />

procedures <strong>for</strong> relatively benign waste handling and removal are listed in the training section <strong>of</strong> this<br />

manual.<br />

Additional standard operating procedures <strong>for</strong> handling general chemistry lab waste are contained<br />

in the instructor’s in<strong>for</strong>mation sections <strong>for</strong> each "Modular Laboratory Program in Chemistry" series <strong>for</strong><br />

experiments assigned by the instructor.<br />

The organic solvent waste procedures are likewise listed in the training section <strong>of</strong> this manual<br />

with specific instructions listed in the a<strong>for</strong>ementioned subchapter. Additional instructions are contained in<br />

the present undergraduate Organic Lab textbook at the end <strong>of</strong> all experimental procedures.<br />

90


H. Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top<br />

Surfaces which have come into contact with Highly Toxic Waste<br />

PROCEDURE FOR LAB ROOM #<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

91


Specific Decontamination Procedures <strong>for</strong> Equipment and Surfaces which have come<br />

into contact with Highly Toxic Waste [EXAMPLE ONLY, prepared by Dr. James<br />

Fishbein, <strong>for</strong>mer Occupant <strong>of</strong> Research Lab # 14]<br />

PROCEDURE FOR LAB ROOM # 14<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Lab Rules <strong>for</strong> Handling Decontamination <strong>of</strong> Personal Protective Equipment (PPE)<br />

and Lab Equipment Contaminated by Diazoate and Nitrosamine Residues<br />

These rules must be followed by all members <strong>of</strong> the group in order to insure your own and others<br />

safety. Failure to follow these rules endangers the health <strong>of</strong> you and your coworkers. Please read and<br />

follow the rules below!!<br />

General rules: 1) ALL unattended reactions in the hood, whether or not they involve nitrosamines or<br />

diazotes, must be labeled to indicate the reaction in progress and any harmful reagents<br />

employed. Unlabeled-unattended reactions are subject to immediate disposal in the acid<br />

bath.<br />

2) ALL reactions involving synthesis <strong>of</strong> diazotes, nitrosamines or nitrosamides must be<br />

carried out in the hoods.<br />

3) ALL items enter any <strong>of</strong> the hoods are not to be removed from the hood until they have<br />

been decontaminated. This rule applies whether or not the items have been used in the<br />

preparation <strong>of</strong> a diazote or nitrosamine or nitrosamide - whatever goes in is assumed to be<br />

contaminated even though likelihood is very low.<br />

4) ALL reactions involving synthesis <strong>of</strong> diazotes or nitrosamines should becarried out on<br />

surfaces that are covered with absorbent bench paper. This greatly aids in cleaning up<br />

any spills.<br />

5) ALL reactions involving diazote or N-nitrosamine syntheses must be cleaned up<br />

completely as soon as the reaction has been completed, subsequent to isolation <strong>of</strong><br />

products. Dirty flasks, tubes, and implements must be decontaminated immediately as<br />

specified below. Do not leave dirty bench paper or beakers or pipettes or spatulas etc.. in<br />

the hoods overnight, begin decontamination immediately.<br />

6) ALL spills <strong>of</strong> any amount <strong>of</strong> diazote or N-nitrosamine should be cleaned up<br />

immediately when they occur. Equipment such as stir plates, lab-jacks, ring-stands can be<br />

rinsed with acetone and the acetone allowed to collect onto the bench paper. More bench<br />

paper can be used as necessary. The bench paper, once air-dried, can be decontaminated<br />

by the procedures below. Always use heavy latex "non-disposable" gloves when cleaning<br />

up spills with acetone as acetone will penetrate the disposable gloves. After<br />

decontaminating the latex gloves, throw them away.<br />

Specific Clean-up Procedures. For N-nitrosamine and N-nitrosamides and urethanes, the<br />

decontamination solution should be 50% sulfuric acid to 50 % water with two packs <strong>of</strong> No-chromix <strong>for</strong><br />

each two gallon container. This is considered fresh until it is discolored at which time it can be<br />

92


egenerated with additional No-chromix. The acid baths should be changed once per month. Do not put<br />

disposable syringe needles in the acid baths!! For diazotes (once past the stage involving nitrosourethanes<br />

in the case <strong>of</strong> syn. compounds) an acidic solution <strong>of</strong> ~ 10% sulfuric acid suffices to decompose these<br />

compounds.<br />

All materials to be decontaminated should be submerged in the acid bath <strong>for</strong> 24hrs. Frequent<br />

checks should be made to ensure that the items are submerged. Large items may have to be turned or<br />

rotated after the first 24hrs and allowed to sit an additional 24hrs. Greater than 0.5g amounts <strong>of</strong><br />

nitrosamines should be decomposed in a separate acid bath, typically a beaker, which should additionally be<br />

agitated by a magnetic stirrer.<br />

Contents <strong>of</strong> NMR tubes should be emptied into a small beaker immediately after use. The tubes<br />

should then be filled with decontaminating acid solution by pipette and submerged <strong>for</strong> 24hrs. The contents<br />

<strong>of</strong> the NMR tubes should be concentrated immediately in the beaker and the residue-containing beaker<br />

should be submerged in acid <strong>for</strong> 24hrs. NMR tube caps should be treated in the acid solution <strong>for</strong> 24hrs and<br />

thrown out.<br />

Any gloves that contact N-nitrosamine or diazotes should be treated by the decontaminating acid<br />

solution. The same should be done with bench paper on which nitrosmaine containing solutions or solids<br />

have been spilled. Gloves or papers that have been used <strong>for</strong> routine handling in the hood need not be<br />

treated but should be put in a plastic bag in the hood which is then tied <strong>of</strong>f and transferred to a clean plastic<br />

bag outside the hood. The outer bag should be tied <strong>of</strong>f and removed.<br />

Glass cuvettes should be submerged in acid solution <strong>for</strong> 24hrs.<br />

Syringes that have been used to inject dilute solutions <strong>of</strong> N-nitroso compounds should be<br />

thoroughly washed, both interior and exterior, with an organic solvent such as acetone. The organic rinsing<br />

can be concentrated and the residue-containing beaker transferred to the acid bathe. The syringe can be<br />

then cleaned using decontaminating acid solution by repeated displacement <strong>of</strong> the plunger in and out <strong>of</strong> the<br />

syringe. The tip <strong>of</strong> the plunger and barrel and tip <strong>of</strong> the syringe should be submerged <strong>for</strong> 1hr. in acid<br />

solution.<br />

93


1. Dr. Alexander – Lab Room # 108<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Benches will be monitored after each use <strong>of</strong> radioactive materials and weekly by smear test and hand-held<br />

counter, as specified in the user’s license. Any surfaces with contamination greater than twice background<br />

will be cleaned with soap and water or commercial cleaner as necessary. Decontamination will proceed<br />

until smear tests are at background.<br />

Benches that are contaminated with low concentrations <strong>of</strong> ethidium bromide will be cleaned with paper<br />

towels (soaked with bleach (Sodium hypochlorite) that will then be disposed <strong>of</strong> with the solid (gel) waste.<br />

In the event <strong>of</strong> a spill <strong>of</strong> high concentration ethidium bromide, the surface will be decontaminated with a<br />

slurry <strong>of</strong> activated charcoal.<br />

94


2. Dr. Bierbach – Lab Room # 107<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Benches will be monitored after each use <strong>of</strong> radioactive materials and weekly by smear test and hand-held<br />

counter, as specified in the user’s license. Any surfaces with contamination greater than twice background<br />

will be cleaned with soap and water or commercial cleaner as necessary. Decontamination will proceed<br />

until smear tests are at background.<br />

Benches that are contaminated with low concentrations <strong>of</strong> ethidium bromide will be cleaned with paper<br />

towels soaked with bleach (Sodium hypochlorite) that will then be disposed <strong>of</strong> with the solid (gel) waste. In<br />

the event <strong>of</strong> a spill <strong>of</strong> high concentration ethidium bromide, the surface will be decontaminated with a<br />

slurry <strong>of</strong> activated charcoal.<br />

95


3. Dr. Brown – Lab Room # 14<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Spills <strong>of</strong> Biohazardous Waste. Spills <strong>of</strong> bacterial cultures should be contained immediately by blotting the<br />

area with paper towels or other absorbent material. Dispose <strong>of</strong> clean-up material in a biohazard bag.<br />

Disinfect the contaminated surface with a germicidal agent such as Wescodyne, bleach, or Lysol.<br />

bb<br />

Spills <strong>of</strong> Carcinogenic, Mutagenic, or Tetraogenic Waste. Spills <strong>of</strong> ethidium bromide should be<br />

contained immediately by blotting the area with paper towels or other absorbent material. Decontaminate<br />

the contaminated surface with bleach, and dispose <strong>of</strong> clean-up material with solid hazardous waste. For<br />

large spills, or spills containing high concentrations <strong>of</strong> ethidium bromide, a slurry <strong>of</strong> activated charcoal will<br />

be used to absorb the ehidium bromide, and will be disposed <strong>of</strong> with solid waste.<br />

Spills <strong>of</strong> Radioactive Waste. Benches will be monitored after each use <strong>of</strong> radioactive materials and<br />

weekly by smear test and hand-held counter, as specified in the user’s license. Any surfaces with<br />

contamination greater than twice background will be cleaned with soap and water or commercial cleaner as<br />

necessary. Decontamination will proceed until smear tests are at background.<br />

Benches that are contaminated with low concentrations <strong>of</strong> ethidium bromide will be cleaned with paper<br />

towels (soaked with bleach (Sodium hypochlorite) that will then be disposed <strong>of</strong> with the solid (gel) waste.<br />

In the event <strong>of</strong> a spill <strong>of</strong> high concentration ethidium bromide, the surface will be decontaminated with a<br />

slurry <strong>of</strong> activated charcoal.<br />

96


4. Dr. Buchmueller – Lab Room # 1<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Benches will be monitored after each use <strong>of</strong> radioactive materials and weekly by smear test and hand-held<br />

counter, as specified in the user’s license. Any surfaces with contamination greater than twice background<br />

will be cleaned with soap and water or commercial cleaner as necessary. Decontamination will proceed<br />

until smear tests are at background.<br />

Benches that are contaminated with low concentrations <strong>of</strong> ethidium bromide will be cleaned with paper<br />

towels (soaked with bleach (Sodium hypochlorite) that will then be disposed <strong>of</strong> with the solid (gel) waste.<br />

In the event <strong>of</strong> a spill <strong>of</strong> high concentration ethidium bromide, the surface will be decontaminated with a<br />

slurry <strong>of</strong> activated charcoal.<br />

Benches contaminated with spills <strong>of</strong> phenol, chloro<strong>for</strong>m, or isoamyl alcohol will cleaned by absorption <strong>of</strong><br />

such spills with either vermiculite or the departmental spill control material (kitty litter, sand, and baking<br />

soda) located in room # 20, Loading Dock. Any spills should be contained in containers and kept in the<br />

hood until eventual removal by our chemical waste removal company.<br />

97


5. Dr. Colyer – Lab Room # 114<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Lab bench tops contaminated with occasional spills will be cleaned with paper towels and cotton<br />

rags soaked with acetone or ethanol, or hot soap and water.<br />

98


6. Dr. Hinze – Lab Room # 109<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign. substance spilled. Usually only very small amounts <strong>of</strong> chemical samples will be<br />

used in this lab.<br />

Chemical spillage will be absorbed with a paper towel dampened with a solvent appropriate to<br />

the toxic substance spilled. Usually only very small amounts <strong>of</strong> chemical samples will be used in this lab.<br />

99


7. Dr. Brad Jones – Lab Room # 118<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Not applicable to our research laboratory.<br />

100


8. Dr. Paul Jones – Lab Room # 14<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

For routine cleaning, benchtops should be washed using a sponge and hot, soapy water followed by<br />

acetone and paper towels. If the spill contains a large amount <strong>of</strong> hydrophobic (oily) material, first wash<br />

the area using an organic solvent (ethyl acetate, ethanol, or acetone) and then wash again as <strong>for</strong> routine<br />

cleaning.<br />

When cleaning spills be sure to wear proper dress and safety equipment (goggles, gloves, lab coat, full<br />

shoes (no open toes)). If you are in doubt as to your ability to safely clean a large spill or about special<br />

hazards (HCl vapor, <strong>for</strong> example), seek help.<br />

Acids (mineral or organic): saturate the affected area with sodium bicarbonate and allow this to sit <strong>for</strong><br />

several minutes. Wipe the area with a sponge or paper towel (dispose each into an acid waste container).<br />

Test the pH <strong>of</strong> the area by spilling a small amount <strong>of</strong> water and using pH paper. Continue treating with<br />

sodium bicarbonate until the area is neutral. Clean as <strong>for</strong> routine cleaning. Be aware that most acid spills<br />

will create irritating and potentially harmful vapors.<br />

Bases (mineral or amines): soak the area with dilute acetic acid until the area is slightly acidic. Wipe up<br />

the spill with a sponge or paper towel (place either in the acid waste bottle) and wash the area as if there<br />

had been an acid spill. Be aware that highly basic solutions present extreme hazards to the skin and eyes.<br />

Organic solvents: bury the area in vermiculite or some other adsorbant (Spill absorbant material is located<br />

in the <strong>Solvent</strong> room, room # 20, Loading Dock area). Place the spill material in a suitably marked<br />

container. Clean the area as <strong>for</strong> routine cleaning. Be aware <strong>of</strong> vapor hazards!<br />

Organic chemicals: You should clean these as <strong>for</strong> organic solvents with the caveat that the compound may<br />

possess significant health hazards. If you are not aware <strong>of</strong> the particular hazards presented by the spilled<br />

compound, look at an MSDS sheet.<br />

Heavy metals: Be particularly <strong>care</strong>ful cleaning these spills. For small spills, prepare an aqueous solution<br />

<strong>of</strong> EDTA and wipe the area thoroughly with this solution. <strong>Use</strong> a sponge or paper towels and place both or<br />

either in the heavy metal waste container you will prepare. Carefully label the container with contents,<br />

your name, lab, lab phone, date, and secure the container in Salem 20.<br />

Thiols/Thioethers: These compounds present no general safety concern other than their foul stench. Wipe<br />

the affected area several times with bleach. Place the paper towel or sponge in a closed container (Do not<br />

mix bleach and normal organic waste). Continue wiping the area with bleach well after the smell seems<br />

to have dissipated. It is likely that you will become insensitive to the smell. Dispose <strong>of</strong> your gloves and,<br />

possibly, your lab coat depending on the taste/mood <strong>of</strong> your labmates. Be prepared to smell like thiol <strong>for</strong><br />

some time. Clearly mark the container as sulfur containing waste and place the material in Salem 20.<br />

101


9. Dr. Bruce King – Lab Room # 17<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

General Procedure: To clean work surfaces or bench tops, spill area is generally diluted with<br />

water or an organic solvent (acetone) depending upon the contamination. The affected area is then wiped<br />

down with a sponge or mop depending on area and size <strong>of</strong> the contamination.<br />

102


10. Dr. Kondepudi – Lab Room # 5<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Clean up benches with cloth and paper towel impregnated with various solvents (preferably<br />

acetone or hot water and soap).<br />

103


11. Dr. Lachgar – Lab Room # 6<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Lab coat, gloves, and safety glasses must be worn by anyone who is going to clean the bench top<br />

or hood surfaces. Any solid waste will be collected into labeled waste bottles using a brush. Then the<br />

surface will be cleaned using paper towels. Any spilled solution on the bench top will be neutralized if<br />

necessary. Then, the surface will be cleaned using paper towels.<br />

104


12. Dr. N<strong>of</strong>tle – Lab Room # 117<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Follow the spill cleanup procedures <strong>for</strong> specific chemicals described in their MSDS sheets. It is useful to<br />

refer to the shortened lab-scale step-by-step spill procedures listed in the "Hazardous Laboratory<br />

Chemicals Disposal Guide", 2nd edition, kept with the Laboratory Manager or in the Stockroom, room #<br />

110. Vermiculite or clay based kitty litter (bentonit, or processed clay) can be used <strong>for</strong> volatile, common<br />

organic solvent spillage. Neutralizing soda ash or baking soda (Sodium bicarbonate) or Sodium carbonate<br />

is used <strong>for</strong> mineral acids. The neutralized and absorbed materials can be swept up and placed in an<br />

appropriately labeled container and taken to the metal surface table in room # 20. Two five gallon plastic<br />

pails <strong>of</strong> absorbent material (1:1:1 mixture <strong>of</strong> sand, kitty liter, and sodium bicarbonate or baking soda) are<br />

kept in the department <strong>for</strong> general use, one in solvent room #20 and the other in the chemical prep room#<br />

103.<br />

Hydr<strong>of</strong>luoric acid spills should be completely neutralized with 5 to 10% solutions <strong>of</strong> lime<br />

water (calcium hydroxide), two bottles <strong>of</strong> which you will find in room #103, along with a case<br />

<strong>of</strong> solid calcium hydroxide. DO NOT BREATHE FUMES OF HF! Be extremely <strong>care</strong>ful<br />

with Hydr<strong>of</strong>luoric acid. Burns from this material are deeply penetrating and can be deadly,<br />

causing massive tissue damage.<br />

Kitty-liter cannot be used as a spill absorbent <strong>for</strong> Hydr<strong>of</strong>luoric acid, since it will react to<br />

<strong>for</strong>m SiF4, a toxic and corrosive gas. Neither should you use sand, which will also react with<br />

it.<br />

105


13. Dr. Sw<strong>of</strong><strong>for</strong>d – Lab Room # 1<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Exercise <strong>care</strong> in washing lab benches near high voltage electrical equipment. Otherwise, use<br />

paper towels Alternatively, use soap and water to regularly clean <strong>of</strong>f bench top work spaces. Alternatively,<br />

use soap and water to regularly clean <strong>of</strong>f bench top work spaces.<br />

106


14. Dr. Tobey – Lab Room # 2<br />

For routine cleaning, wash using water, followed by acetone, and dry with paper towels. If the spill<br />

contains oily materials first wash with acetone or hexanes and proceed as usual with above cleaning<br />

protocol.<br />

Acids: saturate area with sodium bicarbonate and allow to sit on benchtop . Wipe with paper towels<br />

(dispose appropriately). Test area with pH paper and continue with sodium bicarbonate treatment until<br />

neutral.<br />

Bases: Soak area with dilute acetic acid, wipe and treat area as an acid spill area.<br />

Organic solvent: spread vermiculite (or spill control material located in the solvent room # 20 in the<br />

Loading Dock) over the spill area and dispose <strong>of</strong> the material in an appropriately labeled container.<br />

Organic chemicals: Clean as <strong>for</strong> organic solvent but beware that the components mixtures vary and may<br />

have a specific health hazard. Check MSDS and treat accordingly.<br />

Heavy Metals: For small spills use aqueous solution <strong>of</strong> EDTA and wipe area thoroughly which should be<br />

disposed <strong>of</strong> in separately labeled container.<br />

Alkyl Lithium Reagents: If spilled, it will be extremely pyrophoric – treat by slowly added dry ice to it. DO<br />

NOT POUR WATER onto the affected area.<br />

107


15. Dr. Welker – Lab Room # 13 and 18<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Mercury Spill:<br />

When mercury is spilled on a bench top or floor, begin cleanup immediately. Obtain the mercury<br />

spill kit from laboratory stock room. Wear gloves while working with spill. Consolidate as many droplets<br />

as possible using a piece <strong>of</strong> cardboard. Then use pump contained in the mercury spill kit to collect the<br />

mercury. Place mercury in a thick-wall high-density polyethylene bottle and store in well-ventilated area<br />

(hood, etc.). Do not absorb mercury with the emergency zinc absorbent material in the spill kit unless<br />

absolutely necessary (i.e., unless there is far too much to pick up with the pump).<br />

� If necessary, mercury should be cleaned. See "Specific Procedures <strong>for</strong> Safe Removal <strong>of</strong> Highly Toxic<br />

Waste." It is presently impossible to dispose <strong>of</strong> any sort <strong>of</strong> contaminated mercury.<br />

� General Considerations:<br />

Fires are extinguished using dry chemical extinguishers or sand only. No CO2 or H2O fire extinguishers<br />

can be used. Materials to be considered in lab: nBuLi, t-BuLi, LiAlH4, BCl3, Me2BBr, catechol borane,<br />

BBr3, AlCl3, AlBr3, EtAlCl2, AlMe3, AlEt3, BPh3, PhBCl2.<br />

Removal <strong>of</strong> Lewis Acids and other Organometallics:<br />

Warning: Pyrophoric in air, water, and exposure to mildly acidic environments can be corrosive<br />

to skin, eyes, and respiratory tract. Large Scale Removal: compounds are placed in a container in an inert<br />

atmosphere, labeled, and sent <strong>of</strong>f with an appropriate waste removal service. Small Scale Removal: Small<br />

amounts <strong>of</strong> materials may be "quenched" in an inert solvent in an inert atmosphere by slow addition <strong>of</strong> tbutanol.<br />

The resultant solutions are separated with the organic layer being put into an appropriate waste<br />

container and water layer being added to copious amounts <strong>of</strong> water. Small amounts (


16. Undergraduate Lab Rooms # 7, 101, 102, 103, 104, 105, 106, 111<br />

Specific Decontamination Procedures <strong>for</strong> Equipment and Bench top Surfaces which have come into<br />

contact with Highly Toxic Waste<br />

Include here methods <strong>of</strong> cleaning up work surfaces in hoods or bench tops so as to render traces <strong>of</strong><br />

toxic chemicals benign.<br />

Teaching lab bench tops and hoods in rooms 101 through 111 are primarily the responsibility <strong>of</strong><br />

housekeeping and stockroom personnel. Teaching Assistants are responsible <strong>for</strong> pointing out cleaning<br />

needs and occasionally assisting in such cleanup, themselves. The laboratory managers and teaching<br />

instructors will notify the above mentioned personnel <strong>for</strong> any special cleaning requirements. The students<br />

will also be responsible <strong>for</strong> cleaning their particular work area, especially at the end <strong>of</strong> each semester. It<br />

may be necessary occasionally to clean up organic stains with acetone or ethanol. Mineral acids should<br />

be diluted with water and neutralized with baking soda stored in the back <strong>of</strong> each lab be<strong>for</strong>e cleanup.<br />

Soap is also located on the back window benches <strong>of</strong> each lab. Specific stockroom and housekeeping<br />

assignments are listed under the Housekeeping section <strong>of</strong> this manual.<br />

Stains on the newly renovated Organic Lab benchtops (rooms 102 and 106) can be cleaned with<br />

scrubbing pads soaked with water and baking soda.<br />

If highly toxic waste is generated in any undergraduate lab, specific decontamination procedure<br />

literature references will be included along with actual experimental procedures by the lab instructor.<br />

109


I. Laboratory and Fume Hood Inspections<br />

Laboratory hoods in Salem Hall will be inspected on a regular basis by three methods.<br />

1. Annual inspections <strong>of</strong> hood efficacy will be conducted by a certified Industrial Hygienist, at the<br />

request <strong>of</strong> the WFU Physical Facilities Safety Director. Records <strong>of</strong> these inspections will be maintained by<br />

the Laboratory Manager. The air-flow in research labs should be 100 feet per minute face velocity (fpm).<br />

The air-flow <strong>for</strong> the large hoods located in the rear <strong>of</strong> the undergraduate lab hoods should be 60 fpm. The<br />

air-flow <strong>for</strong> undergraduate individual bench-top fume hoods should be 40 to 50 fpm.<br />

2. The hoods will be checked on an in<strong>for</strong>mal basis by the laboratory manager, periodically. An<br />

"Alnor" brand anemometer, type 8500, will be used. It is stored in the Laboratory Manager's <strong>of</strong>fice.<br />

3. If you have reason to suspect that the air-flow <strong>for</strong> your hood is low, contact the lab manager <strong>for</strong><br />

an anemometer flow measurement. In the meantime, get a large beaker or tray <strong>of</strong> warm water and place it<br />

just inside the hood. Drop some dry ice (CO2) pellets into the water and observe the vapor flow.<br />

The vapors are harmless and relatively dense. If most <strong>of</strong> the vapors are drawn through the back<br />

slots, hood flow is generally appropriate. If most escape into the air in front <strong>of</strong> the hood or drop through the<br />

air-foil opening toward the floor, your air-flow is too low. Call Physical Facilities (phone # 4255) <strong>for</strong><br />

service.<br />

Alternately, you can use smoke generators to qualitatively test the air flow. Order them from Flinn<br />

Scientific, Inc., phone #1-800-452-1261 (catalog # S.E. 5010, 30 second time limit, or catalog #S.E. 5011,<br />

3 minute time limit).<br />

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1. Laboratory Inspection Form<br />

WFU Chem. Dept., Salem Hall, Labroom #_________<br />

1. Are safety devices unobstructed or otherwise operating normally with no overcrowding or interference<br />

from lab operations nearby?<br />

Yes________ No________ Actions necessary <strong>for</strong> resolution <strong>of</strong> problem ____________________<br />

________________________________________________________________________________<br />

Identify specific safety devices obstructed or blocked:<br />

Safety shower _____________________________ Eyewash Fountains__________________<br />

Fire Blanket in Hallway _____________________ CO2 Fire Extinguishers_______________<br />

Class D Fire Extinguisher, if applicable ________<br />

2. Are electrical outlets operating correctly? List those that are loose, damaged, or otherwise being used<br />

in a manner which causes electrical hazards.<br />

Yes________ No________ Actions necessary <strong>for</strong> resolution <strong>of</strong> problem ____________________<br />

________________________________________________________________________________<br />

3. Are lab bench worktops orderly and uncluttered? What about shelves, cabinets, drawers, sinks, and<br />

benchtops in hoods? List anything that needs special attention.<br />

Yes________ No________ Actions necessary <strong>for</strong> resolution <strong>of</strong> problem ____________________<br />

________________________________________________________________________________<br />

4. Are safety glasses worn by all personnel? Has everyone been assigned some <strong>for</strong>m <strong>of</strong> safety eyeglasses<br />

and a pair <strong>of</strong> goggles?<br />

Yes________ No________ Actions necessary <strong>for</strong> resolution <strong>of</strong> problem ____________________<br />

________________________________________________________________________________<br />

5. Are chemicals stored and organized in a generally rational fashion within the room? Are totally<br />

incompatible chemicals kept separated from each other on shelves or cabinets?<br />

Yes________ No________ Actions necessary <strong>for</strong> resolution <strong>of</strong> problem ____________________<br />

________________________________________________________________________________<br />

6. Is ventilation within the room appropriate? Are Phoenix Control monitors and hoods functioning as<br />

intended, without excessive false alarms, blinking warning lights, damaged sash doors, etc.?<br />

Yes________ No________ Actions necessary <strong>for</strong> resolution <strong>of</strong> problem ____________________<br />

________________________________________________________________________________<br />

7. Are carcinogens labeled and stored in Designated Storage Areas? Are Hoods used as Designated Work<br />

Areas? (In other words, are very harmful chemicals handled inside hoods generally? ) Has every ef<strong>for</strong>t<br />

been made to prevent contact with and exposure to Particularly Hazardous Chemicals?<br />

Yes________ No________ Actions necessary <strong>for</strong> resolution <strong>of</strong> problem ____________________<br />

________________________________________________________________________________<br />

8. Are instruments or mechanical devices functioning well? Is oil changed <strong>of</strong>ten in vacuum pumps? Are<br />

damaged rubber or Tygon tubes feeding water to condensers checked and replaced when needed? Are<br />

they properly clamped? Is everything placed at a safe distance away from chemicals and outlets?<br />

Yes________ No________ Actions necessary <strong>for</strong> resolution <strong>of</strong> problem ____________________<br />

________________________________________________________________________________<br />

Form completed by ___________________________ Date ______________________<br />

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J. Laboratory Emergencies<br />

1. Emergency Procedure and First Aid Overview<br />

When a fire, explosion, serious injury, or any other emergency occurs in your Research or<br />

Teaching Laboratory, you should first <strong>of</strong> all ask yourself whether it is safe to stay in the lab and whether<br />

anyone is in need <strong>of</strong> immediate medical attention. If you need any help at all, telephone <strong>for</strong> it from your<br />

lab. The Emergency Phone Number In<strong>for</strong>mation sheet must be posted next to the phone in your lab.<br />

(Naturally, the lab phones in nearby labs will have theirs posted as well, in case you must leave your lab<br />

entirely.)<br />

Please note that two first aid kits are located in the chemistry stockroom, room #110. For minor<br />

emergencies (cuts, burns, minor eye and skin injuries, etc.), please call Student Health Services 24 hours a<br />

day during the regular semester (But not at night during the Summer sessions or during regular semester<br />

holiday periods). Save 911 <strong>for</strong> more serious emergencies (breathing difficulties, deep lacerations, broken<br />

bones, injuries from fires, etc.) All students have access to the stockroom telephone (in room #110) and are<br />

expected to call university emergency personnel if teachers and teaching assistants are occupied with<br />

accident victims.<br />

Tell emergency personnel what happened in as concise a manner as possible. Your goal should be<br />

to contact help quickly and then proceed to do what you can yourself. Remember to give the room number<br />

and location <strong>of</strong> the accident.<br />

Do whatever is necessary to give minimal assistance to injured persons. <strong>Use</strong> whatever medical or<br />

first aid knowledge you have and then stand aside to allow more knowledgeable individuals access. Be<br />

ready to move injured persons away from sources <strong>of</strong> further injury.<br />

As you read this manual, you will become aware <strong>of</strong> the many safety procedures and equipment<br />

available to the chemistry department and in your lab. The more you know, the more help you can give.<br />

The more your co-workers know, the more assistance they can give you.<br />

Be especially cognizant <strong>of</strong> the Poison Control Center, phone # 1-800-848-6946. This is a 24 hour<br />

hotline in<strong>for</strong>mation service which can give you emergency first aid and medical in<strong>for</strong>mation <strong>for</strong> chemical<br />

injuries to specific tissues, organs, and areas <strong>of</strong> the body. You must tell them exactly what chemical the<br />

victim was injured with if you expect them to help you. This is a very good service. If necessary, they will<br />

fax specific in<strong>for</strong>mation directly to the chemistry department’s fax machine located in the chemistry <strong>of</strong>fice,<br />

room #110C, fax # 336-758-4656 with the physician’s permission only.<br />

Your Research Laboratory should have a first aid kit available. If it does not, use the kits located<br />

in the stockroom, room #110.<br />

There are two chemical first aid books located above the MSDS sheet collection, near the first aid<br />

kits, and across the room from the emergency breathing apparatus in the Chemistry Department stockroom,<br />

#110. PLEASE REVIEW THESE BOOKS SO THAT YOU WILL BE PREPARED TO MAKE USE<br />

OF THEM SHOULD THE NEED ARISE.<br />

a) Effects <strong>of</strong> Exposure to Toxic Gases: First Aid and Medical Treatment, 3rd Edition, Matheson<br />

Gas Products, Inc., 1988.<br />

b) Lefevre, Marc J., and Conibear, Shirley A. First Aid Manual <strong>for</strong> Chemical Accidents, 2nd<br />

Edition. New York: Van Nostrand Reinhold, 1989.<br />

112


2. Chemical Fire and Large Building Fire Emergency Procedures:<br />

Basically, we do not expect the fire department to encounter any special hazard in putting out fires<br />

in our labs in Salem Hall because we try to keep any chemicals in large quantities stored in specially<br />

designed storage rooms in the loading dock, both <strong>of</strong> which are protected heavily with overhead dry power<br />

extinguisher systems. Small chemical fires in a particular laboratory can generally be extinguished using<br />

the following method:<br />

a) The firefighter should wear self-contained breathing apparatus (SCBA) if toxic fumes from<br />

collections <strong>of</strong> small bottles are emitted at all while burning.<br />

b) <strong>Use</strong> the yellow, portable 30 lb. “Class D” fire extinguisher, one <strong>of</strong> which is placed in each lab<br />

requiring them ( 6 in all, located in room #‟s 2, 13, 14, 16, 19, and 115). They are used <strong>for</strong><br />

smothering water-sensitive or water-reactive chemical fires. They extinguish burning metallic<br />

chemical fires involving magnesium, lithium, sodium, and potassium; and in general, metal<br />

hydrides (like Lithium Aluminum Hydride and sodium hydride, popular chemicals used in the<br />

organic labs in room #‟s 13, 14, 17, 18 <strong>of</strong> Salem Hall) and organometallic chemicals used in room<br />

