Guidelines for care & Use of Dry Solvent Stills [Example]

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Use of Reflux Condensers Both undergraduate organic laboratories and research laboratories frequently require the heating of liquid mixtures to facilitate chemical reactions. These mixtures are composed of reactants dispersed in organic solvents, usually in round-bottomed flasks capped by upright, jacketed water-filled glass tubes refereed to as reflux condensers. Common, generally nontoxic solvents can be refluxed on open laboratory benches. Ideally, however, all reflux condensers should be set up in a hood, in case too much heat is applied and vapors rise out of the condenser. Since boiling solvents do not increase in temperature, increasing the heat applied will only cause loss of solvent vapor, not an increase in reaction rate. A condensation level of 1 or 2 inches above the bottom of the condenser tube is all that is necessary. Tap water is cold enough for most refluxes. However, very low boiling solvents like acetone or ethyl ether may require ice-cooled water supplied with submersible lab pumps. Constant temperature waterbaths can also be used. The condensers should be placed vertically onto the round bottom heating flask and attached firmly to ring stands with metal clamps. The water inlet should be through the lower end of the condenser. Water hoses should be clamped onto water inlets/outlets on the condensers with Ace Glass wire hose clamps (located in the stockroom for Departmental use) or thick copper wire, twisted on firmly with a pair of pliers (Thin wire could eventually slice through the tubing). Hose clamps are not a good idea. Surging pressure in Salem Hall water lines could cause water hoses to slip off if they are held onto a serrated condenser hose adapter fittings with flat hose clamps. The only disadvantage of using wires is that you must cut them off periodically when they become corroded and replace them. Use of Tygon tubing, instead of rubber, will allow you to actually see the water flowing through the hose. You can then run water through with a relatively slow speed, which is all you need in water condenser coils. Also, this means there will be less chance of a spill when inevitable water pressure surges occur in Salem Hall at night. The water pressure never falls to zero, so you basically can’t have the water flow on too low. Once you have connected the water hose clamps, gently but firmly pull on the lines to make sure they are on tight. I am currently looking for inexpensive in-line water flow indicators (will purchase those without molded plastic halves which could pry apart under water pressure surges) which you can attach anywhere in the water line to more readily judge the flow of water through the line. You may also purchase Water-Flow Monitor sensor instruments with solenoid valve automatic water shut-off mechanisms for about $600 from I2R Company. "Bumping" of solvents can be avoided by adding boiling stones. Magnetic stir bars can also be added to stir the boiling solution, allowing more even boiling. Safe Use of Laboratory Centrifuges Lab centrifuges in Salem Hall are of the low-speed type, and do not need special handling requirements. They are supported on suction-cup feet and will not ordinarily wobble to the point of falling off bench tops. Balance them by placing test tubes half filled with water immediately opposite the test tube being centrifuged. Occasionally check the power cord and keep extraneous lab equipment from cluttering bench tops near the centrifuge. 136
Use of the Hydraulic Press (prepared by Dr. Ron Noftle) (Note: Serious injury can result if you do not set the press up properly so pay attention to these directions.) 1. Be sure that the parts of the sample press fit together in alignment. All of the parts must contact each other and the sample perfectly. 2. When you place the assembled sample press in the hydraulic press: a. make sure that it is in the middle of the hydraulic press plate b. place the aluminum plate over the plunger and gradually crank the hydraulic press until the system is tight. c. check to make sure that the sample press is perfectly vertical with respect to the hydraulic press and does not lean at all d. close the Plexiglas door e. crank up the pressure to no more than 12,000 PSI. Allow the sample to sit in the press for a few minutes so that the heat will be dissipated and then gradually release the pressure. Upper Plate of Hydraulic Press (bottom view) Al Plate Sample Press Bottom Plate of Hydraulic Press (side view) You can see that, if the sample press is not placed properly in the hydraulic press, on applying pressure, it (or pieces of it) could fly out at tremendous speed and could go right through the Plexiglas door which is really only a first-line protection. This has happened at other laboratories 137
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Wake Forest University Chemistry De
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11. Dr. Lachgar - Lab Room # 6 ....
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I. INTRODUCTION A hardcopy of this
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II. Telephone #s of Emergency Perso
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B. Emergency Exit Plan for All Sale
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A. Emergency Telephone Numbers of L
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2. Dr. Bierbach - Lab Room #107 Lab
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6. Dr. Hinze - Lab Room #109 Lab Pe
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8. Dr. Paul Jones - Lab Room #113 L
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10. Dr. Kondepudi - Lab Room #5 Lab
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12. Dr. Noftle - Lab Room #117 Lab
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14. Dr. Tobey - Room # 2 Lab Person
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16. Undergraduate - Lab Room #s 7,
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11. Do not force glass tubing into
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2. Cleanliness in the Research Labo
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3. Housekeeping for All Labs Housek
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INVENTORY OF EYEWASH FOUNTAINS AND
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“COMMON FIRE CODE VIOLATIONS “E
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) 4-Bromodimethylaniline HAZARDOUS
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manager and stockroom personnel usi
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Mineral acids (HCl, HNO 3 and H 2 S
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(one kilogram per month, total amou
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All other organic solvents not on t
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3. Preliminary Considerations for S
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OPERATING INFORMATION FOR FHM 400 F
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E. Laboratory Operations which requ
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F. Provisions for Additional Protec
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G. Specific Procedures for Safe Rem
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2. Dr. Bierbach - Lab Room #107 SPE
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3. Dr. Brown - Lab Room #14 SPECIFI
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Dry soft things: Weighing paper, pa
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5. Dr. Colyer - Lab Room # 114 SPEC
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6. Dr. Hinze - Lab Room # 109 SPECI
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8. Dr. Paul Jones - Lab Room # 14 S
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10. Dr. Kondepudi - Lab Room # 5 SP
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� Ammonium hydroxide � Ammonium
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C. General Information for Users (W
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