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CETAC M-7600 Mercury Analyzer Operator's Manual

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<strong>CETAC</strong> M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Operator’s <strong>Manual</strong><br />

<strong>Manual</strong> Part Number 480195 Rev 2


COPYRIGHT<br />

© 2008, 2012 <strong>CETAC</strong> Technologies<br />

480195 Rev 2 , October, 2012<br />

<strong>CETAC</strong> Technologies authorizes its customers<br />

to reproduce, transmit, or store this document<br />

in its entirety, including this page, for the<br />

express purpose of installing, operating, or<br />

maintaining the product described herein.<br />

<strong>CETAC</strong> Technologies<br />

Customer Service & Support<br />

14306 Industrial Road<br />

Omaha, Nebraska 68144, USA<br />

Phone (800) 369-2822 (USA only)<br />

Phone (402) 733-2829<br />

Fax (402) 733-1932<br />

E-mail custserv@cetac.com<br />

REVISIONS<br />

<strong>CETAC</strong> Technologies strives to provide the<br />

scientific community with an unparalleled<br />

combination of effective technology and<br />

continuing value. Modular upgrades for<br />

existing instruments will continue to be a<br />

prime consideration as designs progress.<br />

<strong>CETAC</strong> Technologies reserves the right to<br />

revise this document and/or improve<br />

products described herein at any time without<br />

notice or obligation. Warranty registration<br />

entitles the named owner exclusively to<br />

manual change pages/new editions as they<br />

are published.<br />

TRADEMARK ACKNOWLEDGEMENTS<br />

Windows is a registered trademark of<br />

Microsoft Corporation in the United States and<br />

other countries.<br />

Nafion ® is a registered trademark of DuPont<br />

(E.I. du Pont de Nemours and Company).<br />

Perma Pure is a registered trademark of<br />

Perma Pure LLC.<br />

DuPont, Kapton®, Teflon®, Tefzel® and<br />

Viton® are trademarks or registered<br />

trademarks of E.I. du Pont de Nemours and<br />

Company.<br />

PharMed and Tygon are registered<br />

trademarks of Saint-Gobain Performance<br />

Plastics.<br />

Santoprene is a trademark of Exxon Mobil.<br />

KIMWIPES is a registered trademark and<br />

KIMTECH SCIENCE is a trademark of<br />

Kimberly-Clark Worldwide, Inc<br />

All other marks are the property of their<br />

respective owners.


Contents<br />

1 Introduction .............................................................................................................. 7<br />

Overview.................................................................................................................................... 7<br />

About This Book ..................................................................................................................... 7<br />

Who Should Use This Product ................................................................................... 7<br />

Where to Go for More Information ................................................................................ 8<br />

System Features ..................................................................................................................... 9<br />

System Performance Characteristics .......................................................................... 10<br />

Overview of the <strong>Mercury</strong> <strong>Analyzer</strong> .............................................................................. 11<br />

Supplied Equipment ........................................................................................................... 13<br />

Equipment and Supplies ................................................................................................... 14<br />

Required Equipment and Supplies ........................................................................ 14<br />

Recommended Supplies ............................................................................................. 15<br />

2 Preparing for Installation ................................................................................. 17<br />

Establishing Optimal Operating Conditions ............................................................ 17<br />

Creating the Lab Environment ............................................................................... 17<br />

Choosing a Location ............................................................................................................ 18<br />

Space Requirements .................................................................................................... 18<br />

Work Surface Requirements .................................................................................... 20<br />

Ventilation Requirements ................................................................................................ 20<br />

Power Requirements ......................................................................................................... 20<br />

Unpacking the <strong>Mercury</strong> <strong>Analyzer</strong> ................................................................................. 21<br />

3 Installing the <strong>Analyzer</strong> ....................................................................................... 25<br />

Installation Overview......................................................................................................... 25<br />

Step 1: Position the <strong>Mercury</strong> <strong>Analyzer</strong> and Autosampler.................................. 26<br />

Step 2: Connect the Autosampler Peristaltic Pump to the Rinse Station .... 26<br />

Step 3: Set Up the Autosampler ..................................................................................... 30<br />

Step 4: Connect Power and Data Cables to the Back of the <strong>Mercury</strong><br />

<strong>Analyzer</strong> .......................................................................................................................... 39<br />

Step 5: Connect the Carrier Gas Tubing ..................................................................... 40<br />

Step 6: Install the <strong>Mercury</strong> Trap (KMnO 4) ................................................................ 42<br />

Step 7: Connect the Back of the Autosampler ......................................................... 44<br />

Step 8: Connect to the Host Computer ....................................................................... 45<br />

Summary ......................................................................................................................... 45<br />

Installing a Secondary NIC in Your Own PC ...................................................... 45<br />

Connecting the Communication Cables............................................................... 46<br />

Configuring the Network Metrics .......................................................................... 46<br />

Setting the IP Address for the Secondary NIC ................................................... 50<br />

Changing the Subnet of the <strong>Mercury</strong> <strong>Analyzer</strong>................................................. 51<br />

Connecting a Laptop Computer to the M-<strong>7600</strong> ................................................ 52<br />

Step 9: Install the Gas-Liquid Separator (GLS) ....................................................... 53


M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong> Operator’s <strong>Manual</strong><br />

Contents<br />

Step 10: Connect the Peristaltic Pump on the <strong>Mercury</strong> <strong>Analyzer</strong> .................. 57<br />

Installing the Peristaltic Pump Tubing ............................................................... 57<br />

Installing the Mixing Tee and Drain Tees .......................................................... 59<br />

Step 11: Power On and Verify Communication ...................................................... 63<br />

To Configure the Network Connection ................................................................ 63<br />

To Power On the System for the First Time (PC Configured by <strong>CETAC</strong>) 64<br />

To Power On the System for the First Time (Customer-Supplied PC) ..... 64<br />

To Test the Autosampler ........................................................................................... 68<br />

Step 12: Fill the Rinse Solution Bottle ........................................................................ 68<br />

Step 13: Fill the Reagent Bottle ..................................................................................... 69<br />

Preserving the SnCl 2 ................................................................................................... 69<br />

Step 14: Adjust the Peristaltic Pump Tubing Clamp Tension (Optional) ... 70<br />

Step 15: Check the Reagent Flow ................................................................................. 73<br />

Step 16: Check the Sample Probe Flow ..................................................................... 73<br />

4 Using the <strong>Analyzer</strong> ............................................................................................... 75<br />

Theory of Operation ........................................................................................................... 75<br />

Autosampler .................................................................................................................. 75<br />

QuickTrace M-<strong>7600</strong> Automated <strong>Mercury</strong> <strong>Analyzer</strong> .................................... 76<br />

Software................................................................................................................................... 78<br />

Preparing Reagents and Calibration Standards ..................................................... 79<br />

Gas Parameters .................................................................................................................... 81<br />

Starting the System............................................................................................................. 81<br />

<strong>Mercury</strong> Vapor Lamp Warmup .............................................................................. 82<br />

Turning Off the <strong>Mercury</strong> Vapor Lamp for System Warm-Up ..................... 82<br />

System Warm-Up for Trace or Ultra-Trace Analysis ..................................... 82<br />

System Warm-Up for ppb or Non-Ultra-Trace Analysis ............................... 83<br />

Wetting the GLS .................................................................................................................... 84<br />

Running the Interactive Demo ...................................................................................... 87<br />