#13 primarily. These “Class D” extinguishers could also be used to put out other solid chemical<br />

fires in conjunction with dry power extinguishers (which are better <strong>for</strong> non-metallic solid chemical<br />

fires). If one room‟s “Class D” extinguisher is expended, have someone else collect those from<br />

other nearby rooms. <strong>Use</strong> other smaller dry power extinguishers in the area as needed. We have<br />

two large portable 30 LB CO2 extinguishers, one in room #20, the other in the stockroom, #110,<br />

which we would use <strong>for</strong> organic solvent liquid fires only - not solid chemical fires.<br />

c) If the fire has grown too large to extinguish by this method, then it is time to use water hoses<br />

and saturate the entire room corner or the entire room with water. It is the opinion <strong>of</strong> the<br />

Chemistry Department faculty that with an entire room in flames, the destruction <strong>of</strong> small<br />

containers <strong>of</strong> water-sensitive chemicals via water from water hoses is a small price to pay - they<br />

will be neutralized or otherwise rendered benign with huge volumes <strong>of</strong> water and should not then<br />

present a problem to firefighters, especially if they are wearing the a<strong>for</strong>ementioned self-contained<br />

Breathing Apparatus (SCBA).<br />

The only major fire hazard present in research labs are compressed gas cylinder bottles.<br />

The smaller lecture bottles could be worse, potentially, since some <strong>of</strong> these are poisonous gases,<br />

any <strong>of</strong> which could explode if the temperature is high enough during a fire. Please note that exact<br />

locations <strong>of</strong> all compressed gases, including lecture bottles, will be listed in the last chapter <strong>of</strong> this<br />

manual.<br />

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3. Chemical Spills<br />

Chemical spills in all laboratories should be promptly dealt with and properly reported. Small<br />

spills can in most cases be cleaned up by the lab worker without much trouble. Spills <strong>of</strong> particularly<br />

hazardous chemicals (see section III.F <strong>of</strong> this manual) must be reported to the lab manager and appropriate<br />

precautions taken during your cleanup. Large-scale chemical spills may require room evacuation, or , in<br />

unusual circumstances, a building evacuation. Consult also with more knowledgeable colleagues and your<br />

research advisor or teacher.<br />

Large spills which cannot be contained by you or those helping you in the chemistry department<br />

will be taken <strong>care</strong> <strong>of</strong> by the university's Safety Response Team, supervised by the WFU Physical Facilities<br />

Assistant Safety Director. Call Scott Frazier [WFU Assistant Environmental Health and Safety (EHS)<br />

Director] and in<strong>for</strong>m him what was spilled and the location <strong>of</strong> the spill. His phone # is 4329 (or 4224). Do<br />

not expect anyone to clean up the spill without your assistance.<br />

You should follow these rules when a spill occurs:<br />

1) In<strong>for</strong>m people in the immediate vicinity <strong>of</strong> the spill right away.<br />

2) Administer or receive first aid or attempt to rapidly remove the chemical if exposed to it by<br />

skin contact. This generally means washing with a great deal <strong>of</strong> water. If other procedures<br />

should be followed, you will know what they are, since you should know the harmful affects<br />

<strong>of</strong> the chemical and first aid procedures be<strong>for</strong>e you begin work.<br />

3) Minimize the spread <strong>of</strong> the spill if you can do it without injuring yourself by contact with<br />

corrosive or otherwise toxic fumes or liquids.<br />

4) Clean up the spill.<br />

How you will clean up the spill will, <strong>of</strong> course, depend on what you are working with in your lab.<br />

Again, do not expect the university's Safety Response Team to automatically do it <strong>for</strong> you. They are not<br />

chemists. Spill cleanup procedures <strong>for</strong> specific chemicals are clearly described in their MSDS sheets. It<br />

will usually be more useful to refer to the shortened lab-scale step-by-stop spill procedures listed in Armour,<br />

M. A. Hazardous Laboratory Chemicals Disposal Guide, 2nd edition. Boston: CRC Press, 1996, kept in<br />

the Lab Manager’s <strong>of</strong>fice, room # 9A. These procedures are listed in the "Spillage Disposal" section <strong>for</strong><br />

each chemical. You are requested to skim through this book and thereby be more fully aware <strong>of</strong> the<br />

extremely useful and pertinent in<strong>for</strong>mation therein.<br />

The usual method <strong>of</strong> cleaning up a spill involves diluting it with water if it is aqueous, neutralizing<br />

it if it is corrosive, and finally adsorbing the liquid with an inert adsorbent material so that it can be swept<br />

up and placed in an appropriate labeled container and taken to the metal-covered table in room #20 <strong>for</strong><br />

removal via a waste disposal company. Label this container as containing spillage material and list the<br />

specific chemical name <strong>of</strong> the spilled chemical or chemicals. Mineral acids are diluted with water and<br />

neutralized by sprinkling with baking soda or sodium carbonate or diluting it with solutions <strong>of</strong> sodium<br />

hydroxide. Generally alkaline or basic solutions can be neutralized with dilute solutions <strong>of</strong> hydrochloric<br />

acid, although this <strong>of</strong> course depends on the chemical.<br />

Again, consult with your research director, teacher or appropriate references be<strong>for</strong>e proceeding.<br />

Volatile, common organic solvents can generally be adsorbed on vermiculite or, preferably, clay<br />

based kitty litter (called bentonite) both <strong>of</strong> which are kept in room #20 <strong>for</strong> general use. A large container <strong>of</strong><br />

neutralizing soda ash <strong>for</strong> mineral acids is kept near the acid bins in room #19. You should keep containers<br />

<strong>of</strong> some type <strong>of</strong> adsorbent material on hand in your laboratory.<br />

Two large containers <strong>of</strong> calcium carbonate are kept in room #103, the prep room. Very dilute<br />

solutions <strong>of</strong> baking soda and acetic acid are kept in the undergraduate labs <strong>for</strong> caustic burns (do not clean<br />

out eyes with anything but pure water.)<br />

114


Research hoods are great places to have spills, and are much better than open lab benches or<br />

floors. These hoods have working bench surfaces which are fringed with slightly raised beveled edges,<br />

serving as convenient wide-area containment trays.<br />

There are as many ways to clean up spills as there are chemicals. Consult the literature <strong>for</strong> your<br />

particular problem substances. Remember that many chemicals react strongly and dangerously with water,<br />

and that paper towels soaked with certain chemicals can be very flammable and too hazardous to deposit in<br />

the trash cans.<br />

Sweep the neutralized and absorbed material into a dust bin with a hand broom (located in the<br />

stockroom, room #110, if you don't have them in your lab) while wearing gloves and safety glasses.<br />

The most common spill adsorbent listed in the procedures in the CRC Hazardous Laboratory<br />

Chemicals Disposal Guide is a 1:1:1 mixture by weight <strong>of</strong> sodium carbonate, clay cat litter (bentonite), and<br />

sand. A large container <strong>of</strong> this material is kept in the prep room, # 103 and in the solvent room, #20. It is<br />

labeled as follows:<br />

Chemical Spill Adsorbent<br />

1:1:1 Sodium Bicarbonate,<br />

Kitty litter and Sand<br />

and keep it in a conspicuous area in your lab. You may use baking soda (sodium bicarbonate) instead <strong>of</strong><br />

sodium carbonate. The University Safety Response Team will also have large amounts <strong>of</strong> this material on<br />

hand. It will not always be appropriate to use this material. Again, it depends on what was spilled. Consult<br />

the literature and plan ahead.<br />

SPECIFIC EMERGENCY CHEMICAL SPILL INFORMATION<br />

FOR THE SPILL RESPONSE TEAM (SRT) AND GRADUATE STUDENTS<br />

Call 4329 or 4224 <strong>for</strong> immediate response from the University Safety Response Team <strong>for</strong><br />

large spills. If the spill can be easily contained by you or your instructor or co-lab workers,<br />

obtain the CHEMICAL SPILL ABSORBENT material or baking soda boxes from the<br />

chemical prep room, #103 or the solvent room #20 (loading dock area).<br />

GO TO THESE TWO ROOMS BEFOREHAND AND NOTE THE LOCATION OF THIS<br />

MATERIAL FOR FUTURE REFERENCE.<br />

You will also find two large containers <strong>of</strong> Calcium carbonate, 2 bottles <strong>of</strong> 5% hydrochloric<br />

acid solution, bottles <strong>of</strong> sodium bisulfite, and calcium sulfate.<br />

Hydr<strong>of</strong>luoric acid spills should be completely neutralized with 5 to 10% solutions <strong>of</strong> lime<br />

water (calcium hydroxide), two bottles <strong>of</strong> which you will find in room #103, along with a case<br />

<strong>of</strong> solid calcium hydroxide. DO NOT BREATHE FUMES OF HF! Be extremely <strong>care</strong>ful<br />

with Hydr<strong>of</strong>luoric acid. Burns from this material are deeply penetrating and can be deadly,<br />

causing massive tissue damage.<br />

Kitty-liter cannot be used as a spill absorbent <strong>for</strong> Hydr<strong>of</strong>luoric acid, since it will react to<br />

<strong>for</strong>m SiF4, a toxic and corrosive gas. Neither should you use sand, which will also react with<br />

it.<br />

Safety Response Team<br />

When the Safety Response Team (SRT) answers your call, among their questions will be the<br />

following:<br />

115


a) Is your spill large enough to justify a special trip? Are you in a position to clean<br />

up the spill yourself? (Overreacting is not a good idea!)<br />

b) What is the location <strong>of</strong> the Research Director or teacher <strong>for</strong> your group?<br />

c) Can you communicate to us the means <strong>of</strong> chemically neutralizing your<br />

particular spill? If not, are you willing to help anyway? If you are willing to work<br />

with lab chemicals, you had better be willing to help clean up your own spills. The<br />

SRT people have the right to leave if you are not willing to help.<br />

In general, spills <strong>of</strong> over 5 gallons <strong>of</strong> non-corrosive organic solvents or over one<br />

gallon <strong>of</strong> corrosive organic solvents justify a response from the SRT.<br />

Ruptures or leaks <strong>of</strong> the fifty-five gallon drums <strong>of</strong> acetone in room #20, the 55 gallon<br />

drums marked “Hazardous Waste” <strong>of</strong> waste organic solvents in the <strong>Solvent</strong> Room, or the<br />

numerous 5 gallon smaller drums <strong>of</strong> organic solvents in that room also warrant a visit from<br />

the SRT. They can all be absorbed with a 1:1:1 mixture <strong>of</strong> sand, kitty litter, and sodium<br />

bicarbonate.<br />

Spills <strong>of</strong> aqueous inorganic salts don’t ordinarily require an SRT response, since<br />

they do not normally exhibit corrosive properties or fumes. Mineral acids must be<br />

neutralized, however, and the more acidic they are, the more corrosive they are going to be.<br />

They should first be diluted with water.<br />

When the SRT arrives, they will be wearing respirators, thick gloves and boots, or<br />

possibly self-contained breathing apparatus (SCBA). They will probably “dike” the spill,<br />

i.e., surround it with a small mound or dike <strong>of</strong> absorbent material. Organic solvents will in<br />

general be absorbed with a 1:1:1 mixture <strong>of</strong> sand, kitty-litter, and sodium bicarbonate, as<br />

will aqueous mineral acids and corrosive organic acids.<br />

If you cannot answer their questions about the particular chemical spilled, you<br />

should at least try to find someone who does, and you must participate in helping with spill<br />

containment.<br />

The first thing the SRT will do is attempt to locate spill absorbing in<strong>for</strong>mation <strong>for</strong><br />

the particular chemical involved. If they cannot locate it in their copy <strong>of</strong> the CRC,<br />

Hazardous Laboratory Chemicals Disposal Guide, they may need your advice. In the event<br />

that they can find it in the book, the relevant section in CRC <strong>for</strong> that particular chemical<br />

under its alphabetical chemical name listing is “spillage disposal”.<br />

If a spill response team member cannot readily identify a spilled chemical, they will<br />

employ the following method:<br />

(a) Dike the spill with 1:1:1 mixture <strong>of</strong> sand, kitty-litter, and sodium bicarbonate<br />

(b) Cautiously reach toward the spill and sprinkle above mixture onto surface <strong>of</strong><br />

liquid. If vigorous fuming and reaction occurs, back-<strong>of</strong>f and reconsider the<br />

situation (you at least know that the solution is acidic). Then sprinkle a little<br />

water on the spill. Does water dissolve in the solvent? If so, dilute it with more<br />

water and then dump enough 1:1:1 absorbent material on the spill to fully<br />

absorb it. Let it dry awhile, then sweep it into a container <strong>for</strong> storage. It is<br />

preferable to store it in a hood. If water reacts violently with the solvent,<br />

<strong>care</strong>fully dump the absorbent material only (without diluting with water), over<br />

the pool solvent while attempting to keep as much distance between yourself<br />

and any fumes generated. <strong>Use</strong> the 1:1:1 mixture <strong>of</strong> sand, kitty-litter, and<br />

sodium bicarbonate as a nearly universal absorbent. If it does not work as well<br />

as it should, at least it will absorb the material until you can find the right way<br />

to neutralize the liquid. Spread the mixture on the spill and <strong>care</strong>fully scoop it<br />

into one <strong>of</strong> your white polyethylene trays. Then put it in a nearby hood and<br />

keep it there until you find someone who can tell you how to neutralize it.<br />

(c) If you can’t find the name <strong>of</strong> the chemical in the CRC Waste Disposal Book, ask<br />

a nearby graduate student or pr<strong>of</strong>essor to point out chemicals which are named<br />

in the book, which most closely resemble the spilled chemicals in terms <strong>of</strong><br />

chemical property or structure.<br />

116


K. Provisions <strong>for</strong> medical exams, consultation & exposure assessments<br />

written by Julianne Braun, grad student, and M. Thompson, Lab Manager<br />

1. A Guide to OSHA Air Concentration Acronyms<br />

OSHA regulations require workers to be guarded against excessive exposure to chemical vapors<br />

when working in a lab. If you are routinely exposed over the Permissible Exposure Level, you must request<br />

that the chemical vapor be monitored by the University appointed Industrial Hygienist. Be<strong>for</strong>e you decide<br />

whether or not a particular exposure situation in your laboratory requires air-monitoring, you must have a<br />

clear conception <strong>of</strong> what OSHA means by a permissible exposure level. They were derived from threshold<br />

limit values.<br />

Threshold limit values (TLVs) are definite numerical chemical air-concentration safety limits<br />

determined by the American Council <strong>of</strong> Governmental and Industrial Hygienists (ACGIH, an advisory data<br />

review agency) and are expressed in 3 different ways. They are quantitative limits to which lab workers<br />

may be exposed without adverse effects. The TLVs may take the <strong>for</strong>m <strong>of</strong> Time Weighted Averages<br />

(TWAs), Short-term Exposure Limits (STELs), or Ceiling Limits (CLs). You may sometimes see these<br />

limits described in an incidental 4th way in MSDS sheets as NOEALs (No Observable Adverse Effect<br />

Levels). TWAs are usually based on 8-hour time periods. TWAs are not necessarily concentrations to<br />

which a person's exposure should not be exceeded at any point in time, but are really time weighted<br />

averages. For example, if a TWA is given as 100 parts per million, it may be OK to be exposed to 200 ppm<br />

<strong>for</strong> 4 hours and to 0 ppm <strong>for</strong> the next four hours (time weighted exposure would then be 200 ppm x 4 hours<br />

+ 0 ppm x 4 hours = 800 ppm divided by a total <strong>of</strong> 8 hours = 100 ppm). STELs are similar to TWAs, but<br />

are based on exposure <strong>for</strong> only 15 minutes. Ceiling Limits are levels which cannot be exceeded <strong>for</strong> any<br />

length <strong>of</strong> time, period. They are assigned <strong>for</strong> chemicals which are reported to be acutely toxic.<br />

"TWAs permit excursions above the TLV provided they are<br />

compensated by equivalent excursions below the TLV during the workday".<br />

"For the vast majority <strong>of</strong> substances with a TWA, there is not<br />

enough toxicological data available to warrant a STEL. Nevertheless,<br />

excursions above the TWA should be controlled even where the 8- hour TWA is<br />

within recommended limits".<br />

"Excursions in worker exposure levels may exceed 3 times the TLV<br />

<strong>for</strong> no more than a total <strong>of</strong> 30 minutes during a workday, and under no<br />

circumstances should they exceed 5 times the TLV, provided that the TWA is not<br />

exceeded." (Threshold Limit Values <strong>for</strong> Chemical Substances and Physical<br />

Agents in the workroom environments, ACGIH, 1995).<br />

When OSHA adopted the ACGIH threshold limit values (TLVs), confirming their validity by<br />

incorporating them into employee safety laws, they were subsequently referred to as permissible exposure<br />

levels (PELs). These are the legal concentrations <strong>of</strong> hazardous chemicals the government permits<br />

employees to be exposed to <strong>for</strong> the associated length <strong>of</strong> time. PELs include TWAs, STELs, and CLs. In<br />

addition, OSHA defined "action levels" as TWAs. There are many references in the relevant law in the<br />

code <strong>of</strong> Federal Regulations (29 CFR 1910. 1450 or "Laboratory Standard") to certain provisions <strong>for</strong> airmonitoring<br />

which go into effect when these values are exceeded in the lab. One encounters descriptions <strong>of</strong><br />

employee exposure over the "action level (or in the absence <strong>of</strong> an action level, the PEL)". This essentially<br />

means that if a particular chemical hasn't been assigned a TWA, it is covered by one or the other type <strong>of</strong><br />

PEL, namely a STEL or a CL.<br />

“Many <strong>of</strong> the newer legal limits established by OSHA include an action level concept,<br />

typically 50% <strong>of</strong> the OSHA PEL, at which an employer is to take action to reduce the<br />

level or to ensure that the 8-hour time-weighted PEL is not exceeded.” Furr, Keith A.<br />

CRC Handbook <strong>of</strong> Laboratory Safety, 4th Ed. Boca Raton, Fl: CRC Press, 1995, p. 414<br />

117


The PELs are listed in OSHA's so called "Subpart Z list", referenced as 29 CFR 1910.1000,<br />

Subpart Z, Toxic and Hazardous Substances. Tables Z-1 through Z-3 are best seen at . TWAs, or "action<br />

levels", are listed <strong>for</strong> each particular chemical. In the absence <strong>of</strong> TWAs, CLs are listed. Chemicals which<br />

have STELs are referenced as Substance Specific Standard chemicals, located in 29 CFR 1910. 1001-1050.<br />

Units<br />

Caution should be used in determining whether or not the various regulatory limits <strong>for</strong> air contaminants<br />

have been exceeded. The majority <strong>of</strong> regulatory limits (as presented in the “Z” tables) are listed in two<br />

different sets <strong>of</strong> units: ppm-volume and mg/m 3 . The units are different, but the concentrations are the<br />

same! From the ideal gas law, PV=nRT, it can be seen that at atmospheric pressure and room temperature<br />

the volume <strong>of</strong> a gas, V, will be proportional only to the number <strong>of</strong> moles <strong>of</strong> the gas, n. There<strong>for</strong>e when<br />

concentrations <strong>of</strong> an air contaminant are expressed as ppm(volume), what is being expressed is the volume<br />

<strong>of</strong> contaminant per million volumes <strong>of</strong> air which has nothing to do with the weight <strong>of</strong> the contaminant or the<br />

air. When contaminant concentrations are expressed as mg/m 3 , the molecular weight <strong>of</strong> the contaminant is<br />

important. To convert ppm(volume) to mg/m 3 , the following equation can be used. Note that this equation<br />

is valid at 1 atmosphere pressure and 25 degrees Centigrade. If you are measuring concentrations at high<br />

altitudes where pressure is lower or in rooms where the temperature is much warmer or cooler than 25<br />

degrees, the number <strong>of</strong> liters <strong>of</strong> volume occupied by one mole <strong>of</strong> a gas may be recalculated from the ideal<br />

gas law.<br />

mg Liters <strong>of</strong> contaminant grams 1 mole 1000 Liters<br />

� � � � �<br />

3 3<br />

m 1,000,000<br />

Liters <strong>of</strong> air mole 24. 45 Liters 1 meter<br />

1000<br />

1<br />

Note that the million from the ppm(volume) cancels the 1000 L/m 3 x 1000 mg/g so the equation can be<br />

simplified to<br />

2. Air Monitoring<br />

mg<br />

� ppm � molecular weight �<br />

3<br />

m<br />

1<br />

24. 45<br />

mole<br />

Liters<br />

OSHA requires two types <strong>of</strong> air monitoring when substances <strong>for</strong> which PELs have been adopted<br />

are in use. The first type is "initial monitoring". As indicated in 29CFR1910.1450(d)(1), the employer<br />

must "measure the employee's exposure to any substance regulated by a standard which requires monitoring<br />

if there is reason to believe that exposure levels <strong>for</strong> that substance routinely exceed the action level (or in<br />

the absence <strong>of</strong> an action level, the PEL)". The key to this is whether or not a standard exists <strong>for</strong> that<br />

substance and whether or not there is reason to believe that exposure levels routinely exceed the standard.<br />

Because <strong>of</strong> the way OSHA defines action level, it is appropriate to interpret TWA as "action level". For<br />

instance, if you use something in a lab only once, there's no point in taking air samples to determine an<br />

exposure level because by the time you've analyzed the samples the exposure will have ended. On the other<br />

hand, if you routinely per<strong>for</strong>m a particular procedure involving a substance <strong>for</strong> which a PEL has been<br />

established, the concentration to which you are exposed during that procedure should be measured.<br />

The second type <strong>of</strong> air monitoring is "periodic monitoring". As indicated in 29CFR1910.1450(d),<br />

the employer must "comply with exposure monitoring provisions <strong>of</strong> the relevant standard" if the initial<br />

monitoring discloses employee exposure over the action level (or in the absence <strong>of</strong> an action level, the<br />

PEL). This essentially means that if initial monitoring shows that any <strong>of</strong> the concentration limits are<br />

exceeded, then the air concentration <strong>of</strong> that particular chemical should be measured periodically on a<br />

regular schedule. The frequency <strong>of</strong> monitoring varies according to the specific substance being monitored<br />

and how <strong>of</strong>ten the procedure that results in exposure is used in the lab.<br />

mg<br />

g<br />

118


If and when air-monitoring in your laboratory becomes necessary according to the above criteria,<br />

in<strong>for</strong>m the Chemistry Department Laboratory Manager or the WFU Safety Director so that an Industrial<br />

Hygienist may be contracted to install air pumps and air sampling tubes.<br />

Alternately, the Chemistry Department can purchase constant flow air sampler pumps (from SKC<br />

Company, model # 224-PCXR4) and Drager air sampling tubes from SKC or Fisher Scientific Company.<br />

Please contact Mr. Scott Frazier [WFU Assistant Environmental Health and Safety (EHS) Director], <strong>for</strong><br />

specific details on training <strong>for</strong> air-monitoring devices.<br />

Air-monitoring is critical if you cannot readily reduce the exposure. You must take steps to ensure<br />

that you are working below the PEL, as soon as possible. For starters, it is suggested that you either do all<br />

<strong>of</strong> your work in a hood or devise engineering controls mentioned elsewhere in this manual to reduce<br />

exposure.<br />

3. Medical Monitoring<br />

There are 3 circumstances under which the employer must provide the opportunity <strong>for</strong> medical<br />

monitoring due to chemical exposure. These are:<br />

1. When an employee develops signs or symptoms associated with a hazardous chemical to<br />

which the employee may have been exposed in the laboratory.<br />

2. When air monitoring reveals an exposure level routinely above the action level (or in the<br />

absence <strong>of</strong> an action level, the PEL) <strong>for</strong> a regulated substance and<br />

3. When an event takes place such as a spill, leak, explosion or other occurrence resulting in the<br />

likelihood <strong>of</strong> a hazardous exposure.<br />

When there is an obvious need <strong>for</strong> treatment, medical monitoring is not applicable. First aid<br />

emergency in<strong>for</strong>mation is covered in section III.K.4 <strong>of</strong> this manual. The medical monitoring requirement <strong>of</strong><br />

the OSHA Lab Standard is designed to protect employees from long term exposure.<br />

When and if lab personnel experience any <strong>of</strong> the above 3 types <strong>of</strong> chemical exposure, an exposure<br />

assessment must be conducted. Fill out the appropriate section on the Accident Report Form, entitled<br />

"Exposure Assessment", which contains the following questions:<br />

* Which chemical, or chemicals, used by the lab worker resulted in the exposure? If unknown,<br />

which chemicals in the immediate vicinity <strong>of</strong> the exposure might have been responsible?<br />

* Describe the lab work situation which led to the exposure. How did physical contact with the<br />

chemical occur?<br />

* What safety devices, from hoods to safety glasses or gloves, etc., were or were not used during<br />

the exposure?<br />

* What signs or symptoms associated with chemical exposure were exhibited by the employee,<br />

such as skin rashes, unusually excessive allergies, breathing difficulties, corrosive injuries, etc.<br />

The medical monitoring begins with a "consultation". This entails filling out a 5 to 6 page long<br />

medical questionnaire (the questions are all included in the federal regulations as an appendix, and will be<br />

provided by the WFU Safety Director) which gets reviewed by a licensed physician who determines<br />

whether or not there is a need <strong>for</strong> a medical examination. The physician must prepare a written opinion and<br />

the employee must be notified and allowed to obtain a copy <strong>of</strong> the opinion. The opinion may call <strong>for</strong><br />

examination and any appropriate medical tests which the employer must provide. The written opinion<br />

(based on consultation and/or any follow-up examinations and tests) shall not reveal specific findings <strong>of</strong><br />

diagnoses unrelated to occupational exposure.<br />

119


4. In<strong>for</strong>mation Regarding Student First Aid and Medical Insurance<br />

Please note that two first aid kits are located in the chemistry stockroom, room #110, underneath<br />

the phone. This phone, # 4712, is <strong>for</strong> emergency use only. For minor emergencies (cuts, burns, minor eye<br />

and skin injuries, etc.) please call Student Health Services 24 hours a day during the regular semester at<br />

phone # 5218, but not at night during the summer sessions or during regular semester holiday periods.<br />

During these periods, call Concentra Medical Center at 4410 Providence Lane, Suite I (<strong>of</strong>f North Point<br />

Boulevard), phone # 896-9999. Save 911 <strong>for</strong> more serious emergencies (breathing difficulties, deep<br />

lacerations, broken bones, injuries from fires, etc.) or medical emergencies that fall outside the range <strong>of</strong><br />

operational hours with either Student Health Services or the Concentra Medical Center on North Point<br />

Boulevard.<br />

DO NOT WEAR CONTACT LENSES in laboratories with constant exposure to chemical vapors,<br />

especially organic solvent fumes. In addition to trapping chemical vapors and concentrating them between<br />

the lenses and the eye and causing irritation, washing out your eyes is impossible. It is better to wear<br />

prescription lenses <strong>for</strong> chemical lab work and cover them with Departmental “Wraparound‟ Safety Glasses<br />

or full size goggles.<br />

Teaching Assistants and Pr<strong>of</strong>essors who witness minor student accidents should assist ins<strong>of</strong>ar as<br />

they are able and then transport or otherwise accompany the individual to Student Health Services on the<br />

ground floor <strong>of</strong> the Reynolds Gymnasium. More serious accidents may require transportation <strong>of</strong> the victim<br />

to Concentra Medical Center at 4410 Providence Lane, Suite I (<strong>of</strong>f North Point Blvd., phone # 896-9999).<br />

A Chemistry Department accident report <strong>for</strong>m must be completed <strong>for</strong> all Chemistry Department accidents.<br />

Forms are located in the black filing cabinet in the stockroom # 110.<br />

All undergraduate students should have health insurance be<strong>for</strong>e enrolling <strong>for</strong> classes. The following<br />

in<strong>for</strong>mation regarding student health insurance is provided by the University at:<br />

http://www.wfu.edu/administration/fas/ar/student_health_insurance.html<br />

“Wake Forest University is concerned that all students have adequate health insurance coverage. For<br />

students not covered under a parent's health plan, we strongly suggest obtaining insurance coverage. A<br />

Student Injury and Sickness Plan is available through Student Resources. A summary <strong>of</strong> the coverage and<br />

benefits <strong>of</strong> this plan is available on their website at www.student-resources.net. Wake Forest does not <strong>of</strong>fer<br />

or sponsor any plan <strong>of</strong> insurance, and this link is provided so that you might make an in<strong>for</strong>med choice. Each<br />

student is urged to investigate available options and determine which health insurance company has a policy<br />

best suited to their particular needs.” Contact Student Health Services (at phone # 5218) <strong>for</strong> any further<br />

questions you may have regarding student health insurance options.<br />

All graduate students are required to have health insurance be<strong>for</strong>e enrolling in classes. In<strong>for</strong>mation and<br />

enrollment <strong>for</strong>ms are located at the Graduate School website:<br />

http://www2.wfubmc.edu/graduate/RChealth.html. Research students, either graduate or undergraduate,<br />

who are <strong>of</strong>ficially paid by the university and have accidents should take a copy <strong>of</strong> the completed Chemistry<br />

Department Accident Report <strong>for</strong>m with them to the Human Resources Department in Reynolda Hall, room<br />

# 21, phone # 4945, where they will fill out yet another <strong>for</strong>m, the “First Report <strong>of</strong> Incident” <strong>for</strong>m, with Ms.<br />

Mimi Komos <strong>for</strong> insurance purposes.<br />

Any research workers in the Department not <strong>for</strong>mally enrolled and not being paid by the<br />

University (i.e., visiting Post-Doctorates, students from other schools, etc.) are not automatically covered by<br />

University insurance and are not eligible <strong>for</strong> worker‟s compensation claims. They are responsible <strong>for</strong><br />

obtaining their own medical insurance.<br />

120


5. Worker’s Compensation Procedures and Reporting In<strong>for</strong>mation<br />

(From Mimi Komos at komosmd@wfu.edu or phone number 4945)<br />

Evaluations <strong>of</strong> on-the-job injuries and occupational illnesses are to be referred to Concentra Medical<br />

Center, located at 4410 Providence Lane, <strong>of</strong>f North Point Boulevard. Concentra's hours <strong>of</strong> operation are<br />

Monday-Friday, 8:00 a.m. - 5:00 p.m.<br />

For non-life threatening situations that require medical evaluation immediately, report the illness or injury<br />

to the supervisor, Workers' Compensation Coordinator (x4945) and the Safety and Environmental Affairs<br />

Office (x4224 or x4329) be<strong>for</strong>e seeking appropriate medical attention. The Workers' Compensation<br />

Coordinator or the Safety and Environmental Affairs Office can be contacted <strong>for</strong> a referral appointment to<br />

Concentra Medical Center.<br />

In the event <strong>of</strong> a serious, life threatening situation, dial 911 and the appropriate medical pr<strong>of</strong>essionals<br />

will direct and/or transport patients to the Baptist Hospital Emergency Care Facility. The Safety Response<br />

Team can be dispatched to the scene <strong>for</strong> immediate assistance, Monday-Friday, 8:00 a.m. - 4:30 p.m. by<br />

calling Facilities Management Customer Service at x4255. In addition, when school is in session, the<br />

Student Response Team, under the direction <strong>of</strong> Dr. Cecil Price <strong>of</strong> Student Health Service, is available "after<br />

hours" and weekends by calling Campus Police at x5591.<br />

If a non-life threatening incident occurs after normal work hours, PrimeCare Medical Center, located at<br />