Overview of the <strong>CETAC</strong> QuickTrace Software ..................................................... 87<br />

Learning More .............................................................................................................. 88<br />

QuickTrace M-<strong>7600</strong> Startup Summary ................................................................... 89<br />

Setting Baseline Correction ............................................................................................ 91<br />

Keeping an Instrument Log Book .......................................................................... 91<br />

Viewing the Graphs ..................................................................................................... 92<br />

Setting a One-Point Baseline ................................................................................... 92<br />

Setting a Two-Point Baseline .................................................................................. 94<br />

Summary of Gas and Liquid Flows for Analytical Ranges of the<br />

QuickTrace M-<strong>7600</strong> ................................................................................................ 98<br />

Placing the QuickTrace M-<strong>7600</strong> in Standby Mode ......................................... 100<br />

Cold Shutdown .................................................................................................................. 101<br />

Summary of QuickTrace M-<strong>7600</strong> Shut Down .............................................. 101<br />

5 Maintaining the <strong>Mercury</strong> <strong>Analyzer</strong> ............................................................. 103<br />

Maintenance Schedule ................................................................................................... 103<br />

Daily Maintenance (Always Check Before Analysis) .................................... 103<br />

Weekly Maintenance ................................................................................................ 104<br />

Monthly Maintenance .............................................................................................. 104<br />

Yearly Maintenance .................................................................................................. 104<br />

Autosampler Yearly Maintenance....................................................................... 105<br />

Removal or Inspection of the Sample Cell ............................................................. 105<br />

Opening the Optics Access Panel ......................................................................... 105<br />

Removing the Sample Cell ...................................................................................... 107<br />

4


M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong> <strong>Operator's</strong> <strong>Manual</strong><br />

Contents<br />

Cleaning the Cell Windows ........................................................................................... 107<br />

Quick Exposed Surface Cleaning ......................................................................... 107<br />

Dismantling for Total Cleaning ........................................................................... 109<br />

Cell Assembly...................................................................................................................... 109<br />

Cleaning the Gas-Liquid Separator ........................................................................... 112<br />

Changing the Cell Gas Tubing ...................................................................................... 113<br />

Retubing the Gas-Liquid Separator .......................................................................... 115<br />

GLS Inlet........................................................................................................................ 115<br />

GLS Drain ..................................................................................................................... 116<br />

Replacing the Perma Pure ® Dryer Cartridge ........................................................ 117<br />

GLS Overflow Recovery .................................................................................................. 119<br />

Replacing the Hg Lamp Bulb ........................................................................................ 124<br />

When to Replace or Service the Lamp .............................................................. 124<br />

Cleaning the EOFM ................................................................................................... 124<br />

Getting a Replacement Lamp ............................................................................... 125<br />

Caring for the Lamp ................................................................................................. 126<br />

Replacing the Lamp ................................................................................................. 126<br />

Adjusting the Lamp Current ................................................................................. 129<br />

Replacing the Fuse ........................................................................................................... 131<br />

6 Troubleshooting the <strong>Mercury</strong> <strong>Analyzer</strong> .................................................... 133<br />

Troubleshooting Communication Issues ............................................................... 133<br />

Step 1: Check the Cable ........................................................................................... 133<br />

Step 2: Use the IPSetup Tool to Check the Configuration .......................... 133<br />

Step 3: Check the Subnet Configuration Using the Define QuickTrace<br />

Hardware Tool .................................................................................................. 134<br />

Step 4: Check for an IP address conflict ........................................................... 137<br />

If the IPSetup Tool Does Not Find the M-<strong>7600</strong> .............................................. 138<br />

"Subnet of this PC and the M-<strong>7600</strong> are Not Compatible" Error ............. 139<br />

Cannot Zero Instrument ................................................................................................ 140<br />

"Integration Adjustment Reached" Messages ...................................................... 140<br />

Drifting Baseline ................................................................................................................ 140<br />

Low Absorbance or No <strong>Mercury</strong> Response ........................................................... 141<br />

No Liquid or Gas Flow .................................................................................................... 141<br />

No Sample or Rinse Flow ....................................................................................... 141<br />

No SnCl 2 Flow ............................................................................................................. 142<br />

No Drain Flow ............................................................................................................ 142<br />

No Gas Flow or Low Gas Flow .............................................................................. 142<br />

Double Peak with Low Absorbance .......................................................................... 142<br />

Poor Reproducibility ....................................................................................................... 143<br />

Noisy Baseline .................................................................................................................... 144<br />

Bad DL .................................................................................................................................... 144<br />

Sudden Standard Absorbance Rise During Run .................................................. 144<br />

Poor Accuracy .................................................................................................................... 145<br />

Returning the Product to <strong>CETAC</strong> for Service ........................................................ 146<br />

Shipping the Product ............................................................................................... 146<br />

Product Warranty Statement .............................................................................. 146<br />

Returned Product Procedures .............................................................................. 147<br />

Returned Product Warranty Determination ................................................. 147<br />

7 Safety and Regulatory Information ............................................................. 149<br />

Characteristics ................................................................................................................... 149<br />

Environmental Characteristics ............................................................................ 149<br />

5


M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong> Operator’s <strong>Manual</strong><br />

Contents<br />

Electrical Characteristics ....................................................................................... 150<br />

Safety Notices ..................................................................................................................... 151<br />

Replacement Parts .................................................................................................... 151<br />

Chemical Hazards ...................................................................................................... 151<br />

Power Cord Set Requirements .............................................................................. 151<br />

Power Cord Safety Maintenance ......................................................................... 151<br />

Grounding ..................................................................................................................... 152<br />

Mains Disconnect ....................................................................................................... 152<br />

Mechanical Hazards ................................................................................................. 152<br />

Cleaning Instructions ............................................................................................... 153<br />

Operating Environment .......................................................................................... 153<br />

Explanation of Caution and Warning Notices ............................................... 154<br />

Avertissements en Français ......................................................................................... 155<br />

Electromagnetic Interference ..................................................................................... 156<br />

Explanation of Regulatory Marks .............................................................................. 156<br />

8 Glossary ................................................................................................................. 157<br />

6


1 Introduction<br />

Overview<br />

The <strong>CETAC</strong> QuickTrace M-<strong>7600</strong> mercury analyzer measures trace levels of<br />

mercury in aqueous solution by Cold Vapor Atomic Absorption Spectrometry<br />

(CVAAS). CVAAS does not require heating the sample with a flame, plasma, or<br />

furnace. The mercury analyzer’s modular design permits remarkably easy<br />

maintenance access and a reduced countertop footprint. Sturdy construction,<br />

drift-stabilized double beam optics, thermal and electro-optical lamp<br />

stabilization, and an unusually stable “non-foaming” Gas-Liquid Separator (U.S.<br />

Patent #5,792,663) collectively afford exceptional structural integrity and<br />

signal stability. The QuickTrace M-<strong>7600</strong> exhibits a high signal-to-noise ratio<br />

and ultra-trace detection limits for an absorbance system that is fully<br />

compliant with EPA CVAA methods such as 245.7, 245.1, 245.5, SW846 7470<br />

and 7471.<br />

About This Book<br />

This document describes the procedures for installing, using, and maintaining<br />

the analyzer.<br />

This manual covers the following products:<br />

‣ <strong>CETAC</strong> QuickTrace M-<strong>7600</strong> mercury analyzer<br />

Who Should Use This Product<br />

The primary audience for this manual consists of mercury detection and<br />

mercury measurement laboratory managers, chemists, technicians, fieldservice<br />

engineers and owners of the QuickTrace M-<strong>7600</strong> mercury analyzer.<br />

To use this product effectively, you should have a basic knowledge of mercury<br />

analysis, at least a beginning level of computer experience, and a basic<br />

knowledge of chemical handling procedures including the handling of<br />

organomercurials.<br />

Before operating the QuickTrace M-<strong>7600</strong> analyzer, autosampler, or optional<br />

ADX-500 autodilutor, it is important to read this manual, the QuickTrace<br />

Software <strong>Manual</strong>, the Autosampler Operator’s <strong>Manual</strong>, and (if applicable) the<br />

ADX-500 Autodilutor Accessory Operator’s <strong>Manual</strong>.