7811 North Point Boulevard, may be used as a back-up to Concentra. PrimeCare is open:<br />

8:00 a.m. - 8:00 p.m. Monday - Friday<br />

8:00 a.m. - 6:00 p.m. Saturday<br />

12:00 p.m. - 6:00 p.m. Sunday<br />

A confidential First Report <strong>of</strong> Incident Report must be completed <strong>for</strong> all injuries or<br />

illnesses as soon as possible and submitted to the Workers‟ Compensation Coordinator (x4945). Copies <strong>of</strong><br />

this and other Human Resources <strong>for</strong>ms are available http://www.wfu.edu/hr/<strong>for</strong>ms/index.html<br />

Claims inquiries are to be directed to Risk Management, Wake Forest University Baptist<br />

Medical Center by calling the Claims Manager, at 716-5575. If you have other questions or<br />

concerns regarding Workers' Compensation, please contact Mimi Komos at komosmd@wfu.edu<br />

or x4945.<br />

Additional in<strong>for</strong>mation on this and other policies can be found through the World Wide Web at:<br />

http://www.wfu.edu/hr/policies/index.html<br />

121


6. Accident and Chemical Exposure Assessment Report<br />

Chemistry Department, Salem Hall<br />

Wake Forest University<br />

Name <strong>of</strong> person(s) involved in accident or injury ___________________________________________<br />

undergraduate student___ graduate student___ Date and time <strong>of</strong> accident/injury_______________<br />

Was the individual(s) a university paid research student? yes____ no___<br />

Was the individual(s) a faculty or university staff member? Yes___ no___<br />

Where in Salem Hall did the accident occur? _____________________________________________<br />

Was first aid administered? Yes_____ no____ If yes, by whom? __________________________<br />

How was first aid administered? ________________________________________________________<br />

Describe the accident and what caused it __________________________________________________<br />

___________________________________________________________________________________<br />

___________________________________________________________________________________<br />

___________________________________________________________________________________<br />

___________________________________________________________________________________<br />

___________________________________________________________________________________<br />

____________________________________________________________________________________<br />

___________________________________________________________________________________<br />

___________________________________________________________________________________<br />

___________________________________________________________________________________<br />

___________________________________________________________________________________<br />

List witnesses to the accident, if any ______________________________________________________<br />

What can be done to prevent this type <strong>of</strong> accident from happening again? ________________________<br />

___________________________________________________________________________________<br />

___________________________________________________________________________________<br />

___________________________________________________________________________________<br />

Chemical Exposure Assessment (if applicable)<br />

* Which chemical or chemicals used by the lab worker resulted in the exposure? If unknown,<br />

which chemicals in the immediate vicinity <strong>of</strong> the exposure might have been responsible?<br />

* Describe the lab work situation which led to the exposure. How did physical contact with the<br />

chemical occur?<br />

* What safety devices, from hood to safety glasses or gloves, etc., were or were not used during<br />

the exposure?<br />

* What signs or symptoms associated with chemical exposure were exhibited by the employee,<br />

such as skin rashes, unusually excessive allergies, breathing difficulties, corrosive injuries, etc.<br />

WRITE ON BACK IF MORE SPACE NEEDED<br />

Signature <strong>of</strong> person injured or involved in accident ___________________________________________<br />

Form completed by ________________________________________________<br />

122


L. Standard Operating Procedures (SOPs) <strong>for</strong> Working with Hazardous<br />

Chemicals<br />

1. Sources <strong>of</strong> Chemical Risk Assessment In<strong>for</strong>mation <strong>for</strong> SOPs<br />

Several governmental entities regulate workplace chemical use. Many list various categories and<br />

classes <strong>of</strong> dangerous chemicals which do not necessarily coincide with those <strong>of</strong> other agencies. For<br />

example, the EPA‟s list <strong>of</strong> “extremely hazardous chemicals” contains fewer chemicals than OSHA‟s general<br />

description <strong>of</strong> extremely hazardous chemicals (“acutely toxic” hazardous chemicals), <strong>for</strong> which no <strong>of</strong>ficial<br />

list exists. Nevertheless, all institutions must have safeguards in place <strong>for</strong> working with both EPA and<br />

OSHA regulated extremely hazardous chemicals. Carcinogens are regulated by several different agencies,<br />

none <strong>of</strong> whom agree entirely on a definitive all-inclusive listing. What follows is a summary description <strong>of</strong><br />

all regulations which apply to the Chemistry Department‟s use <strong>of</strong> any chemical whatsoever. All<br />

research and undergraduate teaching laboratories in Salem Hall must provide students with standard<br />

operating procedures (SOPs) to be followed when laboratory work involves the use <strong>of</strong> hazardous chemicals.<br />

"The Chemical Hygiene Plan (CHP) must include the necessary work practices,<br />

procedures and policies to ensure that employees are protected from all potentially<br />

hazardous chemicals in use in their work area. Hazardous chemicals as defined by the<br />

final standard include not only chemicals regulated in 29 CFR part 1910, subpart Z, but<br />

also any chemical meeting the definition <strong>of</strong> hazardous chemical with respect to health<br />

hazards as defined in OSHA's Hazard Communication Standard, 29 CFR 1910.1200"<br />

[from Federal Register, Vol. 55, No. 21, page 3300].<br />

"Hazardous Chemical means any chemical which is a physical hazard or a health<br />

hazard".<br />

"Physical hazard means a chemical <strong>for</strong> which there is scientifically valid evidence<br />

that is a combustible liquid, a compressed gas, explosive, flammable, an organic peroxide,<br />

an oxidizer, pyrophoric, unstable (reactive) or water reactive".<br />

"Health hazard means a chemical <strong>for</strong> which there is statistically significant<br />

evidence based on at least one study conducted in accordance with established scientific<br />

principles that acute or chronic health effects may occur in exposed employees." (29, CFR<br />

1910. 1200, Hazard Communication Standard).<br />

The OSHA Laboratory Standard, the final standard, (29 CFR 1910.1450), defines a hazardous<br />

substance as<br />

". . .a chemical <strong>for</strong> which there is statistically significant evidence based on at<br />

least one study conducted in accordance with established scientific principles<br />

that acute or chronic health effects may occur in exposed employees. The<br />

term health hazard includes chemicals which are carcinogens, toxic or highly<br />

toxic agents, reproductive toxins, irritants, corrosives, sensitizers, hepatotoxins<br />

nephrotoxins, neurotoxins, agents which act on the hematopoietic systems and<br />

agents which damage the lungs, skin, eyes, or mucous membranes."<br />

As you can see, the law is rather insistent that you consider any and all aspects <strong>of</strong> a chemical’s<br />

hazardous properties in preparing a Standard Operating Procedure <strong>for</strong> working with it. You should also<br />

notice that many <strong>of</strong> these laws overlap or use previous laws as the basis <strong>of</strong> newer ones.<br />

123


In addition to consulting those chemicals listed as hazardous laboratory air contaminants in<br />

OSHA's subpart Z – list:<br />

(again, see http://www.osha-slc.gov/OshStd_toc/OSHA_Std_toc_1910_SUBPART_Z.html),hazardous<br />

chemicals can generally be identified by reading the MSDS sheet <strong>for</strong> the particular chemical. These MSDS<br />

sheets are located in the stockroom, room # 110, Salem Hall. This room is accessible 24 hours a day<br />

(via the Salem Hall Submaster Key “SM” issued to all graduate students and all Research<br />

Undergraduate students in the event the door is locked). Health evaluation studies, epidemiological<br />

data, and toxicity assessments listed on these sheets clearly state whether or not a particular chemical is<br />

hazardous, based on the above definitions.<br />

Two other special categories <strong>of</strong> hazardous chemicals are addressed in Salem Hall's Chemical<br />

Hygiene Plan. These are particularly hazardous chemicals and a list <strong>of</strong> about 30 chemicals <strong>for</strong> which<br />

OSHA has "Substance Specific Standards" (29 CFR 1910. 1001-1050). They require more involved<br />

handling procedures and more elaborate means <strong>of</strong> containment, such as using "designated areas", i.e.,<br />

special fume hoods and glove boxes, all <strong>of</strong> which are described specifically on page # 48 <strong>of</strong> this manual.<br />

“Substance Specific Standard” chemicals are usually carcinogens and can generally be handled the same<br />

way as one would handle carcinogens regarded as “particularly hazardous chemicals.” In any case, the<br />

laboratory manager will tell you whether you have any such carcinogens in your chemical inventory.<br />

Consult other sources <strong>of</strong> toxicity in<strong>for</strong>mation kept in the chemistry department Stockroom,<br />

room # 110, such as Lenga, Robert E. Sigma-Aldrich Library <strong>of</strong> Chemical Safety Data, 2nd edition.<br />

Milwaukee, WI: Sigma-Aldrich Corporation, 1988. Read Chapter 3 <strong>of</strong> Prudent Practices, 2nd edition,<br />

pages 29-60. In particular, follow the "Quick Guide to Risk Assessment For Hazardous Chemicals"<br />

in<strong>for</strong>mation found on page 47.<br />

A very good reference <strong>for</strong> toxic hazards <strong>for</strong> particular chemicals is kept in the Chemistry<br />

Department Stockroom, room # 110, <strong>for</strong> your reference:<br />

Patnaik, Pradyot. A Comprehensive Guide to the Hazardous Properties <strong>of</strong> Chemical<br />

Substances. New York: Van Nostrand Reinhold, 1992.<br />

Consult the following book <strong>for</strong> hazards due to reactivity <strong>for</strong> particular chemicals, which is kept in<br />

the Chemistry Department Stockroom <strong>for</strong> your reference:<br />

Urben, P.G., ed. Bretherick’s Handbook <strong>of</strong> Reactive Chemical Hazards, 4th edition.<br />

Ox<strong>for</strong>d: Butterworth-Heinemann Ltd., 1995.<br />

Another good hazardous chemical reference is:<br />

Lewis, Richard J., Sr. Hazardous Chemicals Desk Reference, 3rd edition. New York:<br />

Van Nostrand Reinhold, 1993.<br />

See the “Health Hazards <strong>of</strong> Some Common Chemicals” handout <strong>for</strong> undergraduate Organic<br />

Chemistry labs listed in the training section <strong>of</strong> this manual <strong>for</strong> a good summary <strong>of</strong> toxicity <strong>of</strong> broad classes<br />

<strong>of</strong> chemicals.<br />

One other book you will find useful in preparing SOP‟s <strong>for</strong> Organic reaction setup techniques,<br />

elaborate glassware descriptions, etc., is Harwood, L.M. and Moody, C.J. Experimental Organic<br />

Chemistry: Principles and Practice. Ox<strong>for</strong>d: Blackwell Scientific Publications, 1989. Dr. Mark Welker<br />

has a copy.<br />

The American Chemical Society sometimes publishes letters from chemists regarding unpublished<br />

chemical accident reports, some <strong>of</strong> which involve accidents in “cutting edge” or current academic and<br />

industrial chemical research. See the Chemical & Engineering News “Safety Notes Index” (1976-1989) <strong>for</strong><br />

an index <strong>of</strong> past issues (a hardcopy <strong>of</strong> which appears in the Departmental Chemical Hygiene Plan in the<br />

stockroom, room 110), and the following ACS web site <strong>for</strong> more current issues.<br />

You must be an ACS member to access this site. http://pubs.acs.org/cen/safety/index.html<br />

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2. Summary <strong>of</strong> Regulated Chemicals Covered by this CHP<br />

1. OSHA regulated air-contaminants list, as elaborated in section III.K.1 <strong>of</strong> this manual.<br />

This essentially regulates any and all chemicals which require air-monitoring when<br />

continually released over and above their threshold limit value (TLV) in your lab or<br />

work area as a result <strong>of</strong> poor work habits or improper ventilation. The specific list <strong>of</strong><br />

chemicals, referred to as OSHA Z-list substances, is found in:<br />

http://www.osha-slc.gov/OshStd_toc/OSHA_Std_toc_1910_SUBPART_Z.html<br />

2. OSHA Particularly Hazardous Chemicals, described in section III.F.1 <strong>of</strong> this manual:<br />

carcinogens<br />

teratogens/mutagens<br />

acutely toxic hazardous chemicals<br />

Carcinogens and mutagens/teratogens will be listed in the web site <strong>of</strong> your chemical<br />

inventory (http://www.wfu.edu/chem/cheminventory/index.html)<br />

and in the departmental MSDS sheet inventory, which includes chemicals used in all<br />

laboratories (a hardcopy <strong>of</strong> which will be in the Chemistry Department Stockroom,<br />

room # 110). Acutely toxic hazardous chemicals are not defined clearly by OSHA and<br />

will here be meant to apply generally to all chemicals in the Departmental inventory<br />

with HMIS/NFPA toxicity ratings <strong>of</strong> 3 or 4 (See the HMIS/NFPA hazard rating<br />

descriptions in the Training Section <strong>of</strong> this manual).<br />

3. OSHA “Substance Specific Standard Chemicals”, most <strong>of</strong> which are carcinogens.<br />

Again, if you have any <strong>of</strong> them in your lab, they will be identified in your laboratory<br />

inventory as carcinogens.<br />

http://www.osha-slc.gov/OshStd_toc/OSHA_Std_toc_1910_SUBPART_Z.html<br />

4. Chemicals which require prior approval be<strong>for</strong>e use by students within each lab in Salem<br />

Hall. The Lab Standard requires such a list to be generated by the chemistry<br />

department. It is located in section III.E <strong>of</strong> this manual.<br />

5. The list <strong>of</strong> OSHA P-listed extremely hazardous waste, which should be consulted to<br />

determine whether your lab generates chemical waste which is heavily regulated and<br />

should only be produced by you in limited quantities. Also consult your research<br />

Pr<strong>of</strong>essor <strong>for</strong> further determination <strong>of</strong> what constitutes extremely hazardous waste<br />

generated in your lab (access this list at http://www.epa.gov/docs/epacfr40/chapt-<br />

I.info/subch-I/40P0261.pdf, and go to Part 261.33)<br />

6. EPA’s list <strong>of</strong> “Extremely Hazardous Chemicals” listed only in the Lab Manager’s<br />

Departmental Chemical Hygiene Plan Manual. You will not ordinarily need this list<br />

since it is primarily meant as a “Community Right-to-Know law” source <strong>of</strong> in<strong>for</strong>mation.<br />

This is a listing <strong>of</strong> what EPA regards as extremely hazardous and is reported only when<br />

amounts over and above a certain “reportable amount” are spilled by the institution.<br />

Since we have only very small amounts, this should not be a problem.<br />

http://www.epa.gov/docs/epacfr40/chapt-I.info/subch-J/40P0302.pdf<br />

(go to Table 302.4)<br />

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3. An Introduction to Standard Operating Procedure (SOPs)<br />

A Standard Operating Procedure is a written statement clearly establishing the means by which you<br />

will maintain air concentrations <strong>of</strong> hazardous chemicals below the OSHA Permissible Exposure Level<br />

(PEL) <strong>for</strong> regulated chemicals in subpart Z, Substance Specific Standard chemicals, and particularly<br />

hazardous chemicals. It must also include the means by which you will protect yourself against all other<br />

nonspecific hazardous chemicals, whether they are health hazards or physical hazards, as defined previously<br />

in this section.<br />

<strong>Example</strong>s <strong>of</strong> SOPs would include procedures <strong>for</strong> using laboratory instruments or mechanical<br />

processes involving preparation <strong>of</strong> chemicals such as distillation <strong>of</strong> common laboratory solvents,<br />

repetitional separatory solvent extractions, unusually complicated chemical reactions, high-temperature oil<br />

bath heating techniques, use and handling <strong>of</strong> various classes <strong>of</strong> dangerous chemicals, use <strong>of</strong> rotaryevaporators,<br />

hazardous purification methods, etc., etc. Be sure to include any relevant in<strong>for</strong>mation<br />

concerning types <strong>of</strong> gloves, personal protection equipment, the use <strong>of</strong> hoods, etc.<br />

The following Standard Operating Procedures (SOPs) are composed <strong>of</strong> both generally applicable<br />

procedures <strong>for</strong> all labs in Salem Hall and specific procedures meant <strong>for</strong> your lab only. A collection <strong>of</strong> all<br />

departmental SOPs will be kept in the chemistry department stockroom, room 110, on file with the MSDS<br />

sheets. Research students or faculty members are encouraged to add new SOPs as needed to this section <strong>of</strong><br />

your particular manual. Please post a copy in the Departmental Chemical Hygiene Plan (CHP) in the<br />

stockroom with the laboratory manager.<br />

They can be written in any manner you wish, as long as the relevant safety in<strong>for</strong>mation is<br />

effectively communicated to everyone. You can prepare monolithic literary harangues, short terse<br />

summaries, specific references to monographs kept near the CHP in your lab (such as your ever<br />

present copy <strong>of</strong> Prudent Practices, 2nd edition), chemical or instrumental company MSDS sheets, or<br />

operating manuals, or simple concise statements.<br />

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4. SOPs <strong>for</strong> all laboratories <strong>of</strong> Salem Hall<br />

Laboratory Distillations at Atmospheric Pressure<br />

Distillation is the traditional method <strong>of</strong> purifying a chemical liquid. It is also used to separate one<br />

component in a liquid mixture from another. Distillation in most laboratories <strong>of</strong> Salem Hall involves<br />

refluxing volatile liquids at atmospheric or normal air pressure from a distilling flask through a "simple" or<br />

short path still head, or a longer "fractional" vertically held column, into a slightly downward angled<br />

condenser with a water-cooled jacket into receiving flasks.<br />

Many different sizes and shapes <strong>of</strong> distillation heads and columns exist in chemical laboratories,<br />

but all adhere to the same basic principles <strong>of</strong> safe use. Trouble can arise mainly from excess pressure buildup<br />

due to too rapid heating and unsafe use <strong>of</strong> flammable solvents, resulting in fires. In general, common<br />

high-boiling or nontoxic solvents can be distilled on lab benches, with efficient condenser jacket watercooling.<br />

Very low-boiling or more toxic compounds should be distilled only in a fume hood.<br />

Begin by attaching the water inlet hose on the lower water jacket inlet on the condensing column.<br />

The thermometer bulb should be placed just below the level <strong>of</strong> the roughly horizontal side arm <strong>of</strong> the<br />

distillation head. Just enough heat should be added to the distillation flask to raise the level <strong>of</strong> reflux only<br />

as high as the side arm. Additional heat is not needed.<br />

Do not completely fill the flask with liquid. A half-full or, at most, two-thirds full level is safer.<br />

Be sure all joints are tight, with grease if needed, and that the entire apparatus is well clamped and<br />

supported by ring stands. Fumes leaking through loose joints could come into contact with the heat source<br />

and cause a fire.<br />

Add boiling stones <strong>for</strong> atmospheric pressure distillations. More even boiling can be achieved with<br />

use <strong>of</strong> magnetic stir-bars. You should certainly use stirring <strong>for</strong> high boiling or very toxic compounds. Add<br />

boiling stones and stir bars to cool solutions, be<strong>for</strong>e you begin heating. Dropping cold boiling chips<br />

through a condenser into hot solutions will result in very rapid boiling and has been known to cause boilover<br />

<strong>of</strong> liquid through the top <strong>of</strong> the condenser.<br />

Ordinarily, you should raise the heating mantel on a plat<strong>for</strong>m, or "lab jack" so that you may<br />

quickly remove the source <strong>of</strong> heat if the liquid "bumps" uncontrollably or loss <strong>of</strong> vapor occurs through the<br />

top <strong>of</strong> the condenser. Heat sources ordinarily used in Salem Hall undergraduate organic labs include bare<br />

corning stirrer/hotplates, on low thermostat settings <strong>of</strong> about "3", with distilling flasks just touching or just<br />

above the surface and surrounded in a funnel <strong>of</strong> aluminum foil. Research labs make use <strong>of</strong> various types <strong>of</strong><br />

heat sources, including heating mantels attached to variable trans<strong>for</strong>mers and oil baths on hotplates. When<br />

using oil baths, do not overheat the oil.<br />

The receiving flask should be <strong>of</strong> such design as to efficiently receive the condensed liquid through<br />

the receiving adapter. Vacuum adapters can be used <strong>for</strong> water-aspirator vacuum distillations or inert<br />

atmosphere applications. Gas cylinders <strong>of</strong> nitrogen or argon are commonly attached via hoses to reaction<br />

stills with appropriate regulators and fittings.<br />

Never heat a closed vessel. Always have some means <strong>of</strong> venting heated gasses through distillation<br />

setups. One could also attach a hose to the vacuum adapter and direct it into a hood <strong>for</strong> more effective<br />

removal <strong>of</strong> any uncondensed vapors which may escape from normal atmospheric pressure distillation.<br />

Purging <strong>of</strong> distillation apparatus with inert gasses while distilling is sometimes employed in research<br />

laboratories. Make sure to include some sort <strong>of</strong> "safety valve".<br />

Surround the receiving flask in an ice bath to further condense very volatile organic compounds.<br />

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Make sure coolant is running through the condenser be<strong>for</strong>e you start heating the liquid. The rate <strong>of</strong><br />

distillation, as determined by the number <strong>of</strong> condensed drops falling into the receiving flasks, should be<br />

relatively low, a few drops per second. Do not distill to dryness or "superheating" <strong>of</strong> the flask will occur,<br />

either cracking the glass or leaving a "tarry" residue which may be very flammable or even explosive.<br />

Potentially reactive or explosive solvents should be distilled behind transparent explosion shields<br />

(Instruments <strong>for</strong> Research and Industry, Inc. Catalog #D-15-29 PC, about $325, phone #1-215-379-3333).<br />

One is kept in room # 103 <strong>for</strong> emergencies. Your research advisor should obtain one if you feel it is<br />

necessary <strong>for</strong> any phase <strong>of</strong> your work.<br />

Refill liquid in the receiving flask or disassemble the entire setup only when the glassware has<br />

cooled down from the previous distillation.<br />

128


Compressed Gas Cylinders<br />

Gas cylinders in the Chemistry Department are generally received and stored in the loading dock<br />

area and secured upright in specially made cylinder racks labeled "Full Compressed Gas Cylinders".<br />

Flammable gases (like Hydrogen) and inert nitrogen and argon gases are kept here. A wall separates them<br />

from another incoming storage area near room #20, labeled: "Full Oxygen and Air Compressed Gas<br />

Cylinders" <strong>for</strong> industrial grade air and oxygen cylinders. A cylinder rack <strong>for</strong> empty cylinders, labeled<br />

"Empty Cylinders" is located next to room #19. Please be certain that the cylinders left in the empty rack<br />

are indeed empty (no cylinder should be completely emptied - see rules below).<br />

LEAKING COMPRESSED GAS CYLINDERS OR NATURAL GAS JETS IN LABORATORIES.<br />

If a large compressed gas cylinder or lecture bottle in your lab begins to leak, decide first <strong>of</strong> all<br />

whether it is a harmful gas or an inert one. Unless it is too dangerous to breathe, attempt to stop the<br />

leak be<strong>for</strong>e taking it to the loading dock area and calling security. If the leak occurs around the stem<br />

<strong>of</strong> a large cylinder, <strong>care</strong>fully load it onto a cylinder cart and take it to the loading dock. Call<br />

National Welders, Inc., Winston-Salem (744-0100) <strong>for</strong> immediate advice and cylinder removal. It<br />

might be wise to leave the cylinder on the cart outside the loading dock doors. The Winston-Salem<br />

<strong>of</strong>fice <strong>of</strong> National Welders will call their Charlotte Safety Division (headed by Randy Miller, 704-<br />

644-7513, or Ken Boyte, 704-644-3266) <strong>for</strong> especially difficult compressed gas cylinder leaks. If<br />

natural gas odor permeates your lab room from a gas jet leak which you cannot stop, try to open<br />

windows be<strong>for</strong>e calling security and leaving the room. Such leaks are an especially hazardous source<br />

<strong>of</strong> fire.<br />

Follow these rules when using compressed gas cylinders:<br />

* Identifying labels should be kept in place on cylinders. Missing labels on old lecture bottles<br />

spell trouble - get with your research advisor or the lab manager, find out definitely what the gas is by one<br />

means or another and label it! Keep lecture bottles in ventilated lower hood cabinets when not in use.<br />

* Store flammable gases like hydrogen away from oxidizers and corrosives, like oxygen and<br />

hydrogen chloride gas or ammonia.<br />

* Do not use inappropriate hose material as dispensing tubes from gas cylinder regulators.<br />

Corrosive gases may destroy rubber or latex tubing. Tygon tubing should perhaps be used instead, or<br />

copper or stainless steel, or some other non-corroding material.<br />

* When cylinders are no longer in use, take <strong>of</strong>f their regulators, cap them with valve caps, and<br />

take them back to the loading dock holding area. It is your responsibility to make certain full cylinders are<br />

stored in the "full cylinder" racks and empty cylinders are placed in the "empty cylinder" racks. Do not<br />

allow unused cylinders to accumulate in your laboratory.<br />

Corroded cylinder valve stems, gas line fittings, or regulators are a source <strong>of</strong> danger and should be<br />

exchanged <strong>for</strong> better quality equipment.<br />

* Handle gas cylinders with extreme <strong>care</strong>. They are, <strong>of</strong> course, under a great deal <strong>of</strong> pressure and<br />

would trans<strong>for</strong>m themselves into fairly powerful missiles if the valve stem on top were to be sheared <strong>of</strong>f.<br />

This could conceivably happen if they were dropped, especially if the valve stem falls against something on<br />

the way down. This will only be prevented if you endeavor to keep the valve cap on when moving the<br />

cylinder.<br />

* Take the regulator <strong>of</strong>f the cylinder be<strong>for</strong>e you even consider taking the cylinder somewhere else.<br />

Move the cylinder on one <strong>of</strong> the two-wheeled chain cylinder dollies located in the loading dock area. Chain<br />

the cylinder and push the cart slowly. Never, never move a cylinder without a threaded valve cap cover<br />

attached.<br />

* Never leave cylinders unstrapped in the lab. Secure them against a wall or a lab bench.<br />

* Keep track <strong>of</strong> where you store cylinder caps <strong>for</strong> cylinders being presently used.<br />

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* Do not grease or oil the regulator thread <strong>of</strong> a cylinder valve. Oil on a gas cylinder thread will<br />

soon be under very high pressure. If the gas reacts at all with organic material, this could lead to an<br />

explosion. This is especially true <strong>for</strong> Oxygen gas cylinders. Teflon tape can be used on the outlet side <strong>of</strong><br />

the regulator, but not on the primary fitting connection between the regulator and the cylinder.<br />

* Never use a cylinder without an attached regulator.<br />

* Add flashback arresters to oxygen and hydrogen cylinders when used <strong>for</strong> torches <strong>for</strong><br />

glassblowing or glass working. Flashback occurs when flames actually traverse through the gas line back to<br />

the cylinder outlet.<br />

* Do not completely empty a cylinder be<strong>for</strong>e returning it to the loading dock area. Slight positive<br />

pressure (between say 5 and 15 psi) will keep atmospheric oxygen from contaminating the cylinder<br />

contents, so that the cylinder can be safely refilled by the gas cylinder supplier.<br />

* Do not over-tighten a hand-valve on a gas cylinder. If hand tightening will not completely close<br />

the valve, call the gas cylinder company <strong>for</strong> removal after taking it at once to the loading dock.<br />

* Do not over-tighten the hand-valve on the liquid nitrogen tank in the loading dock area when<br />

you are through dispensing liquid nitrogen. The pipe wrench attached to the wall is <strong>for</strong> opening frozen<br />

valves, not <strong>for</strong> closing the valve. The slightest extra pressure on the valve when closing may damage it.<br />

Over-tightening the valve will crush the Teflon seals inside the valve and when this happens, the valve has<br />

to be rebuilt.<br />

We have placed a pipe wrench near the liquid nitrogen tank, loading dock area, <strong>for</strong> use in<br />

loosening frozen valves, when opening them. Some people are using the wrench <strong>for</strong> closing the valve<br />

afterward, which naturally makes it harder <strong>for</strong> the next person to open it again. PLEASE DON’T OVER-<br />

TIGHTEN THE VALVE WHEN CLOSING IT, or we will remove the wrench. There is no need <strong>for</strong><br />

anything other than hand-tightening to shut <strong>of</strong>f the valve. Occasionally, this hand valve may freeze in the<br />

open position, while you are dispensing liquid nitrogen. This happens especially when you turn it wide<br />

open and take a great deal <strong>of</strong> liquid from the tank. Water vapor in the air, specially on a rainy day, will<br />

actually freeze in the valve and make it hard to close. In this case, it may be justifiable to use the pipe<br />

wrench to just “crack” or “break” the frozen hand valve, without tightening it shut, and then closing it the<br />

rest <strong>of</strong> the way with your hand (in an absolute emergency, you could even pour hot water over the hand<br />

valve to thaw it).<br />

The simplest thing to do, while wearing thick insulation gloves, is to gently turn the valve back and<br />

<strong>for</strong>th when you open it up all the way on - that way, it can’t freeze.<br />

Sometimes, the safety valve (connected to the pressure gauge, on the opposite side <strong>of</strong> the tank from<br />

the dispensing hand-valve) begins releasing high-pressure vapor, with a hissing sound. The safety valve<br />

opens when too much pressure builds up above the layer <strong>of</strong> liquid gas inside the tank. This happens usually<br />

just after the tank has been delivered since the temperature outside is a lot higher than inside the building<br />

and movement <strong>of</strong> the tank during transportation has caused buildup <strong>of</strong> pressure from rapid evaporation.<br />

When the pressure in the tank goes above 22 pounds per square inch (psi), the safety valve automatically<br />

opens.<br />

Sometimes this valve will frost over and freeze, again because <strong>of</strong> water moisture in the air freezing<br />

upon contact with liquid nitrogen. When this happens, open the vent valve (the hand valve connected to the<br />

safety valve with the pressure gauge attached) and bleed <strong>of</strong>f a little pressure until the gauge reads about 18<br />

psi, at which point the emergency venting from the safety valve will stop. Alternately, you could<br />

actually pour hot water over the safety valve and thaw it. National Welders personnel occasionally do this.<br />

You can get the water from the loading dock sink. The lab manager will leave small buckets or pans under<br />

the sink <strong>for</strong> this purpose.<br />

Perhaps you can pour water from one bucket while catching it as it falls from the valve into another<br />

smaller bucket.<br />

130


Summary <strong>of</strong> Liquid N2 Instructions<br />

1. Wear thick gloves or mittens to hold metallic<br />

Delivery Hose and open dispensing Hand Valve.<br />

Alternatively, get a couple <strong>of</strong> thick cotton towels.<br />

2. The attached pipe wrench is <strong>for</strong> opening a frozen<br />

liquid-nitrogen cylinder hand valve, not closing it.<br />

When closing the valve, hand-tighten it only!<br />

3. If the valve freezes open while you are dispensing<br />

liquid nitrogen, use the pipe wrench to just<br />

“crack” or loosen the hand valve and then close it<br />

by hand only. Alternately, pour a little hot water<br />

on the valve to thaw the frozen seal. A water<br />

bucket is located under the sink in the loading<br />

dock area.<br />

4. If there is too much pressure in a full tank just<br />

after the trucks deliver it to the loading dock,<br />

excess nitrogen gas will automatically escape<br />

through the safety valve. If too much goes<br />

through, that valve may freeze. Open the<br />

adjacent vent valve and vent until the pressure<br />

gauge reads 18 psi. If both valves freeze shut<br />

while open, pour hot water over them, using the<br />

bucket under the sink in the loading dock area.<br />

131


Safe Installation and <strong>Use</strong> <strong>of</strong> Gas Cylinder Regulators<br />