Operator’s <strong>Manual</strong><br />

Chapter 1: Introduction<br />

Where to Go for More Information<br />

In addition to this manual, you can refer to the following resources:<br />

‣ The QuickTrace Software <strong>Manual</strong> and built-in help<br />

‣ The M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong> PC Setup Guide<br />

‣ The <strong>CETAC</strong> Autosampler Operator’s <strong>Manual</strong><br />

‣ The ADX-500 Autodilutor <strong>Manual</strong> (optional)<br />

‣ U.S. EPA Method 245.1; method for Hg determination in drinking water<br />

‣ U.S. EPA Method 245.7; <strong>Mercury</strong> in Water by Atomic Fluorescence<br />

Spectrometry<br />

‣ U.S. EPA, Office of Solid Wastes. SW846 Method 7470A; <strong>Mercury</strong> in Liquid<br />

Waste (Cold-Vapor Technique)<br />

‣ U.S. EPA, Office of Solid Wastes, SW846 Method 7471B; <strong>Mercury</strong> in Solid or<br />

Semisolid Waste (Cold-Vapor Technique)<br />

‣ American Society for Testing and Methods. ASTM D3223-91; Standard Test<br />

Method for Total <strong>Mercury</strong> in Water<br />

‣ The <strong>CETAC</strong> Technologies Web site: www.cetac.com<br />

‣ <strong>CETAC</strong> Technologies Customer Service and Support:<br />

1 (800) 369-2822 (USA only)<br />

1 (402) 733-2829<br />

1 (402) 733-1932 (Fax)<br />

E-mail: custserv@cetac.com<br />

8


<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 1: Introduction<br />

System Features<br />

The QuickTrace M-<strong>7600</strong> incorporates the following features to form an<br />

automated, integrated mercury analysis system.<br />

‣ Computer-controlled four-channel high-performance peristaltic pump<br />

(12-roller pump head).<br />

‣ Ozone-free Hg Lamp. No lamp ventilation is needed.<br />

‣ Thermally controlled Hg lamp housing (for a stabilized Hg vapor lamp).<br />

‣ Stable high performance Gas-Liquid Separator (GLS). (U.S. Patent<br />

#5,792,663). Non-foaming/non-bubbling “thin liquid film” GLS design,<br />

which allows trouble-free direct analysis of blood, urine, and fish tissue<br />

digests as well as standard water and waste analysis.<br />

‣ Rigid, shock and vibration-isolated optical rail (mounting the Hg lamp,<br />

collimator lens, absorption tubes, camera, CCD detector, and A/D<br />

converter).<br />

‣ Precise, self-aligning optical mounts, no optical alignment required,<br />

maximizing the convenience of instrument baseline zeroing. This design<br />

extends maintenance intervals without loss of performance.<br />

‣ Long path (220 mm) absorbance cells.<br />

‣ Hg lamp electro-optical feedback beam utilizing a high-performance solidstate<br />

detector for ultra-fine lamp stabilization.<br />

‣ Fixed optical interference filters, three each (254 ± 2 nm wavelength, 20%<br />

T, 12.7 mm dia.). No moving parts.<br />

‣ Standard Perma Pure ® dryer cartridge eliminates the need for Mg(ClO 4) 2<br />

drying agent.<br />

‣ Stabilized double beam optics - traditional double-beam (sample and<br />

reference) with a CCD detector.<br />

‣ Internal ADC (Analog-to-Digital Conversion).<br />

‣ High-rate data sampling.<br />

‣ Computer controlled system shutdown/standby routines.<br />

‣ Integrated optional autosamplers for accommodation of calibration<br />

standards and up to 720 samples.<br />

‣ Ethernet communications.<br />

‣ Gas exhaust Hg vapor safety trap (solid crystalline KMnO 4).<br />

9


Operator’s <strong>Manual</strong><br />

Chapter 1: Introduction<br />

System Performance Characteristics<br />

‣ Ultra-trace detection limits: < 0.5 ppt at 40 mL / min. carrier gas flow 1 .<br />

(Direct steady state absorbance mode, without pre-concentration by gold<br />

amalgamation).<br />

‣ Wide dynamic linear working range, ≅ 4 orders of magnitude.<br />

‣ Short term precision (%RSD @ 95% Confidence) < 6.0% @ 5 ppt, n=5<br />

‣ Short term precision (%RSD @ 95% Confidence) < 1.2% @ 20 ppt, n=5<br />

‣ Long term precision (%RSD @ 95% Confidence) < 2.7%/h @ 200.0 ppt<br />

‣ 99% Confidence Accuracy @ 5 ppt; ±3.1%<br />

‣ 99% Confidence Accuracy @ 20 ppt; ±4.3%<br />

‣ Sample Throughput < 3.5 min/sample at IDL<br />

‣ Ultra-low drift rates ≤ 300 µAbs/hr (after warm-up) raw uncorrected<br />

analog baseline on-screen drifts.<br />

‣ Ultra-low short-term absorbance noise ≤ 200 µAbs (10 -5 Abs).<br />

‣ 0.1% “raw” Hg lamp stability (single beam output).<br />

‣ Unusually fast washout ≈ 240 sec. from 1ppm Hg, at 1000 mL/min gas<br />

flow.<br />

‣ <strong>Mercury</strong> Response: ≥ 14,000 µAbs / ppb 2 at 100 mL/min carrier gas flow.<br />

1 One hour minimum warm-up using the standard Nafion ® dryer and a gas flow equal<br />

to 40 mL/min along with prescribed tubing and reagents. Using pump speed, uptake<br />

and rinse times specified for standard Nafion ® dryer in Table 4-1 (p. 72), and ≥12 s<br />

integration cycle selected on the "flattest" portion of the peak time profile.<br />

2 Using prescribed tubing, reagents, and pump speed.<br />

10


<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 1: Introduction<br />

Overview of the <strong>Mercury</strong> <strong>Analyzer</strong><br />

Power and Status Lights<br />

Perma Pure ® Dryer Cartridge<br />

Gas-Liquid Separator (GLS)<br />

Peristaltic Pump<br />

Figure 1-1<br />

M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong>—Front View.<br />

Sample Probe<br />

Rinse Bottle<br />

Autosampler<br />

(ASX-520 is shown)<br />

Reagent Bottle<br />

Figure 1-2<br />

M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong>—Front View with Autosampler.<br />

11


Operator’s <strong>Manual</strong><br />

Chapter 1: Introduction<br />

Autosampler<br />

Peristaltic Pump<br />

<strong>Mercury</strong> Trap<br />

Autosampler<br />

Power Switch<br />

Electrical<br />

Connectors<br />

M-<strong>7600</strong><br />

Power Switch<br />

Figure 1–2<br />

M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong> —Back View of Complete System.<br />

Auxiliary I/O Ports<br />

Ethernet Port<br />

Auxiliary Input Port<br />

Auxiliary Power<br />

Ports<br />

M-<strong>7600</strong><br />

Power Switch<br />

M-<strong>7600</strong><br />

Power Cord<br />

Figure 1-3<br />

M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong> —Electrical Connectors.<br />

The following components are located on the front of the mercury analyzer<br />

(see Figure 1-2).<br />

‣ POWER Indicator. The top blue LED indicates that the analyzer is<br />

connected to a power source and turned on.<br />

‣ LAMP ON Indicator. Indicates when the internal mercury vapor lamp is<br />

turned on.<br />

‣ OVER RANGE Indicator. Indicates that the internal mercury vapor lamp is<br />

drawing more than the recommended amount of current. This LED will<br />

glow for a few seconds while the mercury lamp warms up when the<br />

mercury analyzer is first turned on and the QuickTrace software is<br />

started or any time the lamp is off and then powered on via software<br />

controls.<br />

‣ Perma Pure ® Dryer Cartridge. Uses a DuPont Nafion ® membrane to<br />

remove humidity from the sample gas.<br />

‣ Gas-Liquid Separator (GLS).<br />

‣ Front Cover. Protects the GLS and dryer cartridge. An LED lamp<br />

illuminates the area behind the cover whenever the mercury analyzer is<br />

turned on.<br />

12


<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 1: Introduction<br />

‣ Peristaltic Pump. A four-channel peristaltic pump is built into the front of<br />

the mercury analyzer.<br />

The following components are located on the back of the analyzer:<br />

‣ POWER Switch. Turns power to the M-<strong>7600</strong> mercury analyzer on and off.<br />

This switch also controls power to the autosampler, when powered<br />

through the mercury analyzer.<br />

‣ Gas Ports. Gas inlet and exhaust ports.<br />

‣ <strong>Mercury</strong> Trap. The trap scrubs mercury from the exhaust gas.<br />

The following electrical connectors are located on the back of the analyzer:<br />

‣ Ethernet Port. The Ethernet port is used to interface the mercury<br />

analyzer with the host computer.<br />

‣ Auxiliary Communication Ports. The two AUX I/O ports and one AUX<br />

INPUT port are reserved for use with other <strong>CETAC</strong> instruments.<br />

‣ Power Output Connectors. Provides power for the autosampler and for<br />

an optional auxiliary device.<br />

Supplied Equipment<br />

The following standard components are supplied with the mercury analyzer:<br />

‣ M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong>.<br />

‣ CD. The CD contains:<br />

• QuickTrace software<br />

• This manual<br />

• Other application-specific information<br />

‣ Gas-Liquid Separator.<br />

‣ Perma Pure ® Dryer Cartridge. Uses a DuPont Nafion ® membrane to<br />

remove humidity from the sample gas. The cartridge is pre-installed in the<br />

mercury analyzer.<br />

‣ KMnO 4 Absorbent Trap. This scrubs mercury from the exhaust gas. The<br />

KMnO 4 is not included.<br />

‣ Bottles. One reagent bottle and one rinse bottle are provided.<br />

‣ PCI Ethernet Adapter Board.<br />

‣ Power Cord and Cables. An Ethernet cable, a power cord for the mercury<br />

analyzer, and a power cord for the autosampler are supplied.<br />

Depending on how the system was ordered, the following optional equipment<br />

may be supplied:<br />

‣ Computer. The mercury analyzer may be ordered with a computer which<br />

is pre-configured with the QuickTrace software.<br />

‣ <strong>CETAC</strong> ASX-520/260/130 Autosampler.<br />

‣ <strong>CETAC</strong> ADX-500 Autodilutor.<br />

‣ ENC-500 Enclosure.<br />

13


Operator’s <strong>Manual</strong><br />

Chapter 1: Introduction<br />

WARNING<br />

The computer, autosampler, and optional accessories have their own<br />

manuals (printed or on CD-ROM). Before using the equipment, read those<br />

manuals to understand the precautions you must take to avoid possible<br />

hazards.<br />

Equipment and Supplies<br />

Required Equipment and Supplies<br />

‣ Inert Gas Regulator.<br />

Two-stage, 10-200 psig (70-1380 kPa) secondary pressure gauge, with<br />

plumbing couple for either a cylinder or Dewar capable of delivering 150<br />

psig (1040 kPa).<br />

‣ AC Power Strip.<br />

Surge protected with six outlets, 15-20 A.<br />

‣ Cylinder or Dewar, UHP Nitrogen or Argon Gas.<br />

Ultra-high purity, dry, research grade N 2 or 99.999% purity Ar. The<br />

QuickTrace M-<strong>7600</strong> has a user replaceable 2-micron filter, which<br />

prevents damage from particulates to the internal gas control components.<br />

‣ <strong>Mercury</strong> Standard Solution.<br />

1000 ppm (minimum order quantity).<br />

‣ Hydrochloric Acid Trace Metal Grade (37%).<br />

Trace metal HCl will be used in the preparation of Hg standards, SnCl 2<br />

reagent and in some method applications. If an application is more<br />

demanding, a better grade of acid may be needed (for example, double<br />

distilled).<br />

‣ Nitric Acid Trace Metal Grade (68-70%).<br />

Trace metal HNO 3 will be used in sample preparation, cleaning glassware<br />

(lab glassware and the QuickTrace Gas-Liquid Separator) and added to<br />

the QuickTrace rinse solution to help maintain the cleanliness of the<br />

system during operation.<br />

‣ Stannous Chloride (Crystals, Di-Hydrate).<br />

Two 500g containers minimum order, “suitable for Hg determination.” The<br />

stock SnCl 2 is introduced into the QuickTrace at a steady flow rate and<br />

therefore any mercury contamination will be negated during the<br />

instrument zero.<br />

‣ Potassium Permanganate. Solid, Crystalline.<br />

The least expensive available grade at a minimum quantity is sufficient<br />

unless it is also to be used for oxidative sample preparation. This lowgrade<br />

reagent stock is sufficient to fill a safety trap for retention of Hg<br />

vapor exhaust from the instrument.<br />

‣ 2-propanol. High Purity, “Spectrophotometric” Grade.<br />

2-propanol will be used for cleaning the optical cells and cell windows.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 1: Introduction<br />