Specific gases require specific regulators. Otherwise, gases incompatible with the metal <strong>of</strong> a<br />

particular regulator may corrode it or even rupture the seals and diaphragms within the regulator. Industrial<br />

standards are in place which generally prevent improper connections between cylinders containing<br />

particular gases and a multitude <strong>of</strong> regulators commercially available (e.g. different thread sizes, clockwise<br />

or counterclockwise thread, or other special connector fitting requirements). However, you should still be<br />

diligent in choosing the proper regulator. Consult the gas cylinder company catalog and your research<br />

director <strong>for</strong> advice.<br />

Follow these steps <strong>for</strong> setting up a regulator attachment (from “Operating Instructions <strong>for</strong> General<br />

Purpose and High Purity Regulators”, Form #0056-0901, 2/83, Victor Equipment Company).<br />

"Important Safety and Operating Instructions<br />

For General Purpose and High Purity Regulators<br />

“Do not use this regulator with gases other than those <strong>for</strong> which it is intended.<br />

“Do not attempt to operate this regulator unless you have been trained in its proper use<br />

or are under competent supervision. Do not use this apparatus unless you are familiar<br />

with the hazards associated with the gas you are using.<br />

“Oxygen is not flammable; however, the presence <strong>of</strong> pure oxygen will drastically<br />

increase the speed and <strong>for</strong>ce with which burning takes place. Oxygen must never be<br />

allowed to contact oil, grease or other petroleum-based substances; there<strong>for</strong>e, use no<br />

oil or grease on regulator, cylinder, valves or equipment. Do not use or store near<br />

excessive heat (over 125 degrees F or 51.5 degrees C) or open flame.<br />

Setting Up Equipment<br />

1. “Secure cylinder to wall, stand or cart so it will not tip over or fall.<br />

2. Remove the protective dust seal from the cylinder valve.<br />

3. Inspect the cylinder valve <strong>for</strong> traces <strong>of</strong> dirt, dust, oil or grease. Remove dirt and<br />

dust with a clean cloth. NOTE: If oil or grease is detected, DO NOT use cylinder.<br />

(See warning note above.) In<strong>for</strong>m your gas supplier <strong>of</strong> this condition immediately.<br />

4. Inspect the regulator <strong>for</strong> damaged threads, dirt, dust, oil or grease. Remove dirt<br />

or dust with a clean cloth. NOTE: If oil or grease is detected or if threads are<br />

damaged, DO NOT use the regulator. Have your distributor or an authorized<br />

repair station clean the regulator and/or repair the damage be<strong>for</strong>e using.<br />

Installing the Regulator<br />

1. Make sure the regulator has the proper CGA inlet fitting to fit the cylinder valve.<br />

If the connection is so equipped, make sure the flat sealing washer is in place<br />

between the regulator and the cylinder valve outlet. Attach the regulator to the<br />

cylinder valve outlet. The treads may be either right hand or left hand depending<br />

on the cylinder and regulator connections. Regulator inlet connections with left<br />

hand threads have a “V” notch machined into the hexagonal nut fitting to signify<br />

a left hand thread.<br />

2. Tighten the regulator inlet nut securely.<br />

3. Make proper connection to outlet <strong>of</strong> regulator valve or fitting.<br />

4. Be<strong>for</strong>e opening the cylinder valve, release the tension on the regulator adjusting<br />

spring by turning the adjusting knob in a counterclockwise (decreasing gas flow)<br />

direction.<br />

Turning on the Cylinder<br />

1. Be sure that tension on regulator adjusting spring is released. After all pressure<br />

has been drained, release all tension on the pressure adjusting knob by turning it<br />

counterclockwise (decreasing) until the knob turns freely. Stand so the cylinder<br />

valve is between you and the regulator. NOTE: Never stand in front or in back <strong>of</strong><br />

a regulator when opening the cylinder valve. Slowly turn the valve handle in a<br />

counterclockwise direction until you hear the gas begin to flow into the regulator.<br />

Wait about 10 seconds, then turn the cylinder valve fully open.<br />

2. To check <strong>for</strong> leaks, close the cylinder valve and observe the high pressure gauge<br />

<strong>for</strong> five minutes. If the high pressure gauge reading drops, there is a leak in the<br />

132


cylinder valve, inlet fitting, high pressure gauge, or regulator seat. If the high<br />

pressure gauge does drop, retighten the regulator-to-cylinder connection and<br />

repeat Step 1. Should the high pressure gauge continue to drop after retightening<br />

the regulator-to-cylinder connection, the regulator must be removed and returned<br />

<strong>for</strong> service.<br />

“Never attempt to tighten a cylinder valve or any parts <strong>of</strong> the valve. If the cylinder<br />

valve is leaking, place the cylinder outdoors and notify the cylinder supplier<br />

immediately.<br />

3. Keep the cylinder valve closed at all times, except when the regulator is in use.<br />

Adjusting Regulator<br />

Delivery Pressure and Flow<br />

1. After the regulator has been securely attached to the cylinder and no leaks exist<br />

(see previous sections), adjust the delivery pressure to the desired pressure setting<br />

by turning the adjusting knob in a clockwise (increasing) direction until the<br />

desired pressure is reached.<br />

2. If the regulator is equipped with an outlet valve (or needle valve), flow can be<br />

regulated by proper adjustment <strong>of</strong> the valve.<br />

Turning Off Cylinder Valve<br />

“When you have finished using the regulator, close the cylinder by turning the handle<br />

in a clockwise direction and allow all pressure to drain from the regulator. Gas will<br />

cease to flow and the pointers on both pressure gauges will indicate “0” when all<br />

pressure has been drained from the regulator. After all pressure has been drained,<br />

release all tension on the pressure adjusting knob by turning it counterclockwise<br />

(decreasing) until the knob turns freely. Turn the outlet valve, if so equipped, in a<br />

clockwise direction to turn <strong>of</strong>f valve.<br />

Removing Regulator<br />

1. “It is not necessary to remove the regulator unless the cylinder is being moved or<br />

an empty cylinder is being exchanged <strong>for</strong> a full one.<br />

2. NEVER attempt to remove the regulator if any pressure is showing on either<br />

pressure gauge. Turn the cylinder valve handle clockwise and allow all pressure<br />

to drain from regulator. Gas will cease to flow and the pointers on both pressure<br />

gauges will indicate “0” when all pressure has been drained from the regulator.<br />

After all pressure has been drained, release the tension on the pressure adjusting<br />

knob by turning it counterclockwise (decreasing) until the knob turns freely.<br />

3. Remove the regulator from the cylinder and replace the protective cap on the<br />

cylinder.”<br />

In<strong>for</strong>mation on Aldrich regulators can be obtained at:<br />

https://www.sigma-aldrich.com/aldrich/bulletin/al_techbull_al151.pdf<br />

Again, remember that specific regulators are made <strong>for</strong> each gas used in the lab, and that some<br />

regulator inlet CGA fittings employ left-handed thread rather than right-handed thread. You will see a "V"<br />

notch on the outlet nut fitting <strong>for</strong> left-handed thread.<br />

If the thread is right-handed, the hexagonal outlet nut fitting will not be so notched, and you can<br />

remove the regulator using a wrench by loosening the fitting in a normal counterclockwise direction<br />

(meaning toward the left as one faces the outlet), or as one anonymous graduate student put it, "Rightie<br />

tightie, lefty, loosie".<br />

DO NOT OVERTIGHTEN regulator fittings while installing them onto the tanks. This may<br />

damage the thread. Slightly more than a good hand-tightening is really all they need. The “ball and socket”<br />

fitting is constructed so as to compress and automatically seal when the tank valve is opened so that the gas<br />

pressure actually tightens the seal, since the metal surfaces at the point <strong>of</strong> contact are made <strong>of</strong> malleable<br />

brass or chrome-plated brass. Even if you did not tighten it enough, nothing worse than a loud hiss <strong>of</strong><br />

escaping gas would occur - after all, you would not expect the regulator to dislodge itself, like an unwinding<br />

propeller, would you? Most people overtighten regulators, making removal difficult and dangerous.<br />

Pounding on a wrench handle to remove regulators is unwise.<br />

Again, in reference to the “ball and socket” joint connection between the regulator inlet shaft and<br />

the cylinder outlet stem - After the male-threaded regulator and female-threaded cylinder fittings are<br />

connected, this is the airtight seal between the two pieces <strong>of</strong> equipment. This is the area which requires the<br />

most cleaning. Sometimes microscratches develop in the “ball and socket” area, resulting in slow gas leaks.<br />

133


Test <strong>for</strong> leaks anywhere by squirting soapy water (such as “Snoop” brand name solution) onto the fitting. If<br />

a steady stream <strong>of</strong> bubbles appears, loosen the fitting, tilt the angle <strong>of</strong> the regulator slightly, and retighten.<br />

The leak would not happen unless scratches from both surfaces coincide – changing the angle <strong>of</strong> metal-tometal<br />

contact lessens the probability <strong>of</strong> matching microscratches.<br />

Teflon tape used on the attachment fitting between regulator and cylinder does nothing to improve<br />

the seal between the surfaces <strong>of</strong> the “ball and socket” joint. Hence, tape should be avoided, except <strong>for</strong> gas<br />

line fittings which employ thread only, such as regulator outlets, or needle valves on the outlet side <strong>of</strong> the<br />

regulator, or gas line connectors further down the gas line, away from the regulator and cylinder. Likewise,<br />

teflon tape can be used to tighten pipe (NPT) thread fittings in gas lines, since these tapered thread fittings<br />

are constructed so as to seal at the threaded metal surfaces. Swagelok fittings seal when the front and back<br />

ferrules within the fitting press against each other – which cannot happen if they are separated by teflon<br />

tape. DO NOT use teflon tape on Swagelok fittings.<br />

The Lab Manager has a useful book entitled “Swagelok Tube Fitter’s Manual” which you are<br />

welcome to consult whenever you wish. The following web site list very good directions <strong>for</strong> working with<br />

swagelok fittings: http://www.swagelok.com/ and click on “Products”, “Catalogs”, “Fittings-Tube”,<br />

“Connects tubing to tubing”, and, finally, any one <strong>of</strong> the remaining options, such as “Reducing Union<br />

Tees”, and on to “Assembly/Installation” PDF files, such as those <strong>for</strong> adapters/ reducers “<strong>for</strong> one-and-aquarter<br />

inch & 25 mm and larger”sizes.<br />

See also the following helpful procedures if your lab has need <strong>of</strong> them:<br />

"Lightup and shut down procedure <strong>for</strong> oxygen fuel torch," National Welders Supply Company,<br />

Inc., PO Box 31007, Charlotte, NC 28231, phone # 1-800-866-4422. [located in the stockroom hardcopy<br />

<strong>of</strong> the CHP, room # 110]<br />

"Atomic Absorption Acetylene: Recommendation <strong>for</strong> <strong>Use</strong>," National Welders Supply Company,<br />

Inc., PO Box 31007, Charlotte, NC 28231, phone # 1-800-866-4422, Company memo from Gary Stiles to<br />

district managers. [located in the stockroom hardcopy <strong>of</strong> the CHP, room # 110]<br />

"Technical In<strong>for</strong>mation Bulletin #AL-167, Instructions <strong>for</strong> Using the Calibration-Gas Cylinder,"<br />

Aldrich Chemical Company, 1001 West Saint Paul Ave., Milwaukee, Wisconsin 53233, phone # 1-800-<br />

558-9160. [located in the stockroom hardcopy <strong>of</strong> the CHP, room # 110]<br />

134


Laboratory Operations Involving Reduced Pressure or Vacuum<br />

Low pressure operations in the chemistry department are frequently used in research laboratories<br />

and less frequently in advanced undergraduate labs, with the exception <strong>of</strong> common vacuum filtration.<br />

Water aspirators in undergraduate labs can safety be used as sources <strong>of</strong> vacuum <strong>for</strong> filtration if<br />

heavy walled Erlenmeyer flasks are employed as the evacuation vessel. A supply <strong>of</strong> such flasks is kept in<br />

the stockroom. All students are assigned one <strong>for</strong> each lab class. It is generally a good idea to place a<br />

smaller "trap" 250 ml flask between the filter and the aspirator, so that water cannot be sucked back into the<br />

system if the water pressure should fall unexpectedly while filtering. Also, the filtrate solution can be<br />

trapped here if accidentally taken up into the vacuum line.<br />

Large glass vacuum desiccators should be taped on the surface with electricians tape in strips, so as<br />

to minimize flying glass from possible implosions. Only chemicals being dehydrated in order to be kept dry<br />

should be stored in a desiccator. When opening a desiccator that is under vacuum, make sure that<br />

atmospheric pressure has been restored first. A "frozen" desiccator lid can be loosened by using a singleedge<br />

razor blade as a wedge, which can then be tapped with a wooden block or gently with a hammer to<br />

raise the lid.<br />

Vacuum distillations can be per<strong>for</strong>med in undergraduate laboratories using water aspirators as a<br />

vacuum source. Research labs sometimes make use <strong>of</strong> vacuum pumps. Problems with super-heating and<br />

sudden boiling, or "bumping", are more likely to occur with distillations under reduced pressure. It is<br />

there<strong>for</strong>e prudent to make use <strong>of</strong> magnetic stir bars. Boiling stones only increase bumping in this situation.<br />

Double-check all clamped fittings. Slowly close and open stopcocks to evacuate the apparatus. Implosions<br />

are possible under high vacuum, so use a safety shield, if your research advisor thinks it necessary. Allow<br />

the system to cool be<strong>for</strong>e allowing air into the apparatus. Oxygen may be all the material inside the flask<br />

needs <strong>for</strong> a small explosion <strong>of</strong> peroxides or other highly reactive material that has been concentrated in the<br />

distillate. Never distill to dryness!<br />

Vacuum pumps should not be used without cold traps to contain volatile vapors in the vacuum line<br />

be<strong>for</strong>e they mix with pump oil. Corrosive organic compounds naturally tend to destroy pump vanes if oil<br />

isn't changed frequently.<br />

Various devices containing mercury are used with vacuum apparatus. Manometers, McLeod<br />

gauges, and thermometers attached to such equipment can easily break or overturn, spilling mercury.<br />

Regularly inspect all mercury containing devices. Try to keep them in a plastic pan <strong>of</strong> sufficient volume to<br />

hold all <strong>of</strong> the mercury in case <strong>of</strong> a break. <strong>Use</strong> the mercury spill-kit hand pump located in the Chem. Dept.<br />

stockroom, #110 to clean up mercury spills and deposit it in the holding tray located in room #20, in the<br />

hood.<br />

135


<strong>Use</strong> <strong>of</strong> Reflux Condensers<br />

Both undergraduate organic laboratories and research laboratories frequently require the heating <strong>of</strong><br />

liquid mixtures to facilitate chemical reactions. These mixtures are composed <strong>of</strong> reactants dispersed in<br />

organic solvents, usually in round-bottomed flasks capped by upright, jacketed water-filled glass tubes<br />

refereed to as reflux condensers.<br />

Common, generally nontoxic solvents can be refluxed on open laboratory benches. Ideally,<br />

however, all reflux condensers should be set up in a hood, in case too much heat is applied and vapors rise<br />

out <strong>of</strong> the condenser. Since boiling solvents do not increase in temperature, increasing the heat applied will<br />

only cause loss <strong>of</strong> solvent vapor, not an increase in reaction rate. A condensation level <strong>of</strong> 1 or 2 inches<br />

above the bottom <strong>of</strong> the condenser tube is all that is necessary.<br />

Tap water is cold enough <strong>for</strong> most refluxes. However, very low boiling solvents like acetone or<br />

ethyl ether may require ice-cooled water supplied with submersible lab pumps. Constant temperature waterbaths<br />

can also be used.<br />

The condensers should be placed vertically onto the round bottom heating flask and attached<br />

firmly to ring stands with metal clamps. The water inlet should be through the lower end <strong>of</strong> the condenser.<br />

Water hoses should be clamped onto water inlets/outlets on the condensers with Ace Glass wire hose<br />

clamps (located in the stockroom <strong>for</strong> Departmental use) or thick copper wire, twisted on firmly with a pair<br />

<strong>of</strong> pliers (Thin wire could eventually slice through the tubing). Hose clamps are not a good idea. Surging<br />

pressure in Salem Hall water lines could cause water hoses to slip <strong>of</strong>f if they are held onto a serrated<br />

condenser hose adapter fittings with flat hose clamps. The only disadvantage <strong>of</strong> using wires is that you<br />

must cut them <strong>of</strong>f periodically when they become corroded and replace them. <strong>Use</strong> <strong>of</strong> Tygon tubing, instead<br />

<strong>of</strong> rubber, will allow you to actually see the water flowing through the hose. You can then run water<br />

through with a relatively slow speed, which is all you need in water condenser coils. Also, this means there<br />

will be less chance <strong>of</strong> a spill when inevitable water pressure surges occur in Salem Hall at night. The water<br />

pressure never falls to zero, so you basically can’t have the water flow on too low. Once you have<br />

connected the water hose clamps, gently but firmly pull on the lines to make sure they are on tight.<br />

I am currently looking <strong>for</strong> inexpensive in-line water flow indicators (will purchase those without<br />

molded plastic halves which could pry apart under water pressure surges) which you can attach anywhere in<br />

the water line to more readily judge the flow <strong>of</strong> water through the line.<br />

You may also purchase Water-Flow Monitor sensor instruments with solenoid valve automatic<br />

water shut-<strong>of</strong>f mechanisms <strong>for</strong> about $600 from I2R Company.<br />

"Bumping" <strong>of</strong> solvents can be avoided by adding boiling stones.<br />

Magnetic stir bars can also be added to stir the boiling solution, allowing more even boiling.<br />

Safe <strong>Use</strong> <strong>of</strong> Laboratory Centrifuges<br />

Lab centrifuges in Salem Hall are <strong>of</strong> the low-speed type, and do not need special handling<br />

requirements. They are supported on suction-cup feet and will not ordinarily wobble to the point <strong>of</strong> falling<br />

<strong>of</strong>f bench tops. Balance them by placing test tubes half filled with water immediately opposite the test tube<br />

being centrifuged.<br />

Occasionally check the power cord and keep extraneous lab equipment from cluttering bench tops<br />

near the centrifuge.<br />

136


<strong>Use</strong> <strong>of</strong> the Hydraulic Press (prepared by Dr. Ron N<strong>of</strong>tle)<br />

(Note: Serious injury can result if you do not set the press up properly<br />

so pay attention to these directions.)<br />

1. Be sure that the parts <strong>of</strong> the sample press fit together in alignment.<br />

All <strong>of</strong> the parts must contact each other and the sample perfectly.<br />

2. When you place the assembled sample press in the hydraulic press:<br />

a. make sure that it is in the middle <strong>of</strong> the hydraulic press plate<br />

b. place the aluminum plate over the plunger and gradually crank<br />

the hydraulic press until the system is tight.<br />

c. check to make sure that the sample press is perfectly vertical<br />

with respect to the hydraulic press and does not lean at all<br />

d. close the Plexiglas door<br />

e. crank up the pressure to no more than 12,000 PSI. Allow the<br />

sample to sit in the press <strong>for</strong> a few minutes so that the heat will<br />

be dissipated and then gradually release the pressure.<br />

Upper Plate <strong>of</strong><br />

Hydraulic Press<br />

(bottom view)<br />

Al Plate<br />

Sample<br />

Press<br />

Bottom Plate<br />

<strong>of</strong> Hydraulic<br />

Press<br />

(side view)<br />

You can see that, if the<br />

sample press is not placed<br />

properly in the hydraulic<br />

press, on applying pressure,<br />

it (or pieces <strong>of</strong> it) could fly<br />

out at tremendous speed and<br />

could go right through the<br />

Plexiglas door which is really<br />

only a first-line protection.<br />

This has happened at other<br />

laboratories<br />

137


Detection and Removal <strong>of</strong> Organic Peroxides<br />

When working with a great variety <strong>of</strong> organic chemicals in research laboratories, you may<br />

encounter bottles <strong>of</strong> older organic ethers or other organic liquids which are capable <strong>of</strong> autooxidation and<br />

subsequent <strong>for</strong>mation <strong>of</strong> explosive peroxides, especially those which have undergone extensive exposure to<br />

air. These are one <strong>of</strong> the worst dangers you may face in such laboratories.<br />

You should be aware <strong>of</strong> which chemicals can conceivably <strong>for</strong>m peroxides, how to chemically test<br />

<strong>for</strong> the presence <strong>of</strong> peroxides, and how to destroy the peroxides within the organic liquid (if the content <strong>of</strong><br />

peroxides is not too high) so that you may still make use <strong>of</strong> the liquid compound.<br />

Please read sections concerning peroxides, pages 54-56, pages 99-101, and 162-163 <strong>of</strong> Prudent<br />

Practices, 2nd Edition <strong>for</strong> specific in<strong>for</strong>mation concerning the above points.<br />

In particular, it shall be standard procedure <strong>for</strong> graduate students working in research laboratories<br />

to search through their labs once a year <strong>for</strong> all chemicals in table 3.13 on page 56 <strong>of</strong> Prudent Practices, 2nd<br />

Edition, and consult with their research advisors as to the condition and age <strong>of</strong> containers <strong>of</strong> such chemicals<br />

and decide whether they should be tested <strong>for</strong> peroxide content via the methods listed on page 100 <strong>of</strong><br />

Prudent Practices, 2nd Edition. The first test mentioned will only indicate peroxides <strong>of</strong> chemical structure<br />

ROOH (R=alkyl). Dialkyl peroxides (ROOR) can be detected with the 2nd method, which employs a 10%<br />

aqueous solution <strong>of</strong> potassium iodide with a starch indicator solution.<br />

Generally, the best method is the last listed, i.e., peroxide test strip paper (EM Quant Test Strips,<br />

catalog #TM-1162, <strong>for</strong> 0.5 to 25 ppm peroxide content detection, and catalog #TM-27173, <strong>for</strong> 0 to 100<br />

ppm peroxide content detection, Lab Safety Supply, Inc., phone #1-800-356-0783).<br />

“Instructions <strong>for</strong> <strong>Use</strong>”<br />

[from Peroxide Test instruction booklet, Merckoquant 10011, E. Merck Co.,<br />

64271 Darmstadt, Germany, phone # (06151)720.]<br />

“Aqueous Solutions:<br />

1. Remove 1 test strip and immediately reclose the tube.<br />

2. Dip the test strip into the solution to be tested <strong>for</strong> 1 sec, such that the<br />

reaction zone is completely wetted (a small square area on the end <strong>of</strong> the<br />

strip, clearly visible).<br />

3. Remove the test strip, shake <strong>of</strong>f excess liquid and compare the reaction zone<br />

with the color scale after 15 sec.<br />

“Organic <strong>Solvent</strong>s (volatile ethers)<br />

1. Remove 1 test strip and immediately reclose the tube.<br />

2. Dip the test strip into the solvent to be tested <strong>for</strong> 1 sec, such that the reaction<br />

zone is completely wetted.<br />

3. Move the test strip slightly to and fro <strong>for</strong> 3-30 sec until the solvent has<br />

evaporated from the reaction zone, then<br />

a) dip into distilled water <strong>for</strong> 1 sec, shake <strong>of</strong>f excess water<br />

or,<br />

b) breathe on it 4 times each <strong>for</strong> 3-5 sec.<br />

4. After 15 sec, compare the reaction zone with the color scale.”<br />

138


At the present time, test strips <strong>for</strong> general use are kept in the small portable refrigerator kept in the<br />

back <strong>of</strong> undergrad lab room #101. Newly purchased tubes <strong>of</strong> these test strip papers should be stored in a<br />

refrigerator, but see the enclosed instruction sheet <strong>for</strong> storage <strong>of</strong> opened containers.<br />

Methods <strong>for</strong> destruction <strong>of</strong> peroxides can be found in the following references:<br />

Gordon A. J. and Ford, R. A. The Chemist’s Companion. New York: John Wiley and Sons,<br />

1972, page 437<br />

Perrin, D.D. and Armarego, W.L.F. Purification <strong>of</strong> Laboratory Chemicals, 3rd Edition. Ox<strong>for</strong>d:<br />

Butterworth-Heinemann Ltd., 1994.<br />

Jackson, H.L. et al., J. Chem. Educ., 47 (1970), page A175.<br />

When opening containers <strong>of</strong> Ethyl ether, tetrahydr<strong>of</strong>uran, or 1,4-dioxane in the solvent room #20,<br />

which are usually purchased in large 5 gallon (or 20 liter) metal containers, please label them with the date<br />

upon which they are first opened.<br />

You should make an attempt to label all chemicals in your laboratory which could conceivably<br />

<strong>for</strong>m peroxides with the opening date. Please see the above mentioned table 3.13 <strong>for</strong> the list <strong>of</strong> such<br />

chemicals.<br />

When bottles are found to actually contain levels <strong>of</strong> peroxides above the 25 ppm concentration<br />

range, you should not, <strong>of</strong> course, use it. You may remove the peroxides via one <strong>of</strong> the above referenced<br />

purification methods (with your research advisor’s guidance) or <strong>care</strong>fully destroy them (again, following<br />

specific instructions) or take them, properly labeled, to the waste holding area in room #20 <strong>for</strong> removal by<br />

the Chemical Waste Company. Even containers with less than 25 ppm peroxide content should not be<br />

handled or used without direct supervision from your research advisor. Obtain his/her judgment as to<br />

whether it is best to remove the peroxides or simply have them taken out by the waste company.<br />

GENERAL METHOD FOR DESTRUCTION OF PEROXIDES WITHIN AN ORGANIC LIQUID<br />

Gently open the cap <strong>of</strong> the bottle and pour the organic liquid into a larger container, such as<br />

a beaker (preferably a large 4 liter polyethylene beaker, found in the general chemistry prep room)<br />

or a larger polyethylene pan. If the organic liquid is soluble or miscible in water, dilute it with<br />

roughly the same volume <strong>of</strong> water. Slowly, with stirring, add a dilute solution <strong>of</strong> sodium bisulfite and<br />

stir <strong>for</strong> about 20 minutes. Then test again <strong>for</strong> destruction <strong>of</strong> peroxides with test strips.<br />

If the liquid is not soluble in water (such as ethyl ether) simply add a smaller volume <strong>of</strong><br />

aqueous sodium bisulfite to the organic liquid in a beaker and stir longer. <strong>Use</strong> a magnetic stirrer.<br />

Again, test the organic layer <strong>for</strong> peroxides. Separate the layers in a separatory funnel and reuse the<br />

organic liquid or bottle it up <strong>for</strong> disposal.<br />

Washing with dilute sodium bisulfite is generally the best way to remove peroxides. You will<br />

find sodium bisulfite in the organic chem. prep room (room #103) if you need it (see reference<br />

Jackson, H.L. et al., J. Chem. Educ., 47 (1970), page A175).<br />

139


5. Laboratory Specific SOPs<br />

<strong>Guidelines</strong> <strong>for</strong> <strong>care</strong> & <strong>Use</strong> <strong>of</strong> <strong>Dry</strong> <strong>Solvent</strong> <strong>Stills</strong> [<strong>Example</strong>]<br />

(Procedure <strong>for</strong>merly used in Dr. Davies’ Lab, written by Nick Huby, grad student)<br />

It is my hope that by requiring each person in the lab to be personally responsible <strong>for</strong> the upkeep <strong>of</strong><br />

the solvent stills the burden that ef<strong>for</strong>t this entails will be equally shared throughout the lab community.<br />

Somewhat optimistically I also hope that this will also engender a greater sense <strong>of</strong> responsibility by people<br />

at all times when using these pieces <strong>of</strong> communal apparatus.<br />

I have decided quite arbitrarily and <strong>of</strong> my accord that each person's period <strong>of</strong> responsibility will<br />

run from twelve noon Wednesday through to twelve noon the following Wednesday. During this time it is<br />

their responsibility to:<br />

i) ensure that the stills are being used in a responsible manner<br />

ii) ensure that the stills do not get dangerously low, i.e. they are filled up as required<br />

iii) ensure that there is an adequate supply <strong>of</strong> pre-dried solvent available to fill the stills with when<br />

required<br />

iv) ensure that the pre-dried solvent bottles contain an adequate amount <strong>of</strong> sodium ribbon<br />

v) ensure that the stills are kept in a usable state, i.e. diethyl ether, tetrahydr<strong>of</strong>uran, and hexane<br />

stills retain the blue color <strong>of</strong> sodium benzophenone ketyl<br />

vi) ensure that water tubing to condensers and argon tubing does not leak<br />

vii) ensure that argon cylinder is not empty<br />

viii) ensure that there is mineral oil in both bubblers<br />

Their period <strong>of</strong> responsibility <strong>for</strong> a still will be extended, as necessary, until that still is in a usable<br />

condition.<br />

Ether<br />

Diethylether <strong>for</strong> use in the still is pre-dried over sodium ribbon and is kept in a bottle in the solvent<br />

cupboard under the oven. Only fill this bottle with anhydrous ether, since anesthesia and<br />

chromatography/extraction grade ether both contain ethanol which reacts with sodium. Sodium ribbon is<br />

used as it has a large surface-to-volume ratio and it can be added directly to the solvent be<strong>for</strong>e the sodium<br />

surface can be tarnished by atmospheric moisture. It will at times be necessary to add further sodium ribbon<br />

to the bottle as old sodium ribbon is consumed. If the build up <strong>of</strong> junk in the bottles becomes too great<br />

most <strong>of</strong> the ether will have to be decanted <strong>of</strong>f, the bottle cleaned, and fresh sodium added to the ether which<br />

was decanted <strong>of</strong>f (follow instructions given <strong>for</strong> starting still from scratch.)<br />

Once pre-dried the ether can be added directly to the ether still. The still also contains sodium<br />

ribbon, the blue color is due to sodium benzophenone ketyl. Provided that the ether is dry it is only<br />

necessary to add a spatula or so <strong>of</strong> benzophenone to obtain this blue color.<br />

140


The oxidation potential <strong>of</strong> sodium is such that it can reduce water and liberate hydrogen gas<br />

concomitantly <strong>for</strong>ming sodium hydroxide. In the presence <strong>of</strong> alcohols the corresponding sodium alkoxide is<br />

<strong>for</strong>med. In the absence <strong>of</strong> water and alcohols (the most likely contaminants) sodium metal can donate an<br />

electron to the carbonyl group <strong>of</strong> benzophenone to <strong>for</strong>m the resonance stabilized ketyl radical.<br />

Ketyl radical is a very sensitive indicator <strong>for</strong> traces <strong>of</strong> moisture and oxygen(a diradical in the<br />

ground state) and the blue color will occasionally be lost during the normal usage <strong>of</strong> the still due to<br />

consumption <strong>of</strong> benzophenone ketyl by the above contaminants. The blue color can be returned in one <strong>of</strong><br />

the following ways:<br />

i) addition <strong>of</strong> further benzophenone and continued refluxing until dry.<br />

ii) crushing the sodium with a glass rod to expose a clean, reactive surface.<br />

iii) starting the still up from scratch. This will periodically occur when the amount <strong>of</strong> reduction<br />

products in the distillation flask build up beyond a certain level or if some idiot pours ether in the<br />

still.<br />

To start the still up from scratch<br />

First destroy any remaining sodium in the flask by slow addition <strong>of</strong> ethanol to the residue<br />

remaining in the flask. This is best carried out in a fume hood as hydrogen will evolve, the flask will grow<br />

warm and ether may be boiled <strong>of</strong>f. the reaction may be slowed by dilution with hexane. Once rapid<br />

evolution <strong>of</strong> hydrogen has ceased cautiously add water to make certain that all the sodium has been<br />

destroyed. Clean out and dry the flask. Refill the flask with pre-dried ether and then add sodium ribbon.<br />

Reflux the ether <strong>for</strong> several hours to make sure it is thoroughly dry be<strong>for</strong>e adding benzophenone.<br />

THF<br />

Instructions <strong>for</strong> the use <strong>of</strong> the THF are still the same as <strong>for</strong> the ether still except that the pre-dried<br />