‣ KIMTECH SCIENCE KIMWIPES® Delicate Task Wipers.<br />

‣ Additional Chemical Compounds.<br />

The sample preparation procedures of the intended analytical method may<br />

require additional chemical compounds. Refer to published method<br />

specifications.<br />

Recommended Supplies<br />

‣ Volumetric flasks 100 mL class A (TC) six each.<br />

‣ Volumetric flasks 1000 mL class A (TC) two each.<br />

‣ Precision air displacement micropipettes, 10 to 10,000 µL (TD).<br />

‣ Replacement tips for micropipettes.<br />

‣ Disposable plastic dropping pipettes.<br />

‣ Graduated cylinders, 10 and 100 mL.<br />

‣ Polypropylene or polyethylene bottle with Cap, 1 L.<br />

‣ Weighing balance, top loading, 0.1 g readability (or better), any available<br />

capacity will work (1.1 kg capacity is good).<br />

‣ Laboratory scoopula and large spatula.<br />

‣ Stopwatch (for measuring liquid uptake rates).<br />

‣ Stirring rod.<br />

‣ Powder funnel, wide bore stem, small overall size.<br />

‣ Wrenches, adjustable 12" and 6".<br />

‣ Screw drivers:<br />

• 1 small Phillips<br />

• 1 medium Phillips<br />

• 1 long-shank medium flat-blade<br />

• 1 small thin flat-blade<br />

‣ Deionized water.<br />

‣ Flow meter 0 – 1,500 mL/min. with 1 mL/min. readability, calibrated to<br />

user’s choice of carrier gas (Ar or N 2).<br />

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Chapter 1: Introduction<br />

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16


2 Preparing for<br />

Installation<br />

Installing the analyzer requires preparation. Before you install the analyzer,<br />

you should evaluate the physical arrangement of the laboratory to choose a<br />

suitable location. Once you choose a location, you must carefully unpack the<br />

analyzer prior to beginning the installation.<br />

This chapter discusses what requirements must be met when you choose a<br />

location. It also describes how to unpack the equipment before installation.<br />

Establishing Optimal Operating Conditions<br />

The mercury analyzer operates reliably even under less than ideal conditions.<br />

It is not, however, indestructible. Malfunction or damage can occur if specific<br />

operating conditions are not met. Meeting these conditions requires that you<br />

create the proper lab environment, replace analyzer components that wear out<br />

under normal use, and purchase the appropriate supplies for use with the<br />

analyzer.<br />

NOTE<br />

Damage or malfunction that results from unsatisfactory operating conditions<br />

may constitute misuse and abuse and be excluded from warranty coverage.<br />

Creating the Lab Environment<br />

To create satisfactory operating conditions in your lab environment, follow<br />

these guidelines:<br />

‣ Operate the analyzer in a conventional lab environment where the<br />

temperature is 60–90 °F (15–32 °C), the humidity is 20–70%<br />

non-condensing, and the unit is not exposed to excessive flammable or<br />

corrosive materials.<br />

‣ Avoid rough handling of the analyzer. If possible, do not expose the<br />

analyzer to vibration or shock.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 2: Preparing for Installation<br />

‣ Protect the analyzer from long-term exposure to condensation, corrosive<br />

materials, solvent vapor, continual standing liquids.<br />

‣ Observe the same general electrostatic discharge precautions as with any<br />

other integrated circuit electronic devices. Low humidity environments,<br />

especially when combined with static-generating materials, require<br />

maximum care.<br />

CAUTION<br />

Discharge static buildup and ground to the analyzer base or cabinet before<br />

performing any maintenance. Do not touch or short-circuit bare contacts or<br />

connectors.<br />

‣ Avoid using the analyzer if strong electromagnetic interference or radio<br />

frequency interference is present. Interference fields can cause erratic<br />

operation of the analyzer.<br />

Choosing a Location<br />

Space Requirements<br />

The QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong> System includes the base unit, PC<br />

with monitor, reagent and rinse bottles, and an optional autosampler.<br />

A typical system requires a minimum footprint for countertop installation of<br />

183cm (6’) X 31cm (2’) X 91cm (3’) (W x D x H). A floor space of 1’ (30cm) X 1’<br />

(30cm) is required for the liquid waste receptacle. The space for the waste can<br />

be directly below the analyzer, or directly in front of the lab bench and in line<br />

with the peristaltic pump.<br />

86 cm (34 inches)<br />

183 cm (6 feet)<br />

Figure 2-1 Footprint of QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

with ASX-520 Autosampler.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 2: Preparing for Installation<br />

71 cm (28 inches)<br />

142 cm (56 inches)<br />

Figure 2-2 Footprint of QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

with ASX-260 Autosampler.<br />

71 cm (28 inches)<br />

142 cm (56 inches)<br />

Figure 2-3 Footprint of QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

with ASX-130 Autosampler.<br />

46 cm<br />

(18.1 in)<br />

20 cm<br />

(7.9 inches)<br />

56 cm<br />

(22.0 inches)<br />

Figure 2-4 Dimensions of the QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong>.<br />

The work surface should be at least 61 cm (24 inches) deep if it is accessible<br />

from both front and back. If the work surface is against a wall, it should be at<br />

least 76 cm (30 inches, if possible) deep. If possible, allow at least 15 cm (6<br />

inches) behind the system for cable egress, ventilation, and access to the<br />

power switches.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 2: Preparing for Installation<br />

Always position the equipment so that it is easy to disconnect the power cord.<br />

Work Surface Requirements<br />

The analyzer must be placed on a sturdy countertop or table. It is not<br />

recommended to place the analyzer on a wheeled cart or folding table.<br />

If the analyzer is to be used in an earthquake zone, choose a location or secure<br />

it so that it will not fall and cause injury or damage during an earthquake.<br />

Ventilation Requirements<br />

During operation, the QuickTrace M-<strong>7600</strong> internally contains trace amounts<br />

of mercury vapor. To prevent inhalation of the vapor, the QuickTrace M-<strong>7600</strong><br />

uses a solid KMnO 4 absorbent trap located on the back of the instrument. This<br />

trap absorbs the mercury vapor prior to final exhaust; therefore no extra<br />

ventilation is required beyond that of a standard laboratory environment.<br />

WARNING<br />

INHALATION HAZARD<br />

Gases exhausting from the QuickTrace M-<strong>7600</strong> cabinet prior to the<br />

external Hg vapor trap (affixed to the rear cabinet panel) contain traces of<br />

mercury vapor and will cause injury if inhaled. Do not run the QuickTrace<br />

M-<strong>7600</strong> unless exhausted gas is properly “scrubbed” or removed. Fill,<br />

maintain, and use the provided KMnO 4 absorbent trap or run a transfer line<br />

to a fume hood.<br />

The ambient temperature should be kept as stable as possible. Locating the<br />

QuickTrace M-<strong>7600</strong> directly in the path of an air conditioner or heater vent<br />

may cause baseline drift, and is not recommended.<br />

NOTE<br />

Due to the likelihood of accelerated damage from corrosion and dust, locating<br />

the QuickTrace M-<strong>7600</strong> in a fume hood with stagnant air automatically voids<br />

the warranty.<br />

Power Requirements<br />

The QuickTrace M-<strong>7600</strong> mercury analyzer includes a built-in switching<br />

power supply which supports line voltages in the range 100-240 VAC at<br />

frequencies of 50-60 Hz. See “Electrical Characteristics” on page 150 for<br />

detailed power requirements.<br />

The autosampler is powered by the M-<strong>7600</strong>'s AUX POWER output. See the<br />

autosampler manual for more details.<br />

The power requirements for the computer can be found on the label affixed to<br />

the bottom of the computer, or in the computer manual which can be found on<br />

the computer CD.<br />

Place the QuickTrace M-<strong>7600</strong> within 1.2 meters of a standard power outlet.<br />

Ensure that you position the analyzer so that the location where the power<br />

supply cord plugs into it is easily accessible (is not blocked) and it can be<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 2: Preparing for Installation<br />

quickly disconnected if needed. In case of hazard, the analyzer should be<br />

disconnected from the power source.<br />

Three power outlets may be required, one each for the QuickTrace M-<strong>7600</strong><br />

mercury analyzer, computer, and monitor. (An AC surge protected power strip<br />

with six or more outlets will suffice).<br />

The supplied power cord meets the requirements of the country where the<br />

instrument was purchased. If the instrument is to be used in a country other<br />

than the one specified at the time of ordering, obtain a new power cord set that<br />

meets the requirements of that country.<br />

WARNING<br />

SHOCK HAZARD<br />

This equipment is designed for connection to a grounded (earthed) outlet.<br />

The grounding type plug is an important safety feature. For continued<br />

protection against electrical shock or damage to the instrument, do not<br />

disable this feature.<br />

Do not apply power to the power supply until ready to operate the analyzer.<br />

Unpacking the <strong>Mercury</strong> <strong>Analyzer</strong><br />

Inspect external packaging upon receipt for signs of shipping damage. Inspect<br />

all items during unpacking and notify the carrier immediately of any concealed<br />

damage.<br />

If the system is shipped or removed from storage during cold weather, allow<br />

the packaged equipment to equilibrate to room temperature before opening<br />

and exposing to warm, humid air. It is usually sufficient to provide four to eight<br />

hours for this purpose.<br />

CAUTION<br />

EQUIPMENT DAMAGE FROM CONDENSATION<br />

If condensation forms on or inside the analyzer, allow it to dry thoroughly before<br />

connecting it to a power source and operating it. Failure to do so may cause<br />

equipment damage.<br />

1 Remove the packing checklist from the shipping container, and check off items<br />

against it. Leave accessories in the packing until you are ready to install them.<br />

NOTE<br />

Keep the factory packaging for use in case the product ever needs to be<br />

returned or shipped to another location.<br />

2 Open the box which contains the M-<strong>7600</strong>.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 2: Preparing for Installation<br />

3 Remove the upper piece of foam.<br />

Figure 2-5<br />

Opening the Box and Removing the Packaging.<br />

4 Ask an assistant to help you lift the M-<strong>7600</strong> from the box.<br />

WARNING<br />

LIFTING HAZARD<br />

Two people are required to lift the M-<strong>7600</strong> when it is in an awkward<br />

position such as in its box. Lifting should be done with a person situated on<br />

either end of the instrument.<br />

Figure 2-6<br />

Lifting the M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong>.<br />

22


<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 2: Preparing for Installation<br />

5 Remove the piece of foam from inside the door of the M-<strong>7600</strong>.<br />

Figure 2-7<br />

Removing Foam from the Door.<br />

6 Store the packaging in case you need to ship the mercury analyzer in the<br />

future.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 2: Preparing for Installation<br />

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24


3 Installing the <strong>Analyzer</strong><br />

Installation Overview<br />

Figure 3-1<br />

Front View of QuickTrace M-<strong>7600</strong> with Autosampler.<br />

Figure 3-2<br />

Rear View of QuickTrace M-<strong>7600</strong> with Autosampler.<br />

25


Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Step 1: Position the <strong>Mercury</strong> <strong>Analyzer</strong> and<br />

Autosampler<br />

1 Position the mercury analyzer.<br />

Keep in mind the factors listed in “Choosing a Location” on page 18. You will<br />

need easy access to the back of the analyzer as you make the connections.<br />

2 Place the autosampler next to the QuickTrace M-<strong>7600</strong> mercury analyzer.<br />

Leave a 1-centimeter gap so that vibration from the autosampler will not be<br />

transmitted directly to the mercury analyzer, and to facilitate passage of<br />

tubing.<br />

Step 2: Connect the Autosampler Peristaltic Pump to<br />

the Rinse Station<br />

It is easiest to connect the rinse station tubing to the autosampler's built-in<br />

peristaltic pump before other cables and tubing get in the way.<br />

In most cases, rinse solution will be “recycled” by returning it to the rinse<br />

solution bottle. If necessary, rinse solution can be pulled from a fresh bottle<br />

and used solution returned to a waste container.<br />

Note that rinse solution flows up through the rinse station.<br />

Rinse Drain Port<br />

Rinse Intake Port<br />

Figure 3-3<br />

Autosampler Rinse Station.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

1 The tubing from the output of the pump to the rinse station intake port is preconnected<br />

at the factory.<br />

Figure 3-4<br />

Pump Output to Rinse Intake Port.<br />

2 Locate in the completion kit the 6 mm (¼") OD Tygon ® tubing. The tubing will<br />

need to be cut to the appropriate lengths.<br />

3 Cut a 38 cm (15") length of tubing. This will run between the drain port of the<br />

rinse station and the rinse input of the peristaltic pump.<br />

4 Connect one end to the input of the outer pump channel.<br />

The pump rotates counterclockwise, so the inputs are on the top and the<br />

outputs are on the bottom.<br />

Figure 3-5<br />

Pump Input Connection from Rinse Drain.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

5 Connect the other end to the drain of the rinse station.<br />

Remove the rinse station and press the tubing very firmly so that it completely<br />

covers the barb of the fitting. It helps to use your other hand to apply counterpressure.<br />

Figure 3-6<br />

Rinse Station Drain Connection.<br />

Figure 3-7<br />

Replacing the Rinse Station.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Figure 3-8<br />

Rinse Station in Place.<br />

6 Cut an approximately 102 cm (40 inch) length of tubing to connect the input of<br />

the pump to the bottle of rinse solution. The tubing should be long enough to<br />

reach the bottom of the rinse bottle. This tube will draw rinse solution from<br />

the bottle.<br />

7 Connect one end of this tube to the remaining input channel of the pump.<br />

Figure 3-9<br />

Pump Input Connection.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

8 Cut an approximately 86 cm (34 inch) length of tubing to extend from the<br />

remaining pump output to the bottle of rinse solution. The tubing should<br />

extend a few inches inside the rinse bottle, but should remain above the liquid<br />

surface. This is the rinse solution drain tube.<br />

Figure 3-10<br />

Pump Output Connection and Liquid Flow Direction.<br />

WARNING<br />

SHOCK HAZARD<br />

In the steps which follow, pay attention to keep the tubing below all of the<br />

wires. Move the tubing, if necessary, so that any leaking liquid will not be<br />

directed onto electrical cables or connectors.<br />

Step 3: Set Up the Autosampler<br />

WARNING<br />

Ensure the power cord is not connected before proceeding with<br />

installation.<br />

See the Autosampler Operator’s <strong>Manual</strong>, included on the CD, for additional<br />

instructions and safety information. You may also refer to the printed Z-Drive<br />

Assembly Quick Installation Guide which comes with the autosampler for more<br />

information on installing the Z-drive assembly.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

The Z-drive is driven by a length of cable (line) which is made of solid Nylon<br />

101 (or in some cases, PEEK.)<br />

CAUTION<br />

Do not allow the cable to bend sharply. Avoid pushing up on the slider or pushing<br />

on the Z-drive cable.<br />

CAUTION<br />

Do not tighten the thumbscrews with anything other than your fingers.<br />

1 Locate the Z-drive assembly.<br />

Sleeve (Protects<br />

Z-Drive Cable)<br />

Sample Tube<br />

Z-Axis Slider<br />

Guide Block<br />

Y-Axis Slider<br />

Z-Drive Cable<br />

Sample Probe<br />

Home flag<br />

Figure 3-11 Z-Drive Assembly (Appearance May Vary Slightly Depending on<br />

Autosampler Model).<br />

2 Slide the Z-drive assembly onto the autosampler arm.<br />

Figure 3-12 Sliding the Z-Drive Onto the Arm of the Autosampler.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