THF bottle (kept in the solvent cupboard under the oven) may be filled with regular grade solvent from the<br />

blue Fisher can in the solvent room.<br />

Hexane<br />

As with the ether and THF, hexane is dried over and distilled from sodium using benzophenone as<br />

its indicator. Because <strong>of</strong> the low solubility <strong>of</strong> benzophenone in this solvent it is necessary to add<br />

approximately ten milliliters <strong>of</strong> dry triglyme (a high boiling point poly-ether) as a co-solvent so that the<br />

strong color reaction is observed. The blue color <strong>of</strong> the ketyl radical may at times be lost when the still is<br />

left to stand at room temperature because <strong>of</strong> this solubility problem but the color should return upon<br />

refluxing <strong>for</strong> a short while.<br />

Hexane does not absorb a lot <strong>of</strong> water and the regular grade <strong>of</strong> hexane found in the blue cans in the<br />

solvent room can be used to top up the pre-dried solvent bottle.<br />

Dichloromethane<br />

Halogenated solvents should never be dried over sodium. This could cause the <strong>for</strong>mation <strong>of</strong><br />

carbenes.<br />

Dichloromethane is dried by distillation from calcium hydride (kept in a desiccator above the<br />

balances.) There is no need to pre-dry dichloromethane <strong>for</strong> use in the still, so the still may be topped up<br />

with solvent directly from the can. Never use sodium metal as a drying reagent <strong>for</strong> Halogenated solvent<br />

(Carbenes are <strong>for</strong>med).<br />

Sodium Ribbon<br />

As noted be<strong>for</strong>e, sodium ribbon is used to dry ether, THF, and hexane because <strong>of</strong> its large surfaceto-volume<br />

ratio and the high reactivity <strong>of</strong> the fresh sodium face which is exposed. Sodium ribbon is <strong>for</strong>med<br />

by use <strong>of</strong> a sodium press (kept in the bottom corner cupboard under the stills.)<br />

Secure the body <strong>of</strong> the press assembly to the edge <strong>of</strong> a work top with two clamps provided. The<br />

movable barrel <strong>of</strong> the die screws on to the notched vertical bar in the press assembly and is moved up and<br />

down by means <strong>of</strong> the lever at the right hand side.<br />

141


Fill the body <strong>of</strong> the die with lumps <strong>of</strong> cut sodium. Sodium is a s<strong>of</strong>t metal and can be easily cut<br />

with a sharp knife. This is best carried out while holding the lump <strong>of</strong> sodium with a pair <strong>of</strong> tweezers under<br />

hexane (the hexane serves to wash <strong>of</strong>f the mineral oil in which the sodium is stored and prevent the sodium<br />

from reacting with the atmospheric moisture.) Sodium should not be handled with your bare hands as it will<br />

react with moisture in your skin to <strong>for</strong>m sodium hydroxide. That slimy feeling is your skin getting turned<br />

into soap!<br />

Place the die onto the plat<strong>for</strong>m <strong>of</strong> the press assembly with the rounded side facing outwards.<br />

Rotate the lever until sodium ribbon is <strong>for</strong>ced from the slit at the bottom <strong>of</strong> the die. This requires ef<strong>for</strong>t!<br />

Have someone standing ready so that the sodium is squeezed directly into the bottle or flask and a minimum<br />

amount <strong>of</strong> reaction occurs with atmospheric moisture. Break the sodium ribbon <strong>of</strong>f with a pair <strong>of</strong> tweezers<br />

and push it below the surface <strong>of</strong> the solvent to be dried.<br />

To remove the barrel from the die body it may be necessary to unscrew the two parts from the<br />

notched vertical bar, placing the barrel and die so that the lower collar is below the level <strong>of</strong> the plat<strong>for</strong>m and<br />

then screwing the barrel onto the notched vertical bar with the lever.<br />

This will have to be repeated three or four times to obtain sufficient sodium ribbon <strong>for</strong> a still. Two<br />

or three repetitions should be sufficient <strong>for</strong> a pre-dried solvent bottle.<br />

After using this piece <strong>of</strong> apparatus fragments <strong>of</strong> sodium metal left in contact with the die and in the<br />

hexane used <strong>for</strong> cutting up lumps <strong>of</strong> sodium may be cleaned and dried in the oven.<br />

Addition <strong>of</strong> sodium to wet solvents will result in the evolution <strong>of</strong> hydrogen. It is prudent not to<br />

tightly stopper a container until rapid hydrogen evolution has ceased to avoid a pressure build up. It is<br />

probably best to leave pre-dried solvent bottles standing in a fume hood overnight first, then break up the<br />

sodium ribbon with a glass rod be<strong>for</strong>e returning the solvent bottle to storage.<br />

142


Standard Operating procedure <strong>for</strong> use <strong>of</strong> the Bomb Calorimeter in the Physical<br />

Chemistry Teaching Laboratory, written by Jason Weibel, graduate student.<br />

The bomb calorimeter is used in the determination <strong>of</strong> the enthalpy <strong>of</strong> combustion <strong>of</strong> a given<br />

sample. Although the samples and equipment used in the experiment are relatively safe and fool-pro<strong>of</strong>, <strong>care</strong><br />

must be taken and, as always, some common sense used. Consult the physical chemistry lab TA‟s manual<br />

<strong>for</strong> in<strong>for</strong>mation about the specific experiment run during the course <strong>of</strong> the semester.<br />

Experimental Setup<br />

1) Connect the equipment required <strong>for</strong> the experiment as shown in the physical chemistry lab TA‟s<br />

manual. Consult the sample containers <strong>for</strong> any specific precautions or concerns in the use <strong>of</strong> the<br />

chemicals.<br />

2) The bomb calorimeter requires an atmosphere <strong>of</strong> oxygen gas surrounding the sample. Obtain a<br />

cylinder <strong>of</strong> the gas and connect to the system. Be sure to secure the gas cylinder to the lab bench<br />

or other immobile, stationary object be<strong>for</strong>e attempting to per<strong>for</strong>m any operations with the cylinder,<br />

including connecting it to the system. Consult the standard safety procedures <strong>for</strong> use <strong>of</strong> gas<br />

cylinders and specifically the in<strong>for</strong>mation concerning the use <strong>of</strong> oxygen cylinders. Also determine<br />

the type <strong>of</strong> regulator required and the <strong>care</strong> and handling <strong>of</strong> such be<strong>for</strong>e putting a regulator on the<br />

system.<br />

Experimental Procedure<br />

1) Make a pellet <strong>of</strong> the sample using the pellet press. Examine the sample container <strong>for</strong> specific<br />

in<strong>for</strong>mation about the chemicals.<br />

2) Place the pellet in the calorimeter and secure the top <strong>of</strong> the bomb. Take <strong>care</strong> to make sure that the<br />

bomb is properly threaded into its connection on the calorimeter.<br />

3) Flush the system with O2 gas. Make sure that the exhaust nozzle <strong>of</strong> the system is in a position to<br />

minimize the chance that anyone will be harmed by objects in or around the bomb calorimeter that<br />

may become dislodged while flushing the system. Close the exhaust nozzle and fill the sample to<br />

approximately 25 atmospheres, watching the pressure gauge on the calorimeter to make sure that<br />

the pressure does not become too high. After the system is brought to the correct pressure, close<br />

the connection to the oxygen cylinder and then open the exhaust nozzle. After the pressure in the<br />

bomb calorimeter returns to atmospheric, close the exhaust nozzle and repeat two more times.<br />

4) Combustion <strong>of</strong> the sample. After the final flushing <strong>of</strong> the sample close the exhaust nozzle and again fill<br />

the bomb calorimeter with oxygen to a pressure slightly greater than 25 atmospheres. MAKE<br />

SURE THAT THE CONNECTION TO THE OXYGEN GAS CYLINDER IS CLOSED AND<br />

PREPARE TO FIRE THE BOMB. If the pressure in the calorimeter is falling slightly, wait until<br />

the pressure is 25 atmospheres and then press the fire button on the calorimeter, if the pressure is<br />

steady simply press the fire button.<br />

5) After the temperature in the bomb has reached a steady value prepare to remove the top <strong>of</strong> the system.<br />

Open the exhaust nozzle <strong>of</strong> the system following the precautions listed in step 3. After the system<br />

has returned to atmospheric pressure unthread the top <strong>of</strong> the bomb and remove. Check <strong>for</strong><br />

anything that appears unusual and then remove the sample holder. The parts <strong>of</strong> the system may<br />

have become hot, so use caution in handing the components <strong>of</strong> the system. Clean the components<br />

<strong>of</strong> the system and repeat experiment as many times as is called <strong>for</strong>.<br />

143


In-house Monitoring <strong>of</strong> Research Laboratory Safety Conditions<br />

In an ef<strong>for</strong>t to encourage closer scrutiny <strong>of</strong> possible safety problems within each research<br />

laboratory, the Laboratory Manager is asking each research group to consider filling out the following two<br />

<strong>for</strong>ms weekly (or bi-weekly) and keep them recorded in a notebook or file close to your Chemical Hygiene<br />

Plan Manual.<br />

Once a month, the Laboratory Manager will check out each laboratory and <strong>of</strong>fer suggestions <strong>for</strong><br />

improvements. The Laboratory Manager will also check the above mentioned records.<br />

An additional <strong>for</strong>m <strong>for</strong> overnight reactions is meant <strong>for</strong> attachment on hoods next to reaction<br />

apparatus (not too close - otherwise they would burn up along with your ill-planned experiment!).<br />

Please note that additional plastic, wire, and metal hose clamps <strong>of</strong> various sizes are located in<br />

countertop drawers in the stockroom (#110) <strong>for</strong> tightening water hose connections on distillation apparatus.<br />

Also, the Laboratory Manager has ordered more miniature submersible pumps <strong>for</strong> each research laboratory,<br />

and has already distributed them. Please do not reflux overnight reactions with water faucet-condenser<br />

connections - use water bath pumps or recirculators as sources <strong>of</strong> water.<br />

Ace glass wire hose clamps are cheap and best <strong>for</strong> standard size hose connections to condenser<br />

apparatus. Order them from Ace Glass (catalog # 11145-20, tubing clamp, phone # 1-800-223-4524).<br />

Keep all or only a portion <strong>of</strong> the following procedures in your CHP, depending upon whether they<br />

are actually applicable to your laboratory setting. If some <strong>of</strong> the instruments or facilities listed in the nightly<br />

shutdown procedure are not present in your lab, discard these entries. If you would rather extend the time<br />

period <strong>for</strong> inspections or change the days, etc., just change the <strong>for</strong>ms via work processor and write your<br />

own. At the very least, please use the “overnight reaction in progress” <strong>for</strong>m with all indicated phone<br />

numbers <strong>for</strong> emergency contact.<br />

144


OVERNIGHT REACTION IN PROGRESS<br />

In case <strong>of</strong> malfunction, please contact:<br />

Graduate Student<br />

Phone Number<br />

Dr.<br />

Phone Number<br />

Actions to be take in case <strong>of</strong> malfunction:<br />

1. Turn <strong>of</strong>f the stirrer/hotplate<br />

2. Cut <strong>of</strong>f water faucet<br />

3. Call security in case <strong>of</strong> extensive damage (5911) or clear<br />

indications <strong>of</strong> problems with fire, flooding, electrical shortage, etc.<br />

4. Other<br />

145


WEEKLY CHECK LIST (DAYTIME HOURS)<br />

provided by Dr. Susan Jackels<br />

To be completed by last person to leave the laboratory each night (weekdays only). Put your initials<br />

in the appropriate space and add to notebook <strong>for</strong> record-keeping at the end <strong>of</strong> the week. You may<br />

also wish to add a few items <strong>of</strong> your own, like balances <strong>of</strong>f, lights out, oven doors closed and<br />

computers <strong>of</strong>f (especially if located next to a water faucet.<br />

Week <strong>of</strong>: Monday Tuesday Wednesday Thursday Friday<br />

Water<br />

faucets<br />

Off ?<br />

Stirrer/Hot<br />

Plate<br />

Distillation<br />

Apparatus<br />

Water<br />

Pumps<br />

Hood<br />

Sashes<br />

Rotary<br />

Evaporator<br />

Vacuum<br />

Pumps<br />

Gas/Air<br />

Jets<br />

Off ?<br />

Heat and<br />

water <strong>of</strong>f ?<br />

Off ?<br />

Closed ?<br />

Water<br />

<strong>of</strong>f ?<br />

Off ?<br />

Closed ?<br />

146


(NIGHTS AND WEEKENDS)<br />

provided by Susan Jackels<br />

Indicate the general purpose <strong>of</strong> your lab entry in comments section (study, monitor overnight<br />

reaction, lab cleanup, use NMR, GC, etc.). Indicate general state <strong>of</strong> lab in Misc. section (OK or list<br />

specific safety problems, instrument failures, difficulties with service facilities, etc.<br />

Date/Initials Time In Time Out Comments Misc. (ok?)<br />

147


Insert: "Technical In<strong>for</strong>mation Bulletin #AL-134 Handling Air-Sensitive Reagents," Aldrich Chemical<br />

Company, 1001 West Saint Paul Ave., Milwaukee, Wisconsin 53233, phone # 1-800-558-9160.<br />

https://www.sigma-aldrich.com/aldrich/bulletin/al_techbull_al134.pdf<br />

Insert: "Technical Bulletin AL-164, Handling Pyrophoric Reagents" Aldrich Chemical Company, 1001<br />

West Saint Paul Ave., Milwaukee, Wisconsin 53233, phone # 1-800-558-9160.<br />

https://www.sigma-aldrich.com/aldrich/bulletin/al_techbull_al164.pdf<br />

Insert: "Technical In<strong>for</strong>mation Bulletin AL-139, Kugelrogr Apparatus" Aldrich Chemical Company, 1001<br />

West Saint Paul Ave., Milwaukee, Wisconsin 53233, phone # 1-800-558-9160. [located in the stockroom<br />

hardcopy <strong>of</strong> the CHP, room # 110]<br />

Acronyms <strong>for</strong> shelf chemical storage codes, Dr. Bierbach’s Lab room # 107<br />

Key <strong>for</strong> Chemical Inventory‟s Location Column<br />

Symbol Location<br />

AA Amino Acids<br />

CS Center Shelf<br />

D1 Desicator Chemicals<br />

FR Refrigerator<br />

HS Halogenated <strong>Solvent</strong>s<br />

MA Mineral Acids/ Thiols<br />

MB Hydroxides/Oxides/Ammonia<br />

MO Miscellaneous Organic Salts<br />

MS Metal Salts<br />

NS N/S Heterocyclics<br />

OA Organic Acids<br />

OB Organic Bases<br />

OS Organic <strong>Solvent</strong>s<br />

PM Precious Metals<br />

QS Quarternary Salts<br />

TOX Toxic/Carcinogens<br />

VA Volatile Amines<br />

In<strong>for</strong>mation Regarding Hydr<strong>of</strong>luoric acid burn treatment, meant mainly <strong>for</strong> Dr, Ron N<strong>of</strong>tle’s<br />

Research Lab in room 117 [hardcopies located in the stockroom hardcopy <strong>of</strong> the CHP, room # 110,<br />

and in Dr. Ron N<strong>of</strong>tle’s Lab room # 117]:<br />

Links <strong>for</strong> treatment <strong>of</strong> Hydr<strong>of</strong>luoric acid burns:<br />

http://membership.acs.org/F/FLUO/hfmedbook.pdf<br />

http://www.airproducts.com/Responsibility/EHS/ProductSafety/ProductSafetyIn<strong>for</strong>mation/Safetygrams/safe<br />

tygram29.htm<br />

http://www.calgonate.com/<br />

148


IV. Training<br />

149


A. Introduction to Training<br />

Students receive safety training <strong>for</strong> each laboratory class taken in the chemistry department. This<br />

applies to all students, including undergraduate, graduate students, and post-Doctorates. As the<br />

undergraduate proceeds through more advanced lab course, he/she will be exposed gradually to more<br />

in<strong>for</strong>mative safety instruction. The bulk <strong>of</strong> such instruction takes place in the freshman and sophomore<br />

years, in Freshman Chemistry Labs, and Organic Chemistry Labs, a total <strong>of</strong> four consecutive semesters <strong>of</strong><br />

direct audio-visual, computer-assisted, and personal instruction. Higher division undergraduate labs receive<br />

printed in<strong>for</strong>mation rein<strong>for</strong>cing previous instruction and encounter more safety rules <strong>for</strong> more complicated<br />

experimental methods directly from lab instructors and chemical literature, texts, etc.<br />

One hardcopy <strong>of</strong> the Chemical Hygiene Plan (CHP) <strong>for</strong> all Laboratories is kept in the stockroom,<br />

room 110, Salem Hall. In addition to the safety text consisting <strong>of</strong> the departmental CHP, it includes the<br />

following description <strong>of</strong> in<strong>for</strong>mation presented to all undergraduate students:<br />

Graduate students and post-doctorates receive much more printed instruction and printed specific<br />

Standard Operating Procedures regarding hazardous chemicals encountered in research labs. Teaching<br />

assistants are generally beginning graduate students in the department and are expected to participate in<br />

beginning undergraduate laboratory safety instruction, since they are expected to guide undergraduates<br />

directly in implementation <strong>of</strong> lab safety rules.<br />

The undergraduate training in<strong>for</strong>mation in this section should be read by graduate students as well,<br />

since many <strong>of</strong> them will act as Teaching Assistants sooner or later. Just skim through the in<strong>for</strong>mation which<br />

does not apply to your T.A. duties.<br />

Summer Session Chemistry Department Research Undergraduates working with chemicals are also<br />

required to undergo safety training, in May or June <strong>of</strong> each year. They will read the Bowman-Gray School<br />

<strong>of</strong> Medicine‟s “The Health Hazards <strong>of</strong> Some Common Chemicals” and “Procedures <strong>for</strong> Handling<br />

Hazardous Chemical Waste” in this manual and read and sign the “Basic Safety Rules <strong>for</strong> All<br />

Undergraduate Laboratories” and view the Safety film seen by research graduate students. Bowman Gray<br />

School <strong>of</strong> Medicine’s chapter on “The Health Hazards <strong>of</strong> Some Common Chemicals” originates from their<br />

Chemical Waste Disposal: Policies and Procedures manual, 1985, pages III 2-6, and is meant not only as<br />

instruction in the specific chemical hazards <strong>of</strong> the chemicals all graduate students and all undergraduate<br />

students work with in our Labs, but also as instruction in hazards encountered in working with hazardous<br />

chemical waste.<br />

150


B. Chemical Hygiene Plan (CHP) <strong>for</strong> Freshman Chemistry Labs<br />

First semester Students <strong>of</strong> Freshman Chemistry Lab 111L receive the following audio-visual and<br />

printed in<strong>for</strong>mation, in addition to safety discussions from the departmental laboratory manager and<br />

instructors:<br />

� Video Audio-Visual Program from American Chemical Society, “Starting With Safety: An<br />

Introduction <strong>for</strong> the Academic Chemistry Laboratory”, covering the following topics;<br />

a) Handling Chemicals Safely<br />

b) Bunsen Burners and Glassware Safety<br />

c) Thermometer Safety<br />

d) Glass Tubing Safety<br />

e) Centrifuge Safety<br />

f) Dressing <strong>for</strong> Safety<br />

g) Behavior in the Laboratory<br />

h) Emergency Equipment<br />

A copy <strong>of</strong> the manual <strong>of</strong> the text <strong>of</strong> this film is kept near the Undergraduate Laboratory CHP in the<br />

stockroom, room #110.<br />

� A Chemistry Department Emergency In<strong>for</strong>mation sheet with all emergency phone numbers needed by<br />

injured students, reproduced on page 6 <strong>of</strong> this manual. This sheet is posted near all laboratory phones<br />

in the building, including the stockroom emergency phone.<br />

� Instructor‟s hand-out in<strong>for</strong>mation on laboratory check-in, which includes remarks concerning the<br />

Additional Safety Sheet (see next page), which is also handed out to each student. This sheet, titled<br />

“Additional Safety In<strong>for</strong>mation, Freshman Chemistry Labs”, includes a brief introduction to National<br />

Fire Protection Agency (NFPA) and HMIS symbols, color codes, and hazard ratings, which appear in<br />

many manufacturers‟ labels on chemical containers. Material Safety Data Sheets are also introduced.<br />

When the audio-visual presentation and discussions are finished, the students must all sign the Wake Forest<br />

University Hazard Communication Training Log <strong>for</strong>m. Throughout the semester, students are required to<br />

wear safety glasses/goggles/or side shields and obtain gloves from the stockroom window when hazardous<br />

chemicals are used <strong>for</strong> a particular experiment.<br />

Chemical preparation personnel (usually an assigned graduate student) <strong>for</strong> Freshman Chemistry<br />

Labs must follow the same safety procedures listed above, and are to regard the General Chemistry CHP as<br />

their own CHP <strong>for</strong> prep work done in room #103. In addition, they will have read the Departmental<br />

Chemical Waste manual and will prepare chemical waste containers <strong>for</strong> the freshman labs. During the<br />

safety film students are told that their teacher (or graduate student teaching assistant) will be handling the<br />

chemical waste generated in these labs.<br />

151


1. Additional Safety In<strong>for</strong>mation, Chemistry Lab 108L and 111L<br />

1. Please note that two first aid kits are located in the chemistry stockroom, room # 110. For minor<br />

emergencies (cuts, burns), please notify your TA or instructor and call Student Health Services during<br />

daylight hours and University Security at night. For more serious injuries (breathing difficulties, severe<br />

lacerations, broken bones, etc.) call 911. Phones <strong>for</strong> emergency use are located in the chemistry<br />

stockroom (#110). All emergency phone numbers are posted on the wall next to the phone. TAKE<br />

SPECIAL NOTE OF THE POISON CONTROL CENTER PHONE NUMBER LISTED AT THE<br />

BOTTOM OF THE EMERGENCY INFORMATION PHONE # SHEET. Call this number if you<br />

ingest or are otherwise harmed by a chemical. Be sure to tell the Poison Control Center operator which<br />

chemical has affected you, or they will not be able to help. This is a very good source <strong>of</strong> in<strong>for</strong>mation.<br />

They can fax the in<strong>for</strong>mation to you <strong>for</strong> physician use at the Chemistry departmental fax #, 336-758-<br />

4656.<br />

2. An emergency oxygen breathing device is located in the stockroom (room #110).<br />

3. Take the time to find safety equipment located in the hallway adjacent to your assigned lab room,<br />

including fire blankets and dry powder fire extinguishers <strong>for</strong> wood or paper fires. The CO2 (carbon<br />

dioxide) fire extinguishers in your lab room work best <strong>for</strong> electrical and organic chemical solvent fires.<br />

When you must use the extinguishers, you will first have to pull the retaining ring out <strong>of</strong> the<br />

extinguisher handle by TWISTING THE PIN LATERALLY TO BREAK THE PLASTIC TIE and<br />

then pulling out the pen, away from the cylinder.<br />

4. Many chemicals used in the lab must be collected in proper containers <strong>for</strong> waste disposal. You will<br />

receive special instructions about disposing <strong>of</strong> any unusually dangerous chemicals. Otherwise, follow<br />

the instructions listed in your lab texts and manuals, or those given by your Teaching Assistant.<br />

5. Material Safety Data Sheets (MSDS) <strong>for</strong> each and every chemical you will encounter in this course are<br />

located in the Chemistry Stockroom (room #110) and are available <strong>for</strong> you anytime you wish to obtain<br />

in<strong>for</strong>mation regarding health hazards encountered in working with the chemical. Read both MSDS<br />

explanatory wall charts located in the hallway between rooms 101 and 105. The Chemical<br />

Hygiene Plan and Safety Manual <strong>for</strong> this course is located in the Chemistry Stockroom (room #110)<br />

next to the MSDS sheet collection.<br />

6. Read the third wall chart located in the hallway between rooms 101 and 105, explaining the<br />

multicolored Hazard Material Identification System (HMIS) labels and the National Fire<br />

Protection Association (NFPA) system labels <strong>for</strong> rating chemical hazards. Some chemical<br />

companies print these hazard labels on their chemical containers. You will encounter some in your lab<br />

and OSHA requires that you be familiar with the numerical / color-coded hazard ratings. Each <strong>of</strong> these<br />

three colored, hazard category fields <strong>for</strong> a chemical (toxicity, flammability, and reactivity) receives a<br />

numerical rating from 0 to 4, with 0 being least dangerous and 4 meaning most dangerous.<br />

7. When you go upstairs to the lab, make certain you have all the equipment listed on your check-in sheet,<br />

which will be located on your lab bench along with a lab student identification card. Discard the<br />

check-in sheet when you are finished with it. Print your name on top <strong>of</strong> the lab card, which will also be<br />

used to record the glassware you break throughout the semester, and give it to the stockroom clerk.<br />

Obtain safety glasses from the stockroom window. We have one style <strong>for</strong> people with normal<br />

vision and another “oversized” style to fit over prescription eyeglasses. The safety glasses will be<br />

your personal property <strong>for</strong> the rest <strong>of</strong> the semester, not to be shared with students in other lab sections.<br />

Don‟t leave them in your locker drawer. Take them home and bring them to each Lab session. Please<br />

return them to the stockroom at the end <strong>of</strong> the semester.<br />

152


2. HMIS / NFPA Chemical Hazard Ratings on Departmental MSDS Sheets<br />

Although the OSHA Laboratory Standard is the particular law applicable to an academic<br />

laboratory setting, it should also include the requirements <strong>for</strong> hazardous chemical assessment contained in<br />

the previous standard, the Hazard Communication Standard.<br />

“....Chemical manufacturers and importers shall evaluate chemicals produced in their workplace<br />

or imported by them to determine if they are hazardous. Employers are not required to evaluate<br />

chemicals unless they choose not to rely on the evaluation per<strong>for</strong>med by the chemical<br />

manufacturer or importer <strong>for</strong> the chemical to satisfy this requirement.”<br />

“Chemical manufacturers, importers, or employers evaluating chemicals shall describe in<br />

writing the procedures they use to determine the hazards <strong>of</strong> the chemical they evaluate. The<br />

written procedures are to be made available, upon request, to employees, their designated<br />

representatives, the Assistant Secretary and the Director. The written description may be<br />

incorporated into the written hazard communication program....”<br />

“The hazard determination requirement <strong>of</strong> this standard is per<strong>for</strong>mance-oriented. Chemical<br />

manufacturers, importers, and employers evaluating chemicals are not required to follow any<br />

specific methods <strong>for</strong> determining hazards, but they must be able to demonstrate that they have<br />

adequately ascertained the hazards <strong>of</strong> the chemicals produced or imported in accordance with the<br />

criteria set <strong>for</strong>th....”<br />

“The standard’s design is simple. Chemical manufacturers and importers must evaluate the<br />

hazards <strong>of</strong> the chemicals they produce or import. Using that in<strong>for</strong>mation, they must then prepare<br />

labels <strong>for</strong> containers, and more detailed technical bulletins called material safety data sheets<br />

(MSDS).<br />

Chemical manufacturers, importers, and distributors <strong>of</strong> hazardous chemicals are all<br />

required to provide the appropriated labels and [MSDS] to the employers to which they ship the<br />

chemicals. The in<strong>for</strong>mation is to be provided automatically. Every container <strong>of</strong> hazardous<br />

chemicals you receive must be labeled, tagged, or marked with the required in<strong>for</strong>mation. Your<br />

suppliers must also send you a properly completed....MSDS....at the time <strong>of</strong> the first shipment <strong>of</strong><br />

the chemical, and with the next shipment after the MSDS is updated with new and significant<br />

in<strong>for</strong>mation about the hazards.<br />

You can rely on the in<strong>for</strong>mation received from your suppliers. You have no independent<br />

duty to analyze the chemical or evaluate the hazards <strong>of</strong> it.”<br />

(29 CFR Chpt. XVII (7-1-95 Edition), 1910.1200 and Appendices C and E).<br />

OSHA generally endorses a universal method <strong>of</strong> hazard assessment originated by the National Paint and<br />

Coatings Association.<br />

This department rates all newly received chemicals with the National Paint and Coatings<br />

Association‟s Hazardous Materials Identification System (HMIS). The laboratory manager has<br />

determined that this practice serves as a convenient system <strong>for</strong> listing individual “particularly<br />

hazardous substances” (that is, carcinogens/mutagens/teratogens/acutely toxic compounds). The<br />

HMIS system is similar in most respects to the National Fire Protection Association system (NFPA). The<br />

NFPA system lists various hazards which are included in the HMIS numerical classification already. See<br />

page 49 <strong>of</strong> Prudent Practices, 2nd edition. A commercial HMIS “Implementation Manual” is also kept in<br />

the Chemistry Department stockroom, room # 110. Both systems serve as a nationally recognized method<br />

<strong>of</strong> rating hazards. All lab chemical suppliers and manufacturers publish Material Safety Data Sheets<br />

(MSDS) <strong>for</strong> chemicals they sell and many supply HMIS / NFPA ratings either on the MSDS or the chemical<br />

bottle label.<br />

This department maintains a set <strong>of</strong> complete MSDS sheets in the stockroom, room # 110, with<br />

HMIS / NFPA ratings printed in the upper right-hand margin on the first page <strong>of</strong> each sheet set. They are<br />

153


ated by stockroom personnel and based on in<strong>for</strong>mation stated in the MSDS sheets. The rating system is<br />

explained below. Chemical manufacturers are legally responsible <strong>for</strong> reliability <strong>of</strong> in<strong>for</strong>mation supplied on<br />

MSDS sheets. When HMIS ratings are not supplied by them, this department will supply them by criteria<br />

listed on the next few pages. SINCE AN ACADEMIC DEPARTMENT LACKS INDUSTRIAL HAZARD<br />

ASSESSMENT CAPABILITY, WAKE FOREST UNIVERSITY CANNOT IN ANY WAY BE HELD<br />

LIABLE FOR THE ACCURACY OF DEPARTMENTALLY SUPPLIED HMIS RATINGS.<br />

Summaries <strong>of</strong> the HMIS / NFPA systems and MSDS sheets in wall chart <strong>for</strong>m are kept in the<br />

undergraduate laboratory hallway bulletin boards, located near the stockroom, room # 110. You are<br />

required to first consult this manual, and read the wall charts <strong>for</strong> basic required introductory in<strong>for</strong>mation. If<br />

you need further elaboration, then view the departmental video entitled “Hazardous Materials<br />

Communication Program, Bowman Gray School <strong>of</strong> Medicine”, kept by the laboratory manager. Also, the<br />

National Paint and Coatings Association Implementation Manual is kept with the laboratory manager <strong>for</strong><br />

your reference if requested.<br />

The ratings are also listed in the inventory <strong>of</strong> all MSDS sheets <strong>for</strong> Salem Hall and <strong>for</strong> each<br />

chemical in each research laboratory.<br />

Please consult the MSDS word dictionary in the training section <strong>of</strong> this manual <strong>for</strong> explanations <strong>of</strong><br />

rating terminology. Note, in particular, that LD subscript 50 refers to lethal dose <strong>of</strong> 50% <strong>of</strong> the population<br />

<strong>of</strong> tested animals. Nearly all <strong>of</strong> the toxicity ratings are based on animal data.<br />

3. HMIS and MSDS Clarifications<br />

Clarification <strong>of</strong> Laboratory Manager‟s reasons <strong>for</strong> continuing to maintain paper copies <strong>of</strong> MSDS, updating<br />

inventory <strong>of</strong> all chemicals within the department, and use <strong>of</strong> HMIS ratings system. (Written by Julianne<br />

Braun, graduate student):<br />

Legal requirements - types <strong>of</strong> hazards, MSDS<br />

29CFR 1910.1450(h)(1)(ii) “Employers shall maintain any material safety data sheets that are<br />

received with incoming shipments <strong>of</strong> hazardous chemicals, and ensure that they are readily accessible<br />

to laboratory employees.”<br />

29CFR 1910.1450(e)(3)(viii) [The chemical hygiene plan shall include…] “Provisions <strong>for</strong><br />

additional employee protection <strong>for</strong> work with particularly hazardous substances. These include<br />

“select carcinogens”, reproductive toxins and substances which have a high degree <strong>of</strong> acute toxicity.<br />