3 Slide the Z-drive assembly onto the Y-axis leadscrew nut (the black block<br />

which moves back and forth along the arm). Lift the bushings with your<br />

fingernails to get them over the edge of the leadscrew nut.<br />

Figure 3-13 Lifting the Bushings Over the Edge of the Leadscrew Nut.<br />

4 Secure the Z-drive assembly to the Y-axis leadscrew nut by tightening the<br />

thumbscrews with your fingers. Never use tools to tighten the thumbscrews.<br />

Figure 3-14<br />

Tightening the Thumbscrews.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

5 Slide the cable onto the rotor on the back of the autosampler (Figure 6).<br />

Figure 3-15 Sliding Z-Drive Cable into Rotor Groove.<br />

6 Secure the guide block to the back of the autosampler with 2 black-capped<br />

thumbscrews (Figure 7). Note that it is important to install the guide block in<br />

the correct orientation.<br />

Figure 3-16 Securing Block to Back of Autosampler.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

7 Turn the rotor clockwise as far as it will go. This will raise the Z-drive to its<br />

highest position. (To avoid damaging the drive cable, always raise or lower the<br />

Z-drive by moving the rotor, rather than by pushing or pulling on the Z-drive<br />

itself.)<br />

Rotor Pin<br />

Stator Stop<br />

Figure 3-17<br />

View of Rotor with Z-Drive at Highest Position.<br />

8 Gently move the Z-axis slider until the gap between the slider and cap is<br />

approximately 2 mm (3/32").<br />

With the Z-drive in its highest position, there should be a gap between the Z-<br />

axis slider and the top cap of the Z-drive of approximately 2 mm (~ 3/32 inch).<br />

If this is not the case, see the Autosampler <strong>Operator's</strong> <strong>Manual</strong> for instructions<br />

on how to adjust the Z-drive travel.<br />

2 mm (3/32”)<br />

Figure 3-18<br />

View of Gap Between Probe Bracket and Cap.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

9 Hold the cable flat against the rotor and secure the cable by tightening<br />

thumbscrew on the rotor. Maintain the 2 mm (~ 3/32 inch) gap while the rotor<br />

pin is making contact with the stator stop (full clockwise rotation of rotor).<br />

The thumbscrew should be as tight as possible using just your fingers.<br />

Figure 3-19<br />

Securing Cable to Rotor.<br />

10 Rotate the rotor back and forth to ensure that it moves freely. Ensure that the<br />

full width of the cable is under the clamp.<br />

Clamp<br />

Figure 3-20<br />

Verifying Cable Movement and Cable Clamp.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

11 Insert the clamp into the slot in the Z-drive. Slide the probe into the Z-drive,<br />

through the hole in the clamp, and tighten the clamp with your fingers.<br />

Figure 3-21<br />

Tightening the Clamp Which Holds the Probe to the Z-Drive.<br />

If the clamp doesn't tighten enough to hold the probe in place, reverse the<br />

orientation of the knurled nut:<br />

Threads Visible<br />

Lip Without Threads<br />

Hole for Sample Probe<br />

Figure 3-22<br />

Clamp Oriented Correctly.<br />

12 Loosen the clamp and adjust the position of the probe so that it is about 2 mm<br />

(3/32 inch) above the top of the rinse station when the Z-drive is in its highest<br />

position.<br />

You can use a large coin, such as a U.S. quarter, to help measure this gap. The<br />

exact distance is not critical, but the probe needs to be high enough that it will<br />

not hit anything when it moves from place to place.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

2 mm<br />

Figure 3-23<br />

Probe Position with Z-Drive in Highest Position.<br />

13 Center the probe over the rinse station and rotate the rotor counterclockwise<br />

to lower the probe into the rinse station.<br />

14 Use the provided spiral wrap to secure the sample tube to the Z-drive cable<br />

about 5 cm (2 inches) above the top of the Z-drive. There should be just a little<br />

curve to the free sample tube when the probe is lowered, and a loop when the<br />

probe is raised.<br />

The sample tube should naturally curve away from the probe so that it won't<br />

rub or get caught. If necessary, loosen the probe and rotate it so that the<br />

sample tube looks like the pictures below:<br />

Spiral Wrap<br />

Slight Curve<br />

Away from<br />

Probe<br />

Loop<br />

Figure 3-24<br />

Securing the Sample Tube.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

15 Use the other spiral wrap to secure the sample tube to the cable at its highest<br />

point.<br />

Figure 3-25<br />

Securing the Sample Tube.<br />

16 Moisten a Kimwipes ® wiper with 10% HNO 3 and wipe the probe to remove any<br />

oil. This is needed so that aqueous samples do not adhere to the probe causing<br />

sample-to-sample contamination or rinse contamination.<br />

17 The Z-drive assembly and sample probe are now properly installed on the<br />

autosampler.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Step 4: Connect Power and Data Cables to the Back<br />

of the <strong>Mercury</strong> <strong>Analyzer</strong><br />

1 Locate the plastic shipping bag labeled “Completion Kit – QuickTrace M-<br />

<strong>7600</strong>.” It contains various power and data cables, small parts, tubing, fittings,<br />

computer CD-ROM, etc.<br />

You will be locating supplies from in kit for throughout the installation process.<br />

It is recommended to leave the parts in this bag, in their original packaging,<br />

until you need them.<br />

2 Place the autosampler power switch in the OFF position.<br />

3 Place the mercury analyzer power switch in the OFF position.<br />

M-<strong>7600</strong><br />

Power Switch<br />

Figure 3-26<br />

Power Switch<br />

4 Connect the line cord to the connector on the back of the mercury analyzer.<br />

If the cord is not of the correct type for your country, contact <strong>CETAC</strong><br />

Technologies. See “Power Cord Set Requirements” on page 151.<br />

Figure 3-27<br />

Power Cord Connected to <strong>Mercury</strong> <strong>Analyzer</strong><br />

5 Connect the power cord into a grounded surge protected power strip.<br />

6 Plug the surge protected power strip into the AC outlet receptacle.<br />

Do not turn on the power switches yet.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

7 Connect the 5-pin end of the autosampler power cable to the back of the<br />

mercury analyzer.<br />

Figure 3-28<br />

Autosampler Power Cable Connected to <strong>Mercury</strong> <strong>Analyzer</strong>.<br />

8 Plug one end of the Ethernet cable into the mercury analyzer.<br />

Figure 3-29<br />

Ethernet Cable Connected to <strong>Mercury</strong> <strong>Analyzer</strong>.<br />

Step 5: Connect the Carrier Gas Tubing<br />

1 In the completion kit bag, find the brass 2-micron gas filter, with associated<br />

brass Swagelok fittings, and a short section of ETFE tubing (attached to the<br />

filter).<br />

2 Determine how far the QuickTrace M-<strong>7600</strong> is located from the gas supply<br />

(UHP nitrogen or argon). Allow a generous service loop of 1/8" nylon tubing<br />

from the roll provided the likely event of system placement changes or<br />

maintenance. This will allow the system to be slid forward for cell maintenance<br />

without disconnecting the gas tubes.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