…”<br />

Why use inventory & ratings to comply ?<br />

The law requires that special treatment be given to certain classes <strong>of</strong> substances. The only way to be<br />

able to comply with the law is to identify which substances we have which require special treatment. The<br />

best means <strong>of</strong> doing this appears to be through an inventory <strong>of</strong> all chemicals in the department. The<br />

inventory can then be cross-referenced with lists <strong>of</strong> those substances requiring special handling.<br />

The OSHA Laboratory Standard (29 CFR 1910.1450) specifically lists those substances which must be<br />

treated as “select carcinogens”, but <strong>for</strong> reproductive toxins and <strong>for</strong> “substances which have a high degree <strong>of</strong><br />

acute toxicity” criteria are given, but not specific lists. The law places the responsibility <strong>for</strong> determining<br />

which chemicals meet the criteria (and thus require special handling, storage, waste removal and<br />

decontamination procedures) on the employer. Because all <strong>of</strong> the MSDS which have been filed in the<br />

MSDS library in the stockroom have been rated according to the HMIS system, it was determined that the<br />

HMIS system <strong>of</strong> ratings would be the most efficient means <strong>for</strong> determining which chemicals meet the<br />

OSHA criteria <strong>for</strong> “reproductive toxins” and “substances which have a high degree <strong>of</strong> acute toxicity”<br />

without having to use some new rating system and rate all our existing MSDS with the new system.<br />

MSDS - paper vs. CD-ROM or network access<br />

Because OSHA requires that MSDS from each source <strong>of</strong> supply be maintained, it is not feasible to attain<br />

legal compliance by use <strong>of</strong> a pre-packaged CD-ROM <strong>of</strong> MSDS. The time and resources required to scan all<br />

<strong>of</strong> our existing MSDS into a custom CD-ROM would probably far exceed their usefulness. Legal<br />

compliance matters aside, I think it would be great to get some health and safety in<strong>for</strong>mation available to<br />

faculty and students via a networked CD-ROM. When considering how much <strong>of</strong> our resources should be<br />

spent on this, please keep in mind that MSDS <strong>for</strong> all chemicals sold by Fisher are available via WWW at<br />

URL http://www.fisher1.com., and from Sigma-Aldrich at:<br />

http://www.sigma-aldrich.com/saws.nsf/msdshelp?OpenForm<br />

154


4. INTERPRETING CHEMICAL HAZARD HMIS RATINGS<br />

The HMIS (Hazardous Material In<strong>for</strong>mation System) rating consists <strong>of</strong> a set <strong>of</strong> three numbers<br />

representing Acute (or immediate) Toxicity, Fire, and Reactivity, in that order, followed by a letter code <strong>for</strong><br />

Personal Protection Equipment and ending with a letter(s) <strong>for</strong> Chronic (or long-term) Toxicity, if necessary.<br />

The numerical hazard ratings are as follows:<br />

4 - severe hazard Chemical Inventory Safety Data Column Key<br />

3 - serious hazard ct = Chronic toxicity hazard, if indicated by an asterisk<br />

2 - moderate hazard at = Acute Toxicity fl = Flammability<br />

1 - slight hazard re = Reactivity pe = personal protective equipment<br />

0 - minimal hazard ct2 = actual description <strong>of</strong> Chronic toxicity hazard<br />

The Personal Protection Equipment code (PPE) begins with letter A <strong>for</strong> least equipment needed<br />

(safety glasses), through H (the most common – standing <strong>for</strong> use <strong>of</strong> safety glasses, lab coat, gloves, and a<br />

hood) and ends with K <strong>for</strong> something extremely dangerous and requiring elaborate protection, such as selfcontained<br />

breathing apparatus. Note that a good fume hood may normally be used in place <strong>of</strong> respirators.<br />

An asterisk next to the Acute Toxicity rating in the first column on the left indicates that a special<br />

“Chronic”, or long-term, hazard exists <strong>for</strong> the chemical, and will be identified by an additional letter(s)<br />

immediately following the capitol letter designation <strong>for</strong> PPE in the last column on the right. In some cases,<br />

a chemical could have more than one chronic health hazard letter designation. These special hazards are:<br />

M –mutagen <strong>Example</strong>: <strong>for</strong> Benzene, *330Hcm<br />

m - suspected mutagen Acute toxicity is 3, with an associated Chronic hazard<br />

T – teratogen Flammability rating is 3<br />

t - suspected teratogen Reactivity rating is 0<br />

C – carcinogen PPE rating is H<br />

c - suspected carcinogen Chronic toxicity rating is cm<br />

A – allergen (<strong>for</strong> suspected carcinogen and<br />

S - can cause silicosis suspected mutagen)<br />

Note that chronic health hazards may also be indicated in plain English on the container<br />

label and/or the MSDS sheet. Chemicals bought from a company and sent without MSDS sheets must be<br />

assumed to have ratings in each category <strong>of</strong> 4 until proven otherwise. Missing hazard data in any category<br />

<strong>of</strong> an MSDS sheet will likewise result in a rating <strong>of</strong> 4 unless the faculty or the laboratory manager judges<br />

the chemical deserving <strong>of</strong> a lower rating based on knowledge <strong>of</strong> chemical properties.<br />

155


5. SOME HMIS RATINGS FOR COMMON CHEMICALS<br />

Concentrated H2SO4 302H Chalk 000A<br />

(Sulfuric acid) toxicity rating is 3<br />

flammability rating is 0<br />

Reactivity /Corrosivity rating is 2<br />

PPE is H (Splash Goggles, gloves,<br />

synthetic apron, vapor respirator)<br />

NaOH 302H Ether 340H<br />

Chlorox 201B Acetone 131H<br />

(Sodium hypochlorite)<br />

Antifreeze 2*10Am Methanol 240C<br />

(Ethylene glycol) *Suspected mutagen<br />

CdSO4 300C MgSO4 200C<br />

PbCrO4 4*00HC FeSO4 200A<br />

*Carcinogen<br />

PbO2 3*00FT Acetic Acid 322H<br />

*Teratogen<br />

toxicity rating is 3<br />

flammability rating is 0<br />

Reactivity /Corrosivity rating is 0<br />

PPE is F (Splash glasses, gloves<br />

synthetic apron, dust respirator)<br />

156


6. Summary <strong>of</strong> HMIS Ratings<br />

(from National Paint and Coatings Association's "HMIS Hazardous Materials Identification System<br />

Implementation Manual", 1981, page 109, reprinted by American Labelmark Co., Labelmaster Division,<br />

Chicago, Illinois.)<br />

I. "Health Hazard Rating<br />

0 Minimal Hazard No significant risk to health.<br />

1 Slight Hazard Irritation or minor reversible injury possible.<br />

2 Moderate Hazard Temporary or minor injury may occur.<br />

3 Serious Hazard Major injury likely unless prompt action is taken and medical treatment given<br />

4 Severe Hazard Life-threatening, major <strong>of</strong> permanent damage may result from single or<br />

repeated exposures.<br />

II. Flammability Hazard Rating<br />

0 Minimal Hazard Materials that are normally stable and will not burn unless heated.<br />

1 Slight Hazard Materials that must be preheated be<strong>for</strong>e ignition will occur. Flammable liquids<br />

in this category will have flash points (the lowest temperature at which ignition<br />

will occur) at or above 200�F (NFPA Class IIB).<br />

2 Moderate Hazard Material that must be moderately heated be<strong>for</strong>e ignition will occur, including<br />

flammable liquids with flash points at or above 100�F and below 200�F (NFPA<br />

Class II & Class IIIA).<br />

3 Serious Hazard Materials capable <strong>of</strong> ignition under almost all normal temperature conditions,<br />

including flammable liquids with flash points below 73�F and boiling points<br />

above 100�F as well as liquids with flash points between 73�F and 100�F<br />

(NFPA Class 1B and 1C).<br />

4 Severe Hazard Very flammable gases or very volatile flammable liquids with flash points below<br />

73�F and boiling points below 100�F (NFPA Class 1A).<br />

III. Reactivity Hazard Rating<br />

0 Minimal Hazard Materials that are normally stable, even under fire conditions, and will not react<br />

with water.<br />

1 Slight Hazard Materials that are normally stable but can become unstable at high<br />

temperatures and pressures. These materials may react with water but they will<br />

not release energy violently.<br />

2 Moderate Hazard Materials that, in themselves, are normally unstable and will readily undergo<br />

violent chemical change but will not detonate. These materials may also react<br />

violently with water.<br />

3 Serious Hazard Materials that are capable <strong>of</strong> detonation or explosive reaction but require a<br />

strong initiating source <strong>of</strong> must be heated under confinement be<strong>for</strong>e initiation;<br />

or materials that react explosively with water.<br />

4 Severe Hazard Materials that are readily capable <strong>of</strong> detonation or explosive decomposition at<br />

normal temperatures and pressures.”<br />

IV. Personal Protective Equipment<br />

Appropriate protective equipment to be worn or used will be indicated by a letter immediately following the<br />

actual numbered HMIS rating (see the HMIS class identification sheet on the next page <strong>for</strong> letter<br />

designations).<br />

V. Chronic Health Hazards<br />

If present, will be so indicated by means <strong>of</strong> an asterisk (*) associated with the HMIS Health Hazard rating,<br />

and specified with a letter listed after the PPE letter rating. The letter designations are:<br />

M, mutagen C, carcinogen<br />

m, suspected mutagen c, suspected carcinogen<br />

T, teratogen A, allergen<br />

t, suspected teratogen S, can cause silicosis<br />

157


LETTER DESIGNATIONS OF<br />

PERSONAL PROTECTIVE<br />

EQUIPMENT FOR THE HMIS<br />

CLASS EYE HAND BODY RESPIRATOR FOOT<br />

A SAFETY GLASSES<br />

B SAFETY GLASSES GLOVES<br />

C SAFETY GLASSES GLOVES SYNTHETIC APRON<br />

D FACE SHIELD GLOVES SYNTHETIC APRON<br />

E SAFETY GLASSES GLOVES DUST<br />

F SAFETY GLASSES GLOVES SYNTHETIC APRON DUST<br />

G SAFETY GLASSES GLOVES VAPOR<br />

H SAFETY GOGGLES GLOVES SYNTHETIC APRON VAPOR<br />

I SAFETY GLASSES GLOVES DUST / VAPOR<br />

J SAFETY GOGGLES GLOVES SYNTHETIC APRON DUST / VAPOR<br />

K AIRLINE HOOD/MASK GLOVES FULL PROTECTIVE SUIT BOOTS<br />

X SITUATIONS REQUIRING SPECIAL HANDLING<br />

158


7. Hazard Communication Training Log Form<br />

Wake Forest University<br />

Hazard Communication Training Log<br />

DATE OF TRAINING: INSTRUCTOR:<br />

TIME OF TRAINING: DEPARTMENT:<br />

LOCATION OF TRAINING:<br />

Student Name (Print) Signature Student Name (Print) Signature<br />

1. 41.<br />

2. 42.<br />

3. 43.<br />

4. 44.<br />

5. 45.<br />

6. 46.<br />

7. 47.<br />

8. 48.<br />

9. 49.<br />

10. 50.<br />

11. 51.<br />

12. 52.<br />

13. 53.<br />

14. 54.<br />

15. 55.<br />

16. 56.<br />

17. 57.<br />

18. 58.<br />

19. 59.<br />

20. 60.<br />

21. 61.<br />

22. 62.<br />

23. 63.<br />

24. 64.<br />

25. 65.<br />

26. 66.<br />

27. 67.<br />

28. 68.<br />

29. 69.<br />

30. 70.<br />

31. 71.<br />

32. 72.<br />

33. 73.<br />

34. 74.<br />

35. 75.<br />

36. 76.<br />

37. 77.<br />

38. 78.<br />

39. 79.<br />

40. 80.<br />

159


C. Chemical Hygiene Plan (CHP) <strong>for</strong> Organic Chemistry Labs<br />

First semester Organic Chemistry lab (CHM 122L) students view the following audio-visual tape<br />

and receive printed safety in<strong>for</strong>mation, in addition to safety instructions from the departmental laboratory<br />

manager and instructors, as follows:<br />

* Audio-Visual Program from the American Chemical Society entitled “Introduction to<br />

Laboratory Safety,” covering the following topics;<br />

a) Chemical toxicity, Threshold Limit Values, and Permissible Exposure Levels <strong>of</strong> Vapors <strong>of</strong><br />

hazardous chemicals<br />

b) Corrosivity, Flammability, and Reactivity definitions, examples, and hazards <strong>of</strong> pyrophoric<br />

and water-reactive chemicals<br />

c) Summary <strong>of</strong> departmental requirements <strong>for</strong> MSDS sheets and sources <strong>of</strong> in<strong>for</strong>mation in<br />

departmental books and literature sources<br />

d) In<strong>for</strong>mation about the Chemical Hygiene Plan requirement, Hazardous Waste Policy, chemical<br />

spills, and the OSHA Laboratory Standard requirement <strong>for</strong> description <strong>of</strong> carcinogens,<br />

mutagens/teratogens, and extremely hazardous chemicals and the requirement <strong>for</strong> designated areas<br />

in research labs<br />

e) Segregation <strong>of</strong> chemicals, storage areas <strong>for</strong> larger volume organic solvents in cabinets under<br />

hoods in back <strong>of</strong> undergraduate Organic Chem labs<br />

f) Fifty-five gallon Acetone drum grounding wires in the solvent room (room #20) <strong>for</strong> anti-static<br />

electricity buildup<br />

h) Organic Peroxide buildup in certain bottles <strong>of</strong> old ether containers, and how to test <strong>for</strong><br />

peroxides with departmentally available test strip paper.<br />

(A copy <strong>of</strong> the major part <strong>of</strong> the text <strong>of</strong> these films is kept near the Undergraduate CHP in the<br />

stockroom, room #110.)<br />

* A Chemistry Department Emergency In<strong>for</strong>mation sheet with all emergency phone numbers<br />

needed by injured students, reproduced on page 6 <strong>of</strong> this manual. This sheet is posted on the wall<br />

next to each laboratory phone in the building, including the stockroom phone.<br />

* Instructor‟s hand-out in<strong>for</strong>mation on laboratory check-in, which includes the following<br />

laboratory safety and regulation discussion, meant as an additional source <strong>of</strong> safety instruction <strong>for</strong><br />

the student, entitled “Laboratory Safety and Regulations <strong>for</strong> Organic Labs”.<br />

� Direct Instruction in the handling <strong>of</strong> Chemical waste by reading Chapter one <strong>of</strong> their textbook,<br />

The Organic Chem Lab Survival Manual, subsection titled “Disposing <strong>of</strong> Waste”, and<br />

following all written and verbal clean-up and chemical waste handout procedures listed in the<br />

experimental instructions prepared by the Lab class instructor <strong>for</strong> each experiment. If the<br />

alternate Organic Lab text is used (Williamson, Kenneth L. Macroscale and Microscale<br />

Organic Experiments, 3rd edition, Houghton Mifflin Co., 1999), Chapter two, “Laboratory<br />

Safety and Waste Disposal,” is required reading <strong>for</strong> the students. It contains detailed<br />

in<strong>for</strong>mation on handling chemicals <strong>for</strong> the entire course.<br />

160


Laboratory Safety and Regulations, Organic Lab 122L and 223L<br />

1. Read chapter 1 <strong>of</strong> your textbook (The Organic Chem Lab Survival Manual), titled "Safety First,<br />

Last, and Always," be<strong>for</strong>e the next lab session. Follow all future experimental clean-up and chemical waste<br />

handout procedures given to you by your Lab T.A. or Lab class instructor.<br />

2. Please note that two first aid kits are located in the Chemistry Dept. Stockroom, Salem #110. For<br />

minor emergencies (cuts, burns) please notify your TA or instructor and call Student Health Services during<br />

daylight hours and University Security at night. For more serious injuries (breathing difficulties, severe<br />

lacerations, broken bones, etc.) call 911. Phones <strong>for</strong> EMERGENCY USE ONLY are located in the<br />

chemistry stockroom (Salem #110) and the Preproom (Salem #103). TAKE SPECIAL NOTE OF THE<br />

POISON CONTROL CENTER PHONE NUMBER LISTED AT THE BOTTOM OF THE EMERGENCY<br />

INFORMATION PHONE # SHEET HANDOUT. THESE SHEETS ARE ALSO POSTED ON THE<br />

WALL NEXT TO EACH PHONE IN ROOMS 110 AND 103. Dial the Poison Control Center phone<br />

number if you ingest or are otherwise badly harmed by a chemical. Be sure to tell the Poison Control<br />

Center operator which chemical has affected you, or they will not be able to help. This is a very good<br />

source <strong>of</strong> in<strong>for</strong>mation. They can fax the in<strong>for</strong>mation to the Department <strong>for</strong> physician use, at fax # 336-758-<br />

4656.<br />

3. An emergency oxygen breathing device is located in the stockroom (Salem #110).<br />

4. Material Safety Data Sheets (MSDS) <strong>for</strong> each and every chemical you will encounter in this course<br />

are located in the Chemistry Stockroom (Salem #110) and are available <strong>for</strong> you anytime you wish to<br />

obtain in<strong>for</strong>mation regarding health hazards encountered in working with the chemical.<br />

5. Read the Basic Safety Rules <strong>for</strong> All Laboratories handout on your assigned lab bench. Keep the first<br />

two pages <strong>for</strong> your reference, but sign and tear <strong>of</strong>f the last page and give it to the stockroom clerk after you<br />

have obtained missing glassware or equipment <strong>for</strong> your lab locker drawers. Obtain safety glasses from<br />

the stockroom window. We have one style <strong>for</strong> people with normal vision and another “oversized”<br />

style to fit over prescription eyeglasses. These are your personal safety glasses <strong>for</strong> the rest <strong>of</strong> the<br />

semester, to be returned when you check out, again to the stockroom window.<br />

6. Take the time to find safety equipment located in the hallway adjacent to your assigned lab room,<br />

including fire blankets and dry powder fire extinguishers <strong>for</strong> wood or paper fires. The CO2 (carbon<br />

dioxide) fire extinguishers in you lab room work best <strong>for</strong> electrical and organic chemical solvent fires.<br />

When you must use the extinguishers, you will first have to pull the retaining ring out <strong>of</strong> the extinguisher<br />

handle by TWISTING THE PIN LATERALLY TO BREAK THE PLASTIC TIE and then pulling out the<br />

pen, away from the cylinder.<br />

7. The Chemical Hygiene Plan and Safety Manual <strong>for</strong> this course is located in the Chemistry Stockroom<br />

(Salem #110) next to the MSDS sheet collection. We have MSDS sheets <strong>for</strong> each chemical in your lab.<br />

Take the time to look over the Hazardous Material Identification System (HMIS) Labeling<br />

Chart located in the hallway just across from your lab room on the bulletin board next to Salem #<br />

105. Chemical companies typically give each chemical an HMIS safety rating on their MSDS sheet.<br />

Also, skim through the 2 posted wall charts titled "Material Safety Sheets: How to Read, <strong>Use</strong>,<br />

and Understand them" and "How to <strong>Use</strong> and Understand Material Safety Data Sheets" located in the<br />

hallway between Salem #s 101 and 105, next to your lab rooms. Completely read through the wall<br />

chart titled “Hazardous Waste Chemical Inventory” on the wall next to room # 103.<br />

8. Other sources <strong>of</strong> risk assessment in<strong>for</strong>mation (i.e., how to determine whether a certain chemical is toxic<br />

or otherwise dangerous to work with) can be found in the departmental Stockroom, Salem # 110. Their<br />

descriptions follow:<br />

A very good reference <strong>for</strong> toxic hazards <strong>of</strong> general categories and classes <strong>of</strong> chemicals is:<br />

Patnaik, Pradyot. A Comprehensive Guide to the Hazardous Properties <strong>of</strong> Chemical<br />

Substances. New York: Van Nostrand Reinhold, 1992.<br />

161


Consult the following book <strong>for</strong> hazards due to reactivity <strong>of</strong> particular chemicals:<br />

Urben, P.G., ed. Bretherick's Handbook <strong>of</strong> Reactive Chemical Hazards, 4th edition. Ox<strong>for</strong>d:<br />

Butterworth-Heinemann Ltd., 1995.<br />

Another good hazardous chemical reference <strong>for</strong> particular chemicals is:<br />

Lewis, Richard J., Sr., Hazardous Chemicals Desk Reference, 3rd edition. New York:<br />

Van Nostrand Reinhold, 1993.<br />

The two volume set <strong>of</strong> Lenga, Robert E. Sigma-Aldrich Library <strong>of</strong> Chemical Safety Data, 2nd<br />

edition. Milwaukee, WI: Sigma-Aldrich Corporation, 1988, is a huge collection <strong>of</strong> safety in<strong>for</strong>mation <strong>for</strong><br />

specific Organic chemicals. The American Conference <strong>of</strong> Governmental Industrial Hygienist‟s Threshold<br />

Limit Values (TLVs) booklet is kept there as well. TLVs are the maximum allowable inhalation levels <strong>of</strong><br />

chemicals present in the laboratory air, measured in milligrams per cubic meter (mg/m 3 ) or parts per million<br />

(ppm) in the air you breathe in the immediate vicinity <strong>of</strong> your work. OSHA has adopted the TLVs and<br />

refers to them in the law as Permissible Exposure Levels (PELs). The hoods in your lab are designed to<br />

keep exposure levels below the PELs <strong>of</strong> chemicals you use. Find this booklet with the other books listed<br />

above in the Chemistry Department Stockroom, # 110.<br />

The Bowman Gray School <strong>of</strong> Medicine's summary titled "Health Hazards <strong>of</strong> Some<br />

Common Chemicals" is included in your online in<strong>for</strong>mation page <strong>for</strong> this course. You will probably<br />

find that this is the most useful source in<strong>for</strong>mation <strong>for</strong> the hazards <strong>of</strong> most <strong>of</strong> the chemicals you will<br />

be using in this lab.<br />

9. First semester Intro Organic Chemistry lab (CHM 122L) students view the following audio-visual tape<br />

and receive printed safety in<strong>for</strong>mation, in addition to safety instructions from the departmental laboratory<br />

manager and/or your instructor:<br />

* Audio-Visual Program from the American Chemical Society entitled "Introduction to<br />

Laboratory Safety," covering the following topics;<br />

a) Chemical toxicity and the three types <strong>of</strong> OSHA Permissible Exposure Levels (PELs) <strong>of</strong><br />

the relatively low air concentrations <strong>of</strong> hazardous chemicals encountered in your lab;<br />

� Time Weighted Averages (TWAs), which are averages <strong>of</strong> air concentrations<br />

measured over an 8 hour workday<br />

� Short Term Exposure Levels (STELs), which allow exposure to a higher<br />

concentration <strong>of</strong> a chemical, usually <strong>for</strong> a 15 minute period<br />

� Ceiling Limits, air concentration levels which cannot be exceded in any case,<br />

usually <strong>for</strong> irritant chemicals<br />

b) Corrosivity, Flammability, and Reactivity definitions, examples, and hazards <strong>of</strong><br />

pyrophoric and water-reactive chemicals<br />

c) Summary <strong>of</strong> departmental requirements <strong>for</strong> MSDS sheets and sources <strong>of</strong> in<strong>for</strong>mation in<br />

departmental books and literature sources<br />

d) In<strong>for</strong>mation about the Chemical Hygiene Plan requirement, Hazardous Waste Policy,<br />

chemical spills, and the OSHA Laboratory Standard requirement <strong>for</strong> description <strong>of</strong><br />

carcinogens, mutagens/teratogens, and extremely hazardous chemicals and the requirement<br />

<strong>for</strong> designated areas in research labs<br />

e) Segregation <strong>of</strong> chemicals, storage areas <strong>for</strong> larger volume organic solvents in cabinets<br />

under hoods in back <strong>of</strong> undergraduate Organic Chem labs<br />

f) Fifty-five gallon Acetone drum grounding wires in the solvent room (Salem #20) <strong>for</strong><br />

prevention <strong>of</strong> static electrical charge buildup<br />

h) Organic Peroxide buildup in certain bottles <strong>of</strong> old ether containers, and how to test <strong>for</strong><br />

peroxides with departmentally available test strip paper.<br />

162


When these audio-visuals and discussions are finished, the students must all sign the Wake Forest<br />

University Hazard Communication Training Log <strong>for</strong>m.<br />

* Lastly, the student must read the Basic Safety Rules <strong>for</strong> All Laboratories <strong>for</strong>m, sign it, and turn<br />

the signature page in to the Stockroom at check-in and pick up safety goggles along with an apron,<br />

cotton towel, and any missing equipment in their laboratory lockers. Throughout the semester,<br />

they are required to wear safety glasses/goggles/or side shields and obtain gloves from the<br />

stockroom window when hazardous chemicals are used <strong>for</strong> a particular experiment<br />

* One laboratory textbook <strong>for</strong> this course (Williamson, Kenneth L. Macroscale and Microscale<br />

Organic Experiments, 3rd edition, Houghton Mifflin Co., 1999) contains both normal-scale and<br />

micro-scale experiments, to cut down on the amount <strong>of</strong> hazardous chemical waste generated in<br />

theses labs. Chapter two, “Laboratory Safety and Waste Disposal,” is required reading <strong>for</strong> the<br />

students. It contains detailed in<strong>for</strong>mation on handling chemicals <strong>for</strong> the entire course. In addition,<br />

each experimental procedure in the book ends with a section entitled “Cleaning Up.” These<br />

contain specific waste disposal in<strong>for</strong>mation which are in all cases followed by the student as the<br />

last step in their experiments unless otherwise instructed by their T.A.‟s to follow the instructions<br />

listed by the Chemical Preparation Personnel or the Hazardous Waste Manual in the Departmental<br />

Chemical Hygiene Plan. The other textbook is titled The Organic Chem Lab Survival Manual and<br />

contains an excellent subsection in the first chapter titled “Disposing <strong>of</strong> Waste”. In addition to<br />

comments in the safety film and the Lab Instructor‟s waste guidelines <strong>for</strong> each experiment, these<br />

textbook chapters and safety film comments constitute the final training all undergraduate students<br />

receive in handling hazardous waste, unless they engage in Summer School undergraduate<br />

chemical research, in which case they are required to read the Departmental Chemical Waste<br />

manual in the Chemistry Department‟s Chemical Hygiene Plan and so certify by signing the .<br />

* The student will also be given, via the on-line Chemistry Dept web page, a handout listing<br />

Health Hazards <strong>of</strong> Some Common Chemicals to be consulted throughout the semester as specific<br />

in<strong>for</strong>mation regarding chemical hazards and toxicity. It is also listed on the next page <strong>of</strong> this<br />

manual.<br />

* Instructors and Chemical Preparation Personnel (graduate students preparing the chemicals<br />

used in the lab) occasionally write specific chemical dispensing instructions and special hazardous<br />

waste instructions <strong>for</strong> the T.A.‟s. These will be handed out during pre-lab lectures.<br />

Second semester Organic Chemistry (CHM 223L) students will receive the Emergency<br />

In<strong>for</strong>mation sheet, the Laboratory Safety and Regulations handout, the Basic Safety Rules <strong>for</strong> all<br />

Laboratories signature handout, and the electronically generated Bowman Gray Health Hazards <strong>of</strong> Some<br />

Common Chemicals.<br />

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1. Health Hazards <strong>of</strong> Some Common Chemicals<br />

(From Bowman Gray School <strong>of</strong> Medicine’s Chemical Waste Disposal: Policies and Procedures, 1985,<br />

pages III 2-6, reprinted with permission)<br />

Some <strong>of</strong> the more obviously dangerous properties <strong>of</strong> common classes <strong>of</strong> chemicals are listed here<br />

as a preliminary source <strong>of</strong> toxicity in<strong>for</strong>mation. Physical and health hazards are described, along with<br />

“signs and symptoms associated with exposures to hazardous chemicals used in the laboratory” (OSHA, in<br />

29 CFR 1910.1450). You will not be using all <strong>of</strong> these chemicals in the undergraduate labs. In fact, the<br />

more dangerous a chemical is, the less likely it will be assigned as a reagent in your lab.<br />

1. “ Acids<br />

Acetic acid is considerably more corrosive to the skin than is generally believed, readily<br />

penetrating the skin producing blisters, dermatitis, and ulcers. Even at room temperature the<br />

vapor is highly irritating to the eyes and to the nose and throat on inhalation.<br />

2. Alcohols<br />

Chromic Acid is a strong oxidizing agent but not a strong acid. It is both poisonous and irritating<br />

to the skin. Precautions should be taken against skin contact with the solid or its solutions and<br />

against inhalation <strong>of</strong> dust from the solid or <strong>of</strong> mist from the solutions. Reaction with chlorides<br />

yields chromyl chloride. Chromic acid and chromyl chloride are suspected carcinogens.<br />

Hydrochloric acid fumes are corrosive to tissues on contact.<br />

Hydr<strong>of</strong>luoric acid is extremely irritating and corrosive to the skin and mucous membranes. It<br />

produces severe skin burns which are slow in healing. Burns must be treated immediately as<br />

tissue necrosis can develop. It is highly toxic by ingestion or inhalation.<br />

Nitric acid is a powerful oxidizing agent. In the oxidation <strong>of</strong> most organic materials, concentrated<br />

nitric acid will produce dense clouds <strong>of</strong> highly toxic red or brown oxides <strong>of</strong> nitrogen. Since<br />

inhalation <strong>of</strong> these oxides in dangerous quantities produces only a mild irritation <strong>of</strong> the<br />

respiratory organs, it is possible to inhale a dangerous concentration without much discom<strong>for</strong>t or<br />

apparent injury.<br />

Picric acid is rapidly absorbed through the unbroken skin and even more rapidly through wounds,<br />

leading to headache, fever, and insomnia. Exposure to the dust <strong>of</strong> picric acid may cause irritation<br />

to the nose and throat and especially <strong>of</strong> the eyes, leading to ulceration <strong>of</strong> the cornea. It is also<br />

hazardous due to its explosive properties.<br />

Sulfuric acid (concentrated) chars and destroys plant or animal tissue because <strong>of</strong> its avidity <strong>for</strong><br />

water, which it removes from organic material with which it comes in contact. The fumes are<br />

extremely irritating both to the skin and to the mucous membranes.<br />

Phosphorus halides and oxy-halides are fuming liquids or solids which decompose rapidly in the<br />

presence <strong>of</strong> water or moist air to <strong>for</strong>m hydrochloric, phosphorous, or phosphoric acids. The<br />

vapors are strongly irritating to the skin, mucous membranes, and respiratory system.<br />

Phenol (carbolic acid) is readily absorbed through the intact skin. Liquid phenol in contact with<br />

skin produces a tingling sensation followed by a loss <strong>of</strong> feeling. The skin becomes white and<br />

wrinkled and later turns dark brown and sloughs <strong>of</strong>f. This is not a true corrosive action, but is a<br />

local gangrene caused by destruction <strong>of</strong> the blood supply to the affected area.<br />

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The alcohols show a regular dependence <strong>of</strong> narcotic action on their physical constants.<br />

Anesthetic power increases with increasing molecular weight. Butyl and amyl alcohol have in<br />

addition a slight irritant action and some degree <strong>of</strong> poisonous action on the protoplasm.<br />

Secondary alcohols are stronger narcotics than the primary alcohols. With the exception<br />

<strong>of</strong> methyl alcohol, the toxicity <strong>of</strong> the alcohols is comparatively small. Methyl alcohol is a<br />

poisonous substance and contact, as well as inhalation, should be avoided. This compound exerts<br />

a particular effect on the optic nerve and ingestion or inhalation may cause blindness.<br />

3. Glycols and alcohol-ethers<br />

These are principally blood and kidney poisons. The glycols are not considered exceedingly<br />

toxic; ethylene glycol and ethyl ether are <strong>of</strong> comparable toxicity. Cellosolve, methyl cellosolve,<br />

and carbitol are common alcohol-ethers which are considered hazardous in high concentrations.<br />

4. Aldehydes and ketones<br />

5. Alkalies<br />

6. Aniline<br />

The aldehydes are primarily irritants but they also have some narcotic action. Formaldehyde is<br />

poisonous and a concentration <strong>of</strong> 5 parts per million is considered the threshold <strong>of</strong> a safe working<br />

atmosphere. Acrolein is a lachrymator and was used in a war gas mixture.<br />

The ketones are narcotic and are markedly stimulating to the respiratory center. In comparison<br />

with some <strong>of</strong> the other solvents, they are relatively harmless although the inhalation or ingestion<br />

<strong>of</strong> large quantities can be toxic.<br />

Sodium and potassium hydroxide are white solids which are extremely soluble in water. The most<br />

common injuries suffered are burns <strong>of</strong> the skin or eyes on contact. They are especially destructive<br />

to eye tissue.<br />

Ammonia is a strong irritant and can produce sudden death from bronchial spasm, but causes no<br />

lasting harm in concentrations small enough to be severely irritating. It is absorbed readily<br />

through the respiratory tract and is rapidly metabolized so that it ceases to act as ammonia. It is<br />

particularly dangerous if splashed in the eyes.<br />

Aniline can be absorbed through the skin and is dangerous to inhale or ingest. Aniline dye<br />

compounds produce cyanoses and affect the central nervous system and bladder.<br />

7. Carbon monoxide<br />

Carbon monoxide is a chemical asphyxiant since it combines with the hemoglobin <strong>of</strong> the blood to<br />

<strong>for</strong>m a stable compound. The affinity <strong>of</strong> carbon monoxide <strong>for</strong> hemoglobin is about 300 times that<br />

<strong>of</strong> oxygen and a preferential absorption always takes place.<br />

8. Cyanides and nitriles<br />

Hydrocyanic acid is a highly toxic colorless gas with the odor <strong>of</strong> bitter almonds. It is readily<br />

absorbed through the skin at high concentrations. It blocks cellular respiration by poisoning the<br />

oxidation catalysts. It is not a respiratory irritant.<br />

Hydrogen cyanide and its simple soluble salts are among the most rapid acting <strong>of</strong> all poisons.<br />

The halogenated materials are also highly toxic and possess some <strong>of</strong> the same properties as HCN.<br />

However, at low concentrations, these materials behave more like the vesicant gases.<br />

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9. Esters<br />

10. Ethers<br />

11. Halogens<br />

Nitriles can cause the same general symptoms as HCN, but the onset is apt to be slower and they<br />

are more likely to be active as primary irritants on the skin or eye. They are also frequently<br />

absorbed rapidly and completely through the intact skin in the same manner as the cyanides. The<br />

halogenated compounds are also highly toxic and possess some <strong>of</strong> the same properties as HCN.<br />

However, at low concentrations, these materials behave more like the highly irritating vesicant<br />

gases such as phosgene and cause severe lachrymatory effect and both acute and delayed<br />

pulmonary edema and irritation.<br />

The action <strong>of</strong> the esters varies widely from the mildly anesthetic and irritant properties <strong>of</strong> ethyl<br />

acetate to the very poisonous, irritant and vesicant action <strong>of</strong> methyl sulfate and the esters <strong>of</strong><br />

<strong>for</strong>mic acid. The <strong>for</strong>mic acid esters are powerful irritants, especially the chlorinated ones. They<br />

have been used as war gases. With increase in molecular weight, the relative toxicity <strong>of</strong> the esters<br />

increases, but because <strong>of</strong> decrease in volatility, the actual danger decreases.<br />

The ethers are powerful narcotics acting rapidly on the central nervous system. They are also<br />

slightly irritant and can be dangerous if inhaled in large quantities.<br />

Chlorine is a dangerous and strong lung irritant and a concentration <strong>of</strong> one part per million <strong>for</strong><br />

an 8 hour exposure is the maximum allowed. This is also the lowest concentration <strong>of</strong>fering a<br />

detectable odor.<br />

Bromine fumes are highly irritating to the eyes and both the upper and lower sections <strong>of</strong> the<br />

respiratory tract. The maximum allowable concentration is one part per million and the least<br />

detectable odor is in the order <strong>of</strong> 3.5 parts per million.<br />

12. Hydrocarbons<br />

13. Metals<br />

Saturated aliphatic hydrocarbons are relatively harmless from the toxicological point <strong>of</strong> view.<br />

Methane and ethane are simple asphysiants; propane and butane have, in addition, anesthetic<br />

properties, while hydrocarbons from pentane and up are narcotic, convulsive and irritant.<br />

Hexane and heptane are the most dangerous.<br />

Unsaturated aliphatic hydrocarbons from ethylene to heptylene have simple asphysiant and<br />

anesthetic properties. Acetylene may also be included in this group.<br />

Cyclic hydrogenated hydrocarbons are more potent than the open chain hydrocarbons but are<br />

less toxic than the aromatic hydrocarbons. Cyclohexane has about the same toxicity as hexane<br />

but has a stronger narcotic action. They have their principal effect on the central nervous<br />

system.<br />

Aromatic hydrocarbons are much more poisonous than the aliphatic group. Benzene has a<br />

destructive influence on blood cells and blood-<strong>for</strong>ming organs following chronic exposure. It also<br />

has an acute narcotic effect and may cause intoxication, unconsciousness or death in a short time<br />

if present in high concentration. It may be carcinogenic.<br />

Halogenated hydrocarbons as a class have the general physiological effect <strong>of</strong> anesthesia and<br />

narcosis. Permanent damage may result to the liver and kidneys. The halogenated hydrocarbons<br />

<strong>of</strong> the benzene group may be blood poisons.<br />

166


Lead, mercury, arsenic, chromium, beryllium, antimony, selenium, and manganese are common<br />

hazardous metals. As a general rule, metals are more hazardous within compounds rather than<br />

the elemental state, and the more soluble the compound is, the more poisonous it is likely to be.<br />

The damage produced from inhalation <strong>of</strong> the metallic dust is greater than by swallowing.<br />

14. Compounds <strong>of</strong> sulfur, phosphorus, and nitrogen<br />

The principal mineral acids (hydrochloric, nitric, sulfuric and phosphoric) and their gases are<br />

hazardous to inhale. The fumes are very irritating to the respiratory tract.<br />

Phosphorous halides are very irritating to the respiratory tract. Formation <strong>of</strong> strong acids on<br />

contact with water can cause severe tissue burns when inhaled.<br />

Hydrogen sulfide is nearly as toxic as hydrogen cyanide but is not absorbed through the skin. Its<br />

characteristic odor is not reliable as a warning signal because higher concentrations, which have<br />

a sweetish odor, also have a paralyzing effect on the olfactory nerves. The gas paralyzes the<br />

respiratory center <strong>of</strong> the brain at toxic levels.<br />

Dimethyl sulfate is an odorless, powerful lung irritant as well as a lachrymator and vesicant. It<br />

can be absorbed through the skin and affects all the mucous membranes and the respiratory<br />

system. It is a suspected carcinogen.<br />

Nitrogen oxides are extremely dangerous because <strong>of</strong> their delayed action. Harmful and even fatal<br />

quantities can be inhaled without immediate noticeable effects. Pulmonary edema usually results<br />

from extended inhalation. Nitration operations and welding can evolve these oxides.<br />

Dimethyl sulfoxide (DMSO) penetrates the unbroken skin and enters the circulatory system<br />

extremely rapidly. It can carry with it dissolved materials which would ordinarily not penetrate<br />

the skin.”<br />

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D. Training <strong>for</strong> Graduate Students, Post-Doctorates, and Research<br />

Undergraduates<br />

All new Graduate Students are required to view the American Chemical Society film titled<br />

Introduction to Laboratory Safety, and to read the Chemical Hygiene Plan <strong>for</strong> the Chemistry Department<br />

and abide by all rules and instructions listed therein (black print text only). They are then required to sign<br />

the “Chemistry Department Certification <strong>of</strong> Safety Training” <strong>for</strong>m below and give it to the laboratory<br />

manager. Research undergraduate students will also view the film, sign the “Basic Safety Rules” <strong>for</strong>m, and<br />

read only the Safety Manual subsections stipulated below. Normally, the training stipulated here will occur<br />

in August <strong>of</strong> each year, (and during May or June <strong>for</strong> summer school research undergraduates). An annual<br />

Gas Cylinder Safety lecture will occur each January. Everyone will receive specific instruction in handling<br />

Hazardous chemical Waste.<br />

168


1. Certification <strong>of</strong> Safety Training Form <strong>for</strong> Graduate Students, Post-Graduates,<br />

and Summer School Undergraduate Research Students<br />

CHEMISTRY DEPARTMENT CERTIFICATION OF SAFETY TRAINING<br />

FOR GRADUATE STUDENTS, POST-DOCTORATES,<br />

AND SUMMER SCHOOL UNDERGRADUATE RESEARCH STUDENTS<br />

I certify that the following Graduate Student or Post-Doctorate has seen the Safety Film and<br />

received the instruction to read the Chemical Hygiene Plan and Safety Manual <strong>for</strong> Salem Hall (with special<br />

emphasis on the Bowman-Gray School <strong>of</strong> Medicine‟s “The Health Hazards <strong>of</strong> Some Common Chemicals”<br />

and “Procedures <strong>for</strong> Handling Hazardous Chemical Waste”),<br />

Or<br />

That the Summer School Research Undergraduate student listed at the bottom <strong>of</strong> this <strong>for</strong>m has<br />

seen the Safety Film and received the normal Departmental Safety Handouts (with special emphasis on the<br />

Bowman-Gray School <strong>of</strong> Medicine‟s “The Health Hazards <strong>of</strong> Some Common Chemicals” and “Procedures<br />

<strong>for</strong> Handling Hazardous Chemical Waste”).<br />

Print name <strong>of</strong> Witnessing WFU Chemistry Pr<strong>of</strong>essor<br />

Signature Date<br />

I have seen the Safety Film, received the Departmental Safety Handouts, and read the Chemistry<br />

Department‟s Chemical Hygiene Plan and Safety Manual, including the “Procedures <strong>for</strong> Handling<br />

Hazardous Chemical Waste”, and “The Health Hazards <strong>of</strong> Some Common Chemicals” and agree to abide<br />

by the rules and regulations stated therein.<br />

Print Graduate Student or Post Doc Name<br />

Signature Date<br />

I have read the Chemistry Department‟s Safety Handouts, read and signed the Basic Safety Rules <strong>for</strong> All<br />

Undergraduate Laboratories, seen the Safety Film, and read the “Procedures <strong>for</strong> Handling Hazardous<br />

Chemical Waste” and “The Health Hazards <strong>of</strong> some Common Chemicals”, and agree to abide by the rules<br />

and regulations stated therein.<br />

Undergraduate Research Student Name<br />

Signature Date<br />

169


2. Yearly Announcement <strong>of</strong> Gas Cylinder Safety and New Graduate Student Safety<br />

Review<br />

New Graduate Student Safety Review<br />

And<br />

Safe <strong>Use</strong> <strong>of</strong> Compressed Gas Cylinders and Regulators<br />

Presented by National Welders<br />

And<br />

Pipe and Swagelok Tube Fittings in Research Laboratories<br />

Presented by Dr. Robert Sw<strong>of</strong><strong>for</strong>d<br />

Tuesday, January 15, 2008<br />

9:00 AM – 1:00 PM<br />

Lecture Room # 10, Ground Floor, Salem Hall<br />

Required Attendance <strong>of</strong> all Research Graduate Students in the<br />

Chemistry Department<br />

Agenda<br />

“Be There or Be Hexagonal”<br />

Demos and Audience Participation!!<br />

9:00 AM – 10:00 AM (c<strong>of</strong>fee and donuts served):<br />

� Safety Review, required <strong>of</strong> all 1 st -year Graduate Students<br />

10:00 – 11:00 AM (c<strong>of</strong>fee and donuts served):<br />

� Gas Cylinders, National Welders, required <strong>of</strong> all Graduate Students<br />

11:00 AM – Noon<br />

� Regulators, National Welders, required <strong>of</strong> all Graduate Students<br />

Noon – 1:00 PM - FREE LUNCH and Follow-Up Discussion with Dr. Sw<strong>of</strong><strong>for</strong>d, open to all Graduate<br />

Students<br />

� Thread sizes (CGA numbers; Gas, Tube, and Pipe Fittings)<br />

� Swagelok fittings and connections<br />

� Sources <strong>for</strong> Various Fittings<br />

170


3. Summer School Safety Training Announcement <strong>for</strong> Research Undergrads:<br />

For Undergraduate Research Students, and Safety Review <strong>for</strong> Graduate Students<br />

DEPARTMENTAL SAFETY TRAINING<br />

SESSION<br />

Thursday, May 31<br />

2:00-3:00 pm<br />

Salem 10<br />

Mike Thompson<br />

Bruce King<br />

This session will be held as an orientation <strong>for</strong> new summer<br />

researchers in the department as well as first/second year<br />

graduate students. All are welcome to attend, light<br />

refreshments provided.<br />

171


4. New Graduate Student and new Undergraduate Research Student Safety<br />

Orientation Announcement, in August <strong>of</strong> each year:<br />

DEPARTMENTAL SAFETY TRAINING<br />

SESSION<br />

Tuesday, August 21<br />

1:00 – 2:30 pm<br />

Salem 210<br />

Mike Thompson<br />

Bruce King<br />

This session will be held as a Chemical Safety Orientation<br />

<strong>for</strong> new Graduate Students in the Chemistry, Physics, and<br />

NanoTechnology Departments who work with chemicals.<br />

Undergraduate Chemical Researchers are also welcome.<br />

172


V. Chemistry Department Purchase Order Request System<br />

Chemicals, equipment, and supplies are usually ordered from outside private companies with the use <strong>of</strong> two<br />

types <strong>of</strong> Purchase Order Forms as follows:<br />

A) The Department‟s new and improved computer generated Purchase Request Form, prepared by<br />

Ms. Melissa Doub, the Business Manager <strong>for</strong> the Chemistry Department, is located at:<br />

http://www.wfu.edu/chemistry/purchase/. Please bookmark this page and remember that you must log on to<br />

it the same way you log on to the Chemical Inventory system (that is, with your username, minus the<br />

@wfu.edu, and your password). If you need to see an example <strong>of</strong> the way to fill out the <strong>for</strong>m, speak to<br />

Melissa Doub in <strong>of</strong>fice # 208, top floor. Purchases <strong>for</strong> over $1000 cannot be placed this way.<br />

B) TYPE IN ALL PERTINENT INFORMATION ON THE DEPARTMENTAL ORDER FORM<br />

� Starting at the top <strong>of</strong> the <strong>for</strong>m, type in the Date you wish to place the order over the phone.<br />

� Fill in the “Ship To” field with your Research pr<strong>of</strong>essor‟s name, or with a combination <strong>of</strong> your<br />

pr<strong>of</strong>essor‟s name and your own. For example:<br />

1. Dr. Albus Dumbledore, or<br />

2. Dr. Albus Dumbledore/Harry Potter, or, <strong>for</strong> that matter, Dr. Albus Dumbledore/Potter is<br />

fine. But please! Always include your research Pr<strong>of</strong>essor’s name in the shipping<br />

address. Do not address Chemistry Department related purchases to your name alone!!!<br />

Graduate students are sometimes difficult to track down and find in the building!<br />

� Fill in the “Bill to Account” field. This is the pr<strong>of</strong>essor's grant number or funding description,<br />

from which said purchase will be paid. The faculty member authorizing the purchase will know<br />

this number or abbreviation/acronym. His/her permission is required <strong>for</strong> obtaining this<br />

in<strong>for</strong>mation. If this is a departmental purchase <strong>for</strong> a teaching lab, you must fill out this field, with,<br />

say, Dept, and scroll to “yes” in the “Departmental Charge?” field.<br />

� Fill out the “Purchase Order To” field with the name <strong>of</strong> the company – its Vendor Address is<br />

optional.<br />

� Fill in the “Company’s WFU Account No.” Most firms accepting large volume business from our<br />

department will have their own particular "account number" <strong>for</strong> all University‟s that buy from<br />

them, in order to expedite their invoicing (billing) records. Fisher Scientific Company's account<br />

number <strong>for</strong> us is 861448-01, <strong>for</strong> example. For Sigma-Aldrich Chemical Company it is 49464319<br />

(unless you have an individual PIN number). SEE THE VENDER’S LIST OF OTHER<br />

COMPANY ACCOUNT NUMBERS AT THE END OF THIS SECTION. If you know this<br />

number, please include it, since the company will usually ask <strong>for</strong> it when you are calling in an<br />

order. If you don't, the lab manager will add it, if you wish him to place the order. Sometimes the<br />

company already knows what this number is if you‟re calling from Wake University Chemistry<br />

Department. Discounts <strong>of</strong>fered to us will be recognized by the company with use <strong>of</strong> this number.<br />

� Fill in the company's telephone number (toll-free, if available)<br />

� You won‟t need to add the Salesperson Name in most cases.<br />

� <strong>Use</strong> the Notes field to add any important in<strong>for</strong>mation to the <strong>for</strong>m regarding the order that you may<br />

wish to refer to later, such as items on back-order, special shipping instructions, original catalog<br />

numbers no longer available <strong>for</strong> items that have received newer catalog numbers, substitute<br />

descriptions, extra discount pricing in<strong>for</strong>mation, technical in<strong>for</strong>mation regarding possible<br />

instrumental problems, questions regarding purity <strong>of</strong> chemicals, etc.<br />

� You can only order up to 20 different catalog items per order. Start out with item # 1. Supply the<br />

Cat. No. (catalog Number) <strong>for</strong> the item. Write in the QTY (<strong>for</strong> quantity <strong>of</strong> items – That is, the<br />

number <strong>of</strong> bottles, or the number <strong>of</strong> packs, or the number <strong>of</strong> cases <strong>of</strong> the item). Lastly, type in the<br />

Description <strong>of</strong> the item. If it is a chemical, type in the amount, unit, and chemical name. For<br />

example, type in 100 grams <strong>of</strong> 4-Nitroaniline, or one case <strong>of</strong> 6 X 500 grams <strong>of</strong> Sodium hydroxide,<br />

etc. If you are ordering anything other than chemicals, type in its description and how much <strong>of</strong> it<br />

you want. For example, type in “3 cases <strong>of</strong> test tubes”, or “5 packs <strong>of</strong> nitrile gloves”, etc.<br />

173


� When you have listed everything you wish to order, call the company, tell them you wish to place<br />

an order, give them the Company’s WFU Account No. if they ask <strong>for</strong> it, tell them to whose<br />

attention the order should be shipped, and make sure they have this exact shipping address:<br />

�<br />

Dr. Albus Dumbledore /Harry Potter or better, simply Dr. Albus Dumbledore<br />

Wake Forest University<br />

Chemistry Department, Salem Hall<br />

Winston-Salem, NC 27109-7486<br />

Fill in the Total Cost field, including tax. At some point during this call to the company<br />

you will be asked to supply the Purchase Order Number <strong>for</strong> this order. In<strong>for</strong>m them that with this<br />

new ordering system, you cannot give them that number until you know how much everything<br />

costs. Now, Click the Submit PO Request box at the bottom <strong>of</strong> the page. (The Reset Form field<br />

merely sets everything back to a blank <strong>for</strong>m if you make mistakes and wish to start over.) After<br />

you click Submit PO Request while you still have the company on the phone, the page you have<br />

so patiently filled out will magically disappear and be replaced with your Chemistry Purchase<br />

Order Detail page, which repeats all the relevant in<strong>for</strong>mation you‟ve typed in, as well as finally<br />

giving you your Purchase Order Number <strong>for</strong> this particular order. Now repeat the Purchase<br />

Order number to the individual on the phone taking your order. You would be well advised at this<br />

point to print the Detail Page out as a hardcopy [Or you can store it as a PDF file on your<br />

computer - Press “file”, click on “Print”, and choose “Adobe PDF” on the printer scroll down list<br />

and store it under My Documents in a file <strong>for</strong> all such Purchase Order copies.] The words<br />

“PLEASE PRINT FOR YOUR RECORDS” will appear at the bottom <strong>of</strong> the Detail Page<br />

anyway, so you may as well keep a copy. If you receive the wrong items from the company, the<br />

Lab Manager will not be able to return them without seeing the in<strong>for</strong>mation on this page. Lastly,<br />

after placing an order with you, the company will usually give you yet another number which you<br />

need to handwrite on this hardcopy, preferably in the section marked “Comments:” at the bottom<br />

<strong>of</strong> the Chemistry Purchase Order Detail page - This is the Confirmation or Reference number.<br />

This is a number which is particularly useful to the company and the lab manager in keeping track<br />

<strong>of</strong> the shipment <strong>of</strong> this order. Returns almost invariably require use <strong>of</strong> this number. If you store<br />

the Chemistry Purchase Order Detail page as a PDF file, you must somehow type in this number<br />

on the PDF file when you‟re finished with everything.<br />

C) Fisher Scientific Company orders<br />

Certain companies are given "blanket purchase order numbers", meaning one P.O. # <strong>for</strong><br />

all orders placed with that company, due to large volume Chemistry Department purchases from<br />

them.<br />

In particular, Fisher Scientific company's blanket P.O.# is C-23837. There is no need to<br />

use the above mentioned standard Departmental Purchase Order Form, as the P.O.# C-23837 was<br />

used long ago. The only record necessary <strong>for</strong> a particular Fisher order is your completed<br />

REQUEST TO ORDER FROM FISHER SCIENTIFIC <strong>for</strong>m, copies <strong>of</strong> which are kept in the<br />

Chemistry Department <strong>of</strong>fice in room 110A or with the Lab Manager. Call in Fisher orders<br />

yourself or request that the laboratory manager place the call. In any case, make sure that the<br />

completed handwritten REQUEST TO ORDER FROM FISHER SCIENTIFIC <strong>for</strong>m ends up<br />

with the laboratory manager, on his desk or in his mailbox. If the order is over $1000 you must<br />

give the ordering in<strong>for</strong>mation to Ms. Melissa Doub in the <strong>for</strong>m <strong>of</strong> a faxed quote from Fisher, who<br />

will issue the quote to the University‟s Purchasing Department in Reynolda Hall. They will call in<br />

the order to and assign their own Purchase Order number to it.<br />

One order is distinguished from another with descriptor numbers added to C-23837, as<br />

follows:<br />

C23837MW-STARTUP-0922<br />

C23837DK-512030-0922<br />

C23837ST-698020-0922<br />

List the Fisher P.O.# (C-23837), the initials <strong>of</strong> the pr<strong>of</strong>essor's name (i.e., MW <strong>for</strong> Dr.<br />

Mark Welker, DK <strong>for</strong> Dr. Dilip Kondepudi, ST <strong>for</strong> Dr. Susan Tobey), the last six digits <strong>of</strong> the<br />

174


faculty members personal "Pr<strong>of</strong>essor‟s Billing Account #", or a brief description <strong>of</strong> the account if<br />

it has no number (i.e., STARTUP funds, NSF account, NIH grant, etc.), and the date (0922).<br />

Fisher <strong>of</strong>fers a larger discount rate than most other companies. Catalog numbers <strong>for</strong> items<br />

made by Kontes, Corning, Brinkman, Buchi, etc., are cross-referenced to Fisher catalog numbers by<br />

secretaries taking your call. Items made by other companies and purchased through Fisher are usually less<br />

expensive. Also, there is no transportation charge <strong>for</strong> Fisher deliveries, but there is a $19 hazardous<br />

chemical fee <strong>for</strong> hazardous chemical shipments. Acros is a part <strong>of</strong> Fisher Scientific Co. (prefix all Acros<br />

chemical catalog #s on a Fisher order with “AC”). Acros competes well with Sigma-Aldrich cost-wise, and<br />

their selection <strong>of</strong> chemicals is just as extensive.<br />

When any shipment arrives, it will be on the receiving table in the loading dock area next to the full<br />

compressed gas cylinders. The laboratory manager will normally deliver packages to each pr<strong>of</strong>essor. Have<br />

an area within your lab designated as the "Receiving Area" bench-top space or desk or floor, if need be.<br />

You may take your shipments up to your lab yourself, if you wish, but you must remove the packing slips<br />

and place them in the packing slip wire basket, next to the receiving table. These are used as shipment<br />

verification receipts. You can keep them in a separate place or drawer within your lab, if you wish. If your<br />

Purchase Order Form in<strong>for</strong>mation was correct, there will be no discrepancies in shipping addresses or<br />

invoicing (billing).<br />

D) National Welders, Inc., a local company which supplies most <strong>of</strong> the Chemistry Department's<br />

compressed gases, has been given a “blanket” purchase order # C23934.<br />

All purchases from this company are given the same number. You don‟t need a Purchase<br />

Order <strong>for</strong>m, as all orders with this local company are verbal. There is no need to distinguish one<br />

purchase from another, as all invoices are well maintained and sent to us by the company. Call<br />

them at 744-0010 and include Salem Hall in the shipping address. They know the rest. Just make<br />

sure they send the cylinders to Wake Forest University, Chemistry Department, Salem Hall,<br />

Reynolda campus.<br />

Commonly ordered large compressed gases are described with cubic-foot (cf) sizes rather<br />

than catalog numbers as follows. <strong>Use</strong> these descriptions when ordering over the phone:<br />

� Argon, size 336<br />

� Argon, High Purity 336<br />

� 10% Hydrogen in Argon<br />

� Air (Industrial grade), size 300<br />

� Helium, size 219<br />

� Hydrogen, size 191<br />

� Nitrogen, size 304<br />

� Oxygen, size 282<br />

� Acetylene, size 140<br />

� Carbon dioxide, size 50<br />

� Carbon monoxide size 200<br />

� Liquid Nitrogen LS 160 liter size (<strong>for</strong> general departmental use, located in the loading dock,<br />

usually cast iron “magnetic” or sometimes stainless steel “non-magnetic” tank<br />

You can also get several <strong>of</strong> the gases above as “Ultra High Purity” (usually Helium) or<br />

“oxygen-Free” (usually Nitrogen) grades.<br />

Returnable, large-size cylinders <strong>of</strong> common gases are normally charged to the<br />

departmental account. Specialized equipment (regulators, lecture bottles, unusual special gas<br />

mixtures etc.) will be charged to individual research accounts. This company will also repair all<br />

types <strong>of</strong> regulators. I think it‟s better to get regulators <strong>for</strong> common gases from Fisher (get catalog<br />

series # 10-572). They are less expensive and already have the needle valves attached.<br />

You should have a Specialty Gases and Equipment catalog from National Welders kept in your<br />

laboratory. Also, keep a copy <strong>of</strong> the Matheson Gas Products Catalog, which lists lecture bottles <strong>of</strong><br />

175


specialty gases sold by Sunox, a local company, 996-3832. If lecture bottles are purchased<br />

from National Welders, they can be returned when empty to them rather than taken out<br />

with garbage to a landfill. Lecture bottles <strong>of</strong> unusual gases can be purchase from National<br />

Welders, <strong>care</strong> <strong>of</strong> Mr. David Young, phone # 1-800-866-4422, ext. 3602, cell phone # 336-817-<br />

5070. I prefer that you purchase lecture bottles from National Welders.<br />

The following liquid gases are usually purchased by Dr. Marcus Wright <strong>for</strong> use in the NMR room,<br />

from National welders, unless otherwise noted:<br />

� Liquid Helium 100 liters (<strong>for</strong> the NMR room, room # 12A)<br />

� Liquid Nitrogen LNS 160, PGS45, or XL50, all High Pressure Stainless Steel “non-magnetic”<br />

tanks <strong>for</strong> the Mass Spectrometer in the NMR room.<br />

� Liquid Nitrogen LNS 160, PGS45, or XL50, all Low Pressure Stainless Steel “non-magnetic”<br />

tanks <strong>for</strong> the NMR.<br />

The following liquid Argon gas tank is purchased by Dr. Brad Jones, <strong>for</strong> use in Lab room # 118,<br />

from National welders, perhaps once every 2 months:<br />

� Liquid Argon LARS50<br />

The following liquid gas is purchased from Magnetic Resources company maybe once a year as a<br />

backup supplier, in case National Welders runs out <strong>of</strong> current amount needed:<br />

� Liquid Helium size 100, Stainless Steel “non-magnetic”, from Magnetic Resources, phone<br />

800-443-5486, <strong>for</strong> the NMR room<br />

Lecture bottles bought from Sigma-Aldrich Chemical Co. can be returned to them via ROADWAY<br />

CO. shipment. Sigma-Aldrich has a standard <strong>for</strong>m to attach to the package. Follow the procedure<br />

they will mail you when you call them at 1-800-558-9160.<br />

Matheson lecture bottle gases can also be purchased by calling Matheson directly in Georgia at<br />

770-961-7891. Returning these empty lecture bottles is relatively easy. See the appropriate<br />

section in the chapter entitled “Procedure For Handling Hazardous Chemical Waste”, #7, “Spent<br />

Lecture Bottle Compressed Gas Cylinders”.<br />

Please note that a good local source <strong>for</strong> copper, stainless steel and aluminum tubing <strong>of</strong> various<br />

sizes is as follows: Ferguson Enterprises, Inc., 7905 North Point Blvd., Winston-Salem, NC phone<br />

# 759-0253.<br />

In particular, standard size copper tubing (l/8 in. outside diameter, 0.028 in. inside diameter),<br />

standard size stainless steel tubing (again, 1/8 in. O.D. and 0.028 in.I.D.) and aluminum tubing can<br />

be ordered here with prompt delivery. We have an account with them (WFU Acct. # 2350).<br />

Fisher also sells copper tubing and Swagelok fittings. The only other source <strong>for</strong> Swagelok fittings<br />

is Charlotte Valve and Fitting Co., 704-598-7040, WFU Acct. # WFU001.<br />

Process and Control Equipment company in Charlotte, NC, phone # 704-334-0881, is a good<br />

source <strong>for</strong> Imperial Eastman polyethylene tubing (Poly-Flow tubing, catalog # 22-P, <strong>for</strong> 1/8th inch O.D.,<br />

and 44-P, <strong>for</strong> 1/4th inch O.D., <strong>of</strong> various colors). This tubing will withstand a maximum working pressure<br />

<strong>of</strong> 125 psi <strong>for</strong> 1/8th inch tubing and 100 psi <strong>for</strong> 1/4th inch tubing.<br />

176


Vendor’s List <strong>for</strong> Wake Forest University Chemistry Department<br />

COMPANY NAME WFU ACCOUNT # TELEPHONE # DISCOUNT<br />

AAPER ALCOHOL & CHEMICAL CO. 020253 800-456-1017<br />

ACE GLASS 36230231 800-626-5381 YES<br />

ACE HARDWARE 768-3886<br />

ACROS ORGANICS (C/O FISHER) 861448-01 800-766-7000 YES<br />

Advanced Appliance Service 767-1435<br />

AETC 362140 201-347-7111<br />

AIR PRODUCTS 71702 299-1361<br />

ALFA AESAR (JOHNSON MATTHEY) 56046733 800-343-0660<br />

AMERICAN CHEMICAL SOCIETY 361266 800-227-5558<br />

American Environmental Services, Inc 704-588-1070<br />

Amersham Pharmacia Biotech 41904 800-526-3593<br />

ANDATACO 113200 619-453-9191<br />

ANDERS SERV CENTER (VCR REPAIR) 869-1292<br />

Agilent Technologies 47157 800-227-9770 yes<br />

ANIXTER 829155 FAX: 919-292-2694<br />

APPLIED SPECTROSCOPY, SOCIETY FOR 913-843-1235<br />

APPLIED WEIGHT TECHNOLOGY 336-260-2988<br />

ATLANTIC MICROLAB 404-242-0084<br />

BARNSTEAD/LABORATORY DEVICES 43707000 800-447-6722<br />

BIORAD 036423-002 800-424-6723<br />

BODMAN 309-300 800-241-8774 YES<br />

BRINKMAN 755265-3 800-645-3050<br />

Brucker-AXS 800-234-XRAY<br />

CALBIOCHEM 113032 619-450-9600<br />

Brucker NMR 978-667-9580<br />

CALICO INDUSTRIES, INC. 511370 800-638-0828<br />

Calumet Photo 888-367-2781<br />

CAMBRIDGE ISOTOPE 271090 800-322-1174<br />

CAMERA CORNER WAK480 800-868-2462<br />

CAPITOL VACUUM 800-237-3933<br />

CARGO-PACK 919-554-3844<br />

CAROLABS 203-393-3029<br />

CAROLINA BALANCE WAK2 996-3631 YES<br />

CAROLINA BIOLOGICAL SUPPLY CO. 4440700 800-632-1231<br />

CENTRAL SCIENTIFIC CO 800-262-3626<br />

CERAMPTEC 759-4656<br />

Charles Supper Company 800-323-9645<br />

CHARLOTTE VALVE & FITTING CO. WFU001 704-598-7040<br />

CHEM CENTRAL (ACETONE DRUMS) 800-755-8879 YES<br />

CHEMGLASS WAK001 800-843-1794 YES<br />

COLE-PARMER 381234-01 800-323-4340<br />

CONSOLIDATED PLASTICS (RUBBER MAID) 97744-893650 800-362-1000<br />

CORPORATE EXPRESS (HINKLES) 770-1500<br />

CPI 3810 800-878-7654<br />

CRESENT CHEMICAL CO. 800-645-3412<br />

177


CURTIN MATHESON SCI. CO. 23-008-409-40 800-241-7670 YES<br />

Cynmar Corporation 22805 800-223-3517 yes<br />

DEGUSSA 001947 908-561-1100<br />

DILLON SUPPLY CO. WS70528 723-2961<br />

Eagle Instrument Services, Inc., Repair <strong>of</strong> Vacuum Pumps 1-888-433-0890<br />

EASTMAN KODAK (OWNED BY FISHER) 1119502 800-766-7000<br />

EDMUND SCIENTIFIC CO. 325522 609-573-6250 YES<br />

E G Forrest 723-9151<br />

EG&G PARK 2WAKFORE1 609-530-1000<br />

ESA, Inc, 22 Alpha Road, Chelms<strong>for</strong>d, MA Zip 01824-4171 978-250-7090<br />

EXCELLINK WAKE 408-295-9000<br />

FARALLON COMPUTING 1232900 510-596-9359<br />

FARCHAN LABORATORIES, INC. 2310001 904-378-5864<br />

FERGUSON ENTERPRISES, INC. 2350 704-598-7040<br />

Fishel Steel Co., Inc. Winston-Salem 788-2880<br />

FISHER SAFETY 861448-01 800-772-6733<br />

FISHER SCIENTIFIC 861448-01 800-766-7000 YES<br />

FISHER, ED MATERIALS DIV. (EMD) 420356-001 800-955-1177<br />

FLINN SCIENTIFIC INC 2710902 800-452-1261<br />

FLUKA (C/O SIGMA-ALDRICH) 49464319 800-558-9160<br />

EG FORREST, 1023 N Chestnut St none 723-9151<br />

FREY 1578608 800-225-3739<br />

Frontier Scientific, Inc 1328 435-753-1901<br />

GALBRAITH LABS 615-546-1335<br />

GATEWAY WAKEFOR1/000 605-232-2000<br />

GENICOM 703-949-1000<br />

G. J. CHEMICAL CO., INC. Cell 910-540-4588 973-968-3348<br />

GFS CHEMICALS 800-858-9682<br />

GLOBAL COMPUTER SUPPLIES 49219708226 800-845-6225<br />

GOLDEN SOFTWARE 303-279-1021<br />

GOW-MAC INSTRUMENT CO. 610-954-9000<br />

GRAINGER(Login chemdept, password 7486) 837412493 759-2000<br />

GRAPHIC CONTROLS 60227656 800-669-1535<br />

GRAYBAR ELECTRIC CO<br />

GRAY SUPPLY CO. 206492 800-238-2244<br />

HALOCARBON PRODUCTS CORP. 1278 201-262-8899<br />

HEWLETT PACKARD 311129252 1-800-888-9909<br />

Hankison International 724-745-1555<br />

HOLOX (FOR DRY ICE) J7134 996-3832<br />

ICN CHEMICALS (INCLUDES K&K LABS) 122143 800-854-0530<br />

INGOLD ELECTRODES INC. (MEC-TRIC) 10704-376 704-376-8555<br />

INMAC (DAVE BARKIN OUR REP 2006) 912028 800-547-5444<br />

INSTS FOR RES AND INDUSTRY (I R) 215-379-3333<br />

International Crystal Labs 1-973-478-8944<br />

JANSEN CHIMICA (SPECTRUM CHEM) WAK030 800-772-8786<br />

JENSON 800-426-1194<br />

JOYCE BROTHERS 6307 765-6927<br />

KEWAUNEE SCIENTIFIC CORP 1-704-873-7202<br />

178


KODAK LABORATORY CHEMICALS BUY FR FISHER<br />

KONTES 66001 800-223-7150<br />

LABELMASTER key Code GA1100 0157623 800-621-5808<br />

LAB GLASS 250150 800-522-7123 YES<br />

LAB SAFETY SUPPLY, INC. 731096 800-356-0783<br />

LAB TECH, INC 11940 770-422-3305<br />

LANCASTER SYNTHESIS, INC. WFU1 800-238-2324<br />

LEEMAN LABS 508-454-4442<br />

LIEBERT CORPORATION 800-543-2378<br />

LONG COMMUNICATIONS 725-2306<br />

MACHINE & WELDING SUPPLY CO. 723-9651<br />

MATHESON GASES 215-648-4007<br />

MAC WAREHOUSE 3813396 OR<br />

9299215 (DK)<br />

MCARTHY SCIENTIFIC CO. 760-731-6570<br />

MELLES GRIOT 11899 800-835-2626<br />

METTLER 19330 800-638-8537<br />

MIDWEST CENTER FOR MASS SPEC. 402-472-3507<br />

MILLIPORE CORP/WATERS 5140 97437 800-645-5476<br />

MISCO 1080104 800-876-4726<br />

MONOMER POLYMER (DAJAC LABS) 215-364-6111<br />

NATIONAL CABINET LOCK 864-297-6655<br />

NATIONAL WELDERS SUPPLY CO. 1491355 744-0010 YES<br />

NEWARK ELECTRONICS (NITA MOORE) 82590 292-7240 YES<br />

New England Biolabs C8495 899-632-5227<br />

NORELL, INC. NC WFU 800-222-0036<br />

OCEAN OPTICS 415 813-733-2447<br />

OMEGA ENGINEERING, INC. 397970 1-800-826-6342<br />

OMNI INSTRUMENTS (CHRIS DEATON) 228-388-9211<br />

ONYX ENVIRONMENTAL SERVICES 1-800-626-1461<br />

OTIS ELEVATOR 996-5030<br />

PARR INSTRUMENT CO. 13018 309-762-7716<br />

Pharmacia Biotech, Amersham 41904 800-526-3593<br />

Picometrics, France,701Chemin,d’Embeoune 31450-Montlaur 33(0)5.61.28.56.88<br />

PINE INSTRUMENT COMPANY WAFU 412-458-6391<br />

PCR, INC. 393076 800-331-6313<br />

PERKIN ELMER 100020571 800-762-4002, opt 1, 2<br />

PFALTZ AND BAUER UW0001 800-225-5172<br />

Physician Sales and service (PSS) 393075 800-874-2240, ext.3905<br />

PROCESS CONTROL EQUIPMENT 38400 704-334-0881<br />

POLYMICRO TECHNOLOGIES, INC. WAK-0002 602-375-4100<br />

POLY SOFTWARE NITERNAT'L 801-485-0466<br />

PUBLIC SCIENTIFIC GLASS 924-2183<br />

Qiagen 42840 800-426-8157<br />

QUARK ENTERPRISES, INC. WAKEF 800-955-0376<br />

RADIO SHACK (PINE RIDGE PLAZA) C00003223061424 722-0903<br />

REAGENTS INC. (ACETONE DRUMS) 504826 800-732-8484 YES<br />

RELIANCE GLASS WAKE FOREST U 800-323-3334<br />

179


RESEARCH INFORMATION SYSTEMS 619-438-5526<br />

RESEARCH SYSTEMS, INC. (RSI) 303-786-8900<br />

ROADWAY EXPRESS 993-4811<br />

SAFE LAB/NOW BH SCIENTIFIC GLASS 233014 800-932-7120<br />

SAFETY SUPPLY AMERICA 861448-01 800-772-6733<br />

SCHWEIZERHALL 963479 800-243-6564<br />

SCIENTIFIC PRODUCTS (BAXTER) 327607519002 800-234-5227<br />

SIGMA-ALDRICH 20385 800-558-9160<br />

Silicycle 877-745-4292<br />

SMALL PARTS INC. 27109WAF 800-423-9009<br />

SOUTHEASTERN LAB APPARATUS, INC. 100740 803-279-7668<br />

SPECTRUM CHEM (JANSSEN CHIMICA) WAK030 800-772-8786<br />

STN 0896924A 800-753-4CAS<br />

Stratagene 1174 800-424-5444<br />

STREM CHEMICALS, INC. 4-00905 800-647-8736<br />

Sunnyside Ice(dry Ice, if Iinde Gas quits selling<br />

it)<br />

723-5161<br />

SUPELCO 49464319 800-247-6628<br />

TCI AMERICA WAK22 800-423-8616<br />

TECH DATA 964225 800-237-8931<br />

TEKTRONIX, INC. 34111014 800-835-9433<br />

Thermo Electron Scientific Instruments Corp 800-642-6538<br />

THOMAS SCIENTIFIC 337952000 800-345-2100 YES<br />

Thomasville City Ice (picnic Ice in bulk) 472-7426<br />

TopBulb 430635 800-238-2244<br />

Topogen 800-867-6436<br />

TRIMETRIX WFU02 206-527-1801<br />

UNITED CHEMICAL TECHNOLOGIES WAWNB2 800-541-0559<br />

VAN WATERS AND ROGERS (VWR) 2038462 800-932-5000<br />

VESUVIUS MCDANIEL 2574 412-843-8300<br />

VIKING OFFICE PRODUCTS 377193 800-421-1222<br />

WATERS 5140 97437 800-252-4752<br />

WELCH VACUUM TECHNOLOGIES 847-676-8819 or 847-676-8800, ext. 8819<br />

WILMAD GLASS CO., INC. 250150 800-220-5171<br />

180


MISCELLANEOUS INFORMATION<br />

Acros is a part <strong>of</strong> Fisher Scientific Co. (prefix all Acros chemical catalog #s on a Fisher order with “AC”)<br />

Spectrum Chemical Mfg. Corp. is now part <strong>of</strong> Jansen Chimica.<br />

K & K Laboratories is now a part <strong>of</strong> ICN Chemicals.<br />

Schweizerhall and Chemalog now sell chemicals only in bulk quantities.<br />

Mallinckrodt and J. T. Baker sells their chemicals through Scientific Products until recently called Baxter or<br />

VWR (Van Waters and Rogers). VWR has merged with Scientific Products and is now called VWR<br />

Scientific Products.<br />

Baxter Chemicals is now Scientific Products.<br />

Kodak Laboratory Chemicals was bought out by Fisher Scientific Co. Buy Kodak Chemicals, using the<br />

Kodak catalog number from Fisher at 1-800-766-7000, through the ARCOS Organics catalog. ACROS<br />

sells addition chemicals as well, and all are sold at a 10% discount.<br />

Kimble Glassware is sold through its retail dealers, such as Fisher, Scientific Products (Baxter), etc.<br />

Curtin Matheson Sci. Co. has been bought out by Fisher.<br />

181


VI. Purchasing Procedure <strong>for</strong> DEA Controlled Substances<br />

Chemical purchases by faculty will occasionally result in chemical manufacture mailings warning<br />

<strong>of</strong> Drug En<strong>for</strong>cement Administration (or DEA) regulations which apply to the purchase <strong>of</strong> certain "drug<br />

precursors" or "essential chemicals" involved in criminal preparation <strong>of</strong> illicit drugs. The pertinent section<br />

<strong>of</strong> the Code <strong>of</strong> Federal Regulations is as follows: 21 CFR 1310.05 and 1310.06. The listing <strong>of</strong> such<br />

chemicals occurs in section 21 CFR 1310.02, which can be accessed at:<br />

http://www.access.gpo.gov/nara/cfr/waisidx_00/21cfr1310_00.html<br />

According to Mike Callan and Brian Reese <strong>of</strong> the Greensboro branch <strong>of</strong> the DEA, the university,<br />

and the chemistry department in particular, do not "manufacture, distribute, export, or import" the chemicals<br />

listed above in 21 CFR 1310.02. There<strong>for</strong>e, we are not subject to reporting requirements. We should,<br />

however, report any suspicious activity regarding these chemicals to the Greensboro DEA <strong>of</strong>fice (phone #<br />

547-4219) and keep them in a secure research, teaching lab, or storage room.<br />

Aldrich Chemical Co. requires annual signature updates from the Chemical Department <strong>for</strong> their<br />

DEA records. Since all chemicals in Salem Hall are purchased only via Faculty signatures on Purchase<br />

Order Forms, chemicals cannot possibly be bought by anyone else.<br />

The list <strong>of</strong> present authorized buyers <strong>of</strong> chemicals in Salem Hall is listed here:<br />

Alexander, Rebecca<br />

Bierbach, Ulrich, Pr<strong>of</strong>.<br />

Brown, Bernard, Pr<strong>of</strong>.<br />

Buchmueller, Karen, Pr<strong>of</strong>.<br />

Colyer, Christa, Pr<strong>of</strong>.<br />

Day, Cynthia, Pr<strong>of</strong>.<br />

Doub, Melissa, Chemistry Department Administrative Assistant<br />

Glisen-King, Angela, Pr<strong>of</strong>.<br />

Hinze, Willie L., Pr<strong>of</strong>.<br />

Jones, Bradley, Pr<strong>of</strong>.<br />

Jones, Paul, Pr<strong>of</strong>.<br />

King, Bruce, Pr<strong>of</strong>.<br />

Kondepudi, Dilip, Pr<strong>of</strong>.<br />

Lachgar, Abdessadek, Pr<strong>of</strong>.<br />

N<strong>of</strong>tle, Ronald, Pr<strong>of</strong>.<br />

Sw<strong>of</strong><strong>for</strong>d, Robert, Pr<strong>of</strong>.<br />

Tobey, Suzanne, Pr<strong>of</strong>.<br />

Thompson, Michael, Laboratory Manager<br />

Welker, Mark, Pr<strong>of</strong>.<br />

Welder, Cathy, Pr<strong>of</strong>.<br />

Wright, Marcus, Pr<strong>of</strong>.<br />

182


VII. Alcohol Dispensing Procedure<br />

Pure Ethyl alcohol is stored in two sealed and locked areas in Salem Hall. The dispensing area is<br />

the solvent room, #20. When you need pint size bottles <strong>of</strong> 200 pro<strong>of</strong> or 5 gallon containers <strong>of</strong> 190 pro<strong>of</strong><br />

(95%) ethyl alcohol <strong>for</strong> your research or teaching laboratory, please obtain them from that room.<br />

A. Alcohol <strong>Use</strong> Logbook<br />

When removing ethyl alcohol, please enter the proper in<strong>for</strong>mation in the “Alcohol <strong>Use</strong> Logbook”,<br />

which is kept permanently in that room on a shelf just above the alcohol. You must indicate the Date the<br />

alcohol was taken, the amount (in pints <strong>of</strong> 200 pro<strong>of</strong> or gallons <strong>of</strong> 190 pro<strong>of</strong>), the alcohol purity (200<br />

pro<strong>of</strong> /100% or 190 pro<strong>of</strong> / 95%), and the pr<strong>of</strong>essor name under whose authority you are dispensing alcohol<br />

or the teaching lab course number which requires the alcohol.<br />

VIII. OSHA/EPA Inspection Procedure <strong>for</strong> Salem Hall<br />

The following procedure, provided by the Bowman Gray School <strong>of</strong> Medicine Environmental<br />

Health Office, will serve as our temporary policy <strong>for</strong> Chemistry Department OSHA/EPA inspections. A<br />

more detailed listing <strong>of</strong> recommendations is kept on the next page <strong>of</strong> the hardcopy <strong>of</strong> this manual kept in the<br />

stockroom, room # 110.<br />

Call Mr. Scott Frazier [WFU Assistant Environmental Health and Safety (EHS) Director] (phone #<br />

4329 or 4224) and alert him to the need <strong>for</strong> attending the inspection. Ask him to:<br />

a) Bring a loaded camera and tape recorder, if available.<br />

b) Take the inspector only where he/she wishes to go, until further notice from the Chemistry<br />

Department laboratory manager or Faculty member.<br />

c) Call Ms. Donna Hamilton <strong>of</strong> the Reynolda Campus Legal Dept. (phone # 5967) or the legal<br />

Dept. itself (phone # 6100).<br />

d) Note the location <strong>of</strong> your Chemical Hygiene Plan, in your lab or on your computer.<br />

e) Follow the Procedure listed on the next page.<br />

f) Recognize that OSHA records <strong>for</strong> Salem Hall are kept in the chemistry stockroom file cabinet,<br />

top file drawer. Keys to this cabinet are kept in the chemistry <strong>of</strong>fice #208 with Mrs. Melissa Doub<br />

(Administrative Assistant, phone # 5325), with Mr. Scott Frazier [WFU Assistant Environmental<br />

Health and Safety (EHS) Director], phone # 4329 or 4224) and with Michael Thompson ( lab<br />

manager <strong>of</strong> Salem Hall, work phone # 5324, home phone # 896-8615).<br />

A good source <strong>of</strong> in<strong>for</strong>mation in the event Mr. Frazier is not available is Michelle Adkins (WFU<br />

Director <strong>of</strong> Environmental Health and Safety), phone # 5385 (cell 480-8480), or Mr. Frazier‟s equivalent on<br />

the Hawthorne BGSM campus, Mr. Dave Brown, BGSM Director <strong>of</strong> Environmental Health and Safety,<br />

phone # 716-9375, pager # 806-7921. (Here is more specific contact in<strong>for</strong>mation <strong>for</strong> Michelle Adkins,<br />

CHMM, Director <strong>of</strong> Environmental Health and Safety, adkinsmm@wfu.edu, phone: 336-758-5385,<br />

cell: 336-480-8480, fax: 336-758-3088).<br />

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IX. Chemical Inventories<br />

A. Inventory <strong>of</strong> All Chemicals and MSDS Sheets in the Chemistry<br />

Department<br />

All incoming MSDS sheets <strong>for</strong> each and every chemical purchased <strong>for</strong> the Chemistry Department<br />

are kept in a central area <strong>of</strong> the building in a set <strong>of</strong> orange-red binder notebooks. They are mailed from the<br />

manufacturer <strong>of</strong> the chemical to Salem Hall.<br />

As chemicals are unpacked in the Dockyard area, the packing slips are placed in a basket on the<br />

wall next to the receiving table. The chemicals are dated in ink on the bottle label and taken to the<br />

particular lab in the building where it is to be used, after entering the chemical and its MSDS sheet into the<br />

on-line chemical inventory. The MSDS sheets are alphabetically arranged in the online inventory system<br />

and a hardcopy <strong>of</strong> the MSDS inventory is kept in a black notebook near the actual the actual MSDS sheets.<br />

These MSDS sheets are accessible 24 hours a day. The inventory web site is:<br />

http://www.wfu.edu/chem/cheminventory/index.html<br />

Presently, designated storage areas are assigned in each laboratory <strong>for</strong> storage <strong>of</strong> carcinogens and<br />

teratogens/mutagens. Chemicals with a high degree <strong>of</strong> acute toxicity will be given an HMIS/NFPA acute<br />

toxicity rating <strong>of</strong> 3 or 4 on the MSDS sheet by the chemical‟s manufacturer. Also “Select carcinogens” are<br />

identified from manufacturer‟s MSDS data. There is at present only one universally acknowledged list <strong>of</strong><br />

known human teratogens. It is contained on page XXV <strong>of</strong> Shepard, Thomas H.,Catalog <strong>of</strong> Teratogenic<br />

Agents, 8th edition, The Johns Hopkins University Press, Baltimore, MD: 1995. See<br />

http://depts.washington.edu/~terisweb/teris/<br />

They are listed below. Most <strong>of</strong> them are hormones or drugs:<br />

CHEMICAL NAME CAS # CHEMICAL NAME CAS #<br />

Aminopterin 54-62-6 Methimazole 60-56-0<br />

Androgenic hormones Methylaminopterin<br />

Busulfan 55-98-1 Methylene blue<br />

Captopril 62571-86-2 Organic mercury 7439-97-6<br />

Carbamazepine 298-46-4 Penicillamine 52-67-5<br />

Chlorobiphenyls Primidone 125-33-7<br />

Cocaine 50-36-2 Quinine 130-95-0<br />

Colchicine 64-86-8 1,3-cis-retinoic acid 4759-48-2<br />

Coumarin anticoagulants Streptomycin 57-92-1<br />

Cyclophosphamide 50-18-0 Tetracycline 60-54-8<br />

Diethylstilbestrol 56-53-1 Tetracycline-7-H3 36051-40-8<br />

Diphenylhydantoin Tetracycline Hydrochloride 64-75-5<br />

Disulfiram 97-77-8 Tetracycline Phosphate 13930-32-0<br />

Enalapril 75847-73-3 Thalidomide 50-35-1<br />

Ergotamine 113-15-5 Toluene abuse 108-88-3<br />

Etretinate Trimethadione<br />

Iodides Valproic acid 99-66-1<br />

Lead 7439-92-1 High Vitamin A 68-26-8<br />

Lithium 7439-93-2<br />

Additional sources <strong>of</strong> possible teratogens or mutagens are listed on page 46 <strong>of</strong> Prudent Practices.<br />

Until a definite, all-inclusive list <strong>of</strong> teratogens or mutagens is published, it shall be the practice <strong>of</strong> the<br />

Chemistry Department to designate such substances in the MSDS inventory based on in<strong>for</strong>mation contained<br />

in the MSDS sheet and so rated in HMIS/NFPA <strong>for</strong>mat as defined previously.<br />

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B. Instructions <strong>for</strong> the <strong>Use</strong> <strong>of</strong> the Online Inventory System<br />

(prepared by Amanda Price and Mike Thompson)<br />

1. Go to: http://www.wfu.edu/chem/cheminventory/index.html<br />

2. Enter the inventory system by clicking on “Online Chemical Inventory Database”.<br />

3. The Home Page <strong>for</strong>mat allows the user to choose from several inventory options.<br />

These include:<br />

a) Entering new chemicals into the inventory <strong>of</strong> a specific<br />

Faculty Group or Undergraduate Lab Class [“Add Inventory” button]<br />

b) Viewing a specific Faculty Group’s entire current inventory, or<br />

Searching <strong>for</strong> a particular chemical in all departmental inventories (including<br />

your own) by chemical name (partially or fully named), CAS number, or the<br />

date it was entered [“Search/Update Inventory” button]. You can also view<br />

the entire inventory <strong>of</strong> the various storerooms (“room 19” <strong>for</strong> departmental<br />

storage, “general” <strong>for</strong> inorganic chemicals in room 103, “Organic” <strong>for</strong> organic<br />

chemicals in room 103, “Inorganic” <strong>for</strong> Advanced Inorganic course # 361 in<br />

room 19, “Indicator” <strong>for</strong> indicators and dyes in a cabinet in room 103, “room<br />

7” <strong>for</strong> the Physical Chemistry lab, “<strong>Solvent</strong>” <strong>for</strong> large solvent and ethanol<br />

containers in departmental storage room # 20), all <strong>of</strong> which are included in<br />

the category <strong>of</strong> Individual Faculty Group Inventory.<br />

You can also search <strong>for</strong> a list <strong>of</strong> all lecture bottles under the chemical<br />

search option in the location field.<br />

c) Searching <strong>for</strong> safety in<strong>for</strong>mation from MSDS sheets, listed by chemical name<br />

or CAS number [“Search MSDS” button]<br />

d) Adding MSDS sheets to the MSDS Inventory [“Add MSDS” button]<br />

It is best to search <strong>for</strong> an individual chemical by CAS number (Chemical Abstract Service<br />

number), which is completely specific <strong>for</strong> a particular chemical, since searching by name will<br />

result in multiple listings <strong>of</strong> any chemical name which contains your chemical as part <strong>of</strong> its<br />

name.<br />

4. Once an option has been chosen, the required in<strong>for</strong>mation must<br />

be entered (username and which inventory) and then submitted [Click the “Submit”<br />

button]. This allows the user to view the requested inventory, specific chemical listing, or<br />

new chemical entry <strong>for</strong>m.<br />

5. Adding a chemical to the inventory:<br />

a) Again, the user must enter a username and choose which Faculty Group or<br />

Undergrad Lab inventory or storage room one wishes to work with.<br />

b) Once this is done and has been submitted, a new screen will appear with an<br />

entry <strong>for</strong>m indicating several empty in<strong>for</strong>mation fields. These include:<br />

1) Chemical name (don’t list “HPLC Grade”, or 98%, etc., unless you<br />

really need to)<br />

2) CAS number (DO NOT USE HYPHENS between numbers)<br />

3) Catalog number<br />

4) Supplier<br />

5) Quantity (how many bottles, containers, etc.?)<br />

6) Size (numerical amount, 25, 500, 1, etc.) and Unit (grams, mL, Kg,<br />

etc.)<br />

7) Location (shelf number, cabinet label, which hood, etc.?)<br />

c) The user must completely fill all fields be<strong>for</strong>e submitting<br />

new in<strong>for</strong>mation into the inventory.<br />

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d) After submitting a new entry, the user can continue to add chemicals to the<br />

same inventory or go back to the Main Menu and select another option. Your<br />

new chemicals will be automatically alphabetized when you have finished<br />

entering them into your inventory and exit the inventory.<br />

6. A hard copy <strong>of</strong> an individual inventory can be obtained by listing an individual Faculty<br />

Group (or individual teaching lab/storeroom) inventory and printing directly from the File<br />

menu.<br />

7. The Lab Manager can obtain a hard copy <strong>of</strong> the MSDS inventory by selecting “Search<br />

MSDS” (<strong>of</strong> a particular Department) on the main page <strong>of</strong> the inventory website and, then,<br />

selecting “Chem” from the drop-down menu on the Search MSDS page. Once the computer<br />

has finished searching <strong>for</strong> all chemicals in that inventory, it will indicate “Total matches<br />

found: xxxx (or a certain number over 1000, at least) - Too many to display here. Click here<br />

to download the file so you can open it in Excel.” Click there to download the file into Excel.<br />

Click on this link and save the file in the Excel folder under <strong>Use</strong>rdata. Replace old/existing<br />

files with the same name when asked to do so while downloading the updated inventory file.<br />

Now the full MSDS inventory can be viewed in Excel <strong>for</strong>mat, and printed if necessary. The<br />

Lab Manager can also get hardcopies <strong>of</strong> any shorter Faculty Group chemical inventory the<br />

same way, when listing any such inventory which happens to be over 1000 entries in size. The<br />

database system apparently cannot list overly large inventories, and they must be downloaded<br />

into an Excel file.<br />

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C. General In<strong>for</strong>mation <strong>for</strong> <strong>Use</strong>rs<br />

(Written by Yue-Ling Wong, Academic Computing Specialist, March 5, 2001)<br />

URL <strong>of</strong> the Online Chemical Inventory Database<br />

http://www.wfu.edu/chem/cheminventory<br />

/db/<br />

<strong>Use</strong> <strong>of</strong> the Databases<br />

1. Any WFU user who has a valid username and password can search both the inventory and<br />

MSDS databases. There<strong>for</strong>e, when you access the web pages <strong>of</strong> the database, it will first prompt<br />

you <strong>for</strong> username and password. Enter YOUR valid WFU username and password.<br />

If it does not prompt you, or the username on the <strong>for</strong>m shows another person's username, then exit<br />

all Netscape application (close all Netscape browser windows, Netscape e-mail, calendar, etc.) and<br />

start Netscape again and go to the database's URL again.<br />

2. Only designated users can add and update the databases. Mike Thompson is the one who can<br />

assign user permission to add or update the databases. The user permission categories are by<br />

departments, by databases (inventory and msds), by privileges (adding and updating). For<br />

example, a user can be allowed to add chemical to an inventory in the chemistry department only,<br />

but cannot update the inventory.<br />

3. Searching <strong>for</strong> a particular chemical is limited to 1000 matches. It will not display the search<br />

result on the web page if it is over 1000 matches. If this happens, it will save the results in an<br />

Excel spreadsheet and you can download it. You can also try to limit the search.<br />

Note: The Excel spreadsheet will list the username <strong>of</strong> the person doing the search, the date and<br />

time <strong>of</strong> the search, and the criteria <strong>of</strong> the search. There<strong>for</strong>e, if you are going to keep the Excel<br />

spreadsheet, this should provide you enough in<strong>for</strong>mation about “who, when and what”. If someone<br />

is doing a search <strong>of</strong> over 1000 matches at about the same time you are or be<strong>for</strong>e you download the<br />

Excel spreadsheet, you may encounter problems getting the correct Excel spreadsheet. But, always<br />

check the in<strong>for</strong>mation <strong>of</strong> “who, when, what” at the top <strong>of</strong> the spreadsheet to make sure you are<br />

getting the matches you are expecting. If it is not your search result, try re-submit the search again<br />

and download the Excel spreadsheet ASAP.<br />

4. You can Update your inventories but there is no direct "Delete" on the web. It's because it is<br />

too easy to delete items unintentionally on the web. If you want to delete an item, try use Update,<br />

and add the word "delete" (all small cases) in front <strong>of</strong> the item's chemical name. We will remove<br />

those items that are labeled "delete" from the databases on a regular basis. But, you can at least<br />

change your mind and "undelete" the items (by removing the “delete” word in the chemical name)<br />

as long as we have not removed those items yet.<br />

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D. Individual Chemical Inventories <strong>of</strong> the Chemistry Department, Salem<br />

Hall:<br />

listed in the Order they appear in the scroll-down list in the Oracle-based<br />

online Chemical Inventory:<br />

Faculty Inventories:<br />

Dr. Alexander (listed as Alexanr in online inventory), room # 108, Salem Hall<br />

Dr. Bierbach (bierbach), room # 107<br />

Dr. Brown (brownba), room # 14<br />

Dr. Buchmueller (Buchmueller), room # 1<br />

Dr. Colyer (colyer), room # 114<br />

Dr. Hinze (hinze), room # 109<br />

Dr. Jones (jones), room # 118<br />

Dr. Paul Jones (jonespb), room # 113<br />

Dr. Bruce King (King), room # 17<br />

Dr. Kondepudi (Kondepudi), room # 5<br />

Dr. Lachgar (lachgar), room # 6<br />

Dr. N<strong>of</strong>tle (n<strong>of</strong>tle), room # 117<br />

Dr. Sw<strong>of</strong><strong>for</strong>d (Sw<strong>of</strong><strong>for</strong>d), room # 7<br />

Dr. Tobey (Tobey), room # 2<br />

Dr. Welker (welker), room # 13<br />

Undergraduate Lab and Departmental overflow Inventories:<br />

General Chemistry Labs 111L, 230L, and 260L (general), room # 103<br />

Departmental Dyes and Indicators cabinet (indicator), room # 103<br />

Advanced Inorganic Chemistry Lab 361L (inorganic), room # 19<br />

Everyday Chemistry Lab 108L (nonmajors), room # 103<br />

Organic Chemistry Labs 122L and 223L (organic), room # 103 and 19<br />

Loading Dock Departmental Overflow Chemicals (room19), room # 19<br />

Physical Chemistry Lab 341L (room7), room # 7<br />

Loading Dock <strong>Solvent</strong> Room (solvent), room # 20<br />

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