3 Connect one end of this tube to the gas inlet side of the 2-micron brass filter<br />

and tighten the Swagelok fitting securely.<br />

Figure 3-30<br />

Completed Assembly of Gas Inlet Tubing with Filter.<br />

NOTE:<br />

A 2-micron in-line filter must always be used. The 2-micron filter has been<br />

selected for minimal pressure drop and minimal flow fluctuation. Do not<br />

substitute other filters.<br />

4 Connect the ETFE tube into the bulkhead fitting labeled “GAS INLET.” Make<br />

sure that the flow arrow on the gas filter is pointing in the direction to the gas<br />

in fitting.<br />

Tighten the fitting as tight as you can get it using your fingers. (This fitting<br />

needs to be very secure, but do not use pliers to tighten it.)<br />

Figure 3-31<br />

Carrier Gas Inlet Tubing Connected to <strong>Mercury</strong> <strong>Analyzer</strong>.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

5 Connect the other end of the nylon tube to the gas supply regulator, using ¼"<br />

NPT 1/8" Swagelok fitting provided.<br />

CAUTION<br />

Exceeding 825 kPa (120 psig) gas supply pressure to the QuickTrace M-<strong>7600</strong> may<br />

rupture the bulkhead fittings, causing the unit to malfunction.<br />

CAUTION<br />

Use only “research-grade”, “dry” UHP Nitrogen or Argon. Do not use “welding”<br />

grade gases - these may permanently damage the QuickTrace M-<strong>7600</strong>.<br />

Step 6: Install the <strong>Mercury</strong> Trap (KMnO4)<br />

A tube filled with crystalline potassium permanganate will serve as the<br />

mercury vapor trap. The vapor trap will clean the QuickTrace M-<strong>7600</strong><br />

exhaust vapors, to prevent the release of mercury vapor into the lab<br />

atmosphere.<br />

WARNING<br />

INHALATION HAZARD<br />

Do not operate the mercury analyzer unless the mercury trap is in place<br />

and functioning correctly.<br />

1 In the plastic bag labeled “Completion Kit - QuickTrace M-<strong>7600</strong>,” find the<br />

polyethylene tube with a seven inch (17.8 cm) length of dark Viton ® tubing<br />

attached to one end.<br />

2 Remove one end cap from the polyethylene tubular body. Do NOT remove the<br />

heatshrink wrapped Luer fitting from the end cap.<br />

3 Inspect both end cap interiors to ensure that the ends are lightly plugged with<br />

fine glass wool. If not, lightly pack a small, loose wad of fine glass wool into the<br />

small i.d. section of each cap. Pack enough glass wool to stop the potassium<br />

permanganate from filtering through, but not restrict the gas flow.<br />

4 Put on protective eyewear and gloves.<br />

5 With the glass wool in place, use a powder funnel to fill this tube with dry<br />

crystalline solid potassium permanganate (KMnO 4). While filling, have one end<br />

fully capped, hold the other end straight upward, and use the powder funnel to<br />

guide the KMnO 4 crystals into the tube. Fill to the top, tapping a finger lightly<br />

on the tube to settle the KMnO 4, and finally place the end cap on securely.<br />

WARNING<br />

CHEMICAL BURN HAZARD<br />

Be sure to wear protective eyewear and safety gloves when handling<br />

chemicals.<br />

6 Snap the filled mercury trap into the black holders.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

7 Attach the black Viton ® tube with fitting to the connection labeled “GAS<br />

EXHAUST.”<br />

Figure 3-32<br />

KMnO 4 Absorbent Trap Connected to <strong>Mercury</strong> <strong>Analyzer</strong>.<br />

The mercury vapor trap needs to be cleaned and refilled when the brown color<br />

approaches the open end. This is the formation the MnO 2 as the KMnO 4 is<br />

reduced. The potassium permanganate may last at least one year depending on<br />

frequency of use, except in the unlikely event of a major overflow accident in<br />

the QuickTrace M-<strong>7600</strong>.<br />

NOTE<br />

So long as the KMnO 4 is dry, free flowing (not caked), dark purple crystals, it is<br />

perfectly OK.<br />

WARNING<br />

POISON HAZARD<br />

The mercury vapor trap contains potassium permanganate (KMnO 4 ) and<br />

may contain mercury. Handle and dispose of the used KMnO 4 according to<br />

your laboratory’s procedures and your country’s hazardous waste<br />

regulations.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Step 7: Connect the Back of the Autosampler<br />

1 Connect one end of the USB cable to the autosampler.<br />

Figure 3-33<br />

USB Cable Connected to Autosampler.<br />

2 Connect the power cable to the autosampler.<br />

This is the cable which was connected in step 7 on page 40. The autosampler<br />

will be powered by the automatic switching power supply within the M-<strong>7600</strong>.<br />

Figure 3-34<br />

Power Cable Connected to Autosampler.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Step 8: Connect to the Host Computer<br />

The <strong>CETAC</strong> M-<strong>7600</strong> mercury analyzer is controlled by a PC through an<br />

Ethernet connection.<br />

<strong>CETAC</strong> recommends that this PC be equipped with two network cards. One<br />

card is used for communication with your laboratory network, and the other<br />

card is used exclusively for communication with the M-<strong>7600</strong> mercury analyzer.<br />

In most cases, a PC is supplied with the mercury analyzer, and this PC has two<br />

network cards.<br />

NOTE<br />

In most cases, <strong>CETAC</strong> will pre-configure the network cards for your laboratory.<br />

If you were not able to supply the necessary network information to <strong>CETAC</strong>, or<br />

if you will be supplying your own PC, then set up the network cards yourself as<br />

described below. If the PC is already set up, skip to “Step 9: Install the Gas-<br />

Liquid Separator (GLS)” on page 53.<br />

If you wish to use a laptop computer or if you cannot install a secondary<br />

network card, see “Connecting a Laptop Computer to the M-<strong>7600</strong>” on page 52.<br />

The information in this section is also supplied in the <strong>CETAC</strong> M-<strong>7600</strong> <strong>Mercury</strong><br />

<strong>Analyzer</strong> PC Setup Guide which is included with the mercury analyzer.<br />

Summary<br />

Primary NIC<br />

Secondary NIC<br />

Connects to Laboratory network 192.168.0.149 (address of the M-<strong>7600</strong>)<br />

Interface Metric 100 2<br />

Default IP Address Obtain automatically 192.168.0.100 (address of the PC)<br />

Installing a Secondary NIC in Your Own PC<br />

Most PC’s come with a single network interface, but a secondary network<br />

interface card (NIC) can easily be installed in most desktop and tower PCs. To<br />

install the second NIC:<br />

1 Power off the PC.<br />

2 Install secondary network interface card (NIC), following the manufacturer's<br />

instructions.<br />

You will need to set a static IP address for this card, as shown on page 50.<br />

3 Install all of the PC peripherals such as the keyboard, mouse, and monitor.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Connecting the Communication Cables<br />

Power Cord<br />

Keyboard and<br />

Mouse<br />

Monitor (Cable<br />

Not Shown)<br />

Figure 3-35<br />

PC Before Connection to the M-<strong>7600</strong>.<br />

1 Connect the USB cable from the autosampler to the computer.<br />

2 Connect the Ethernet cable from the mercury analyzer to the computer.<br />

USB to Autosampler<br />

Ethernet to M-<strong>7600</strong><br />

Figure 3-36<br />

PC After Connection to the M-<strong>7600</strong>.<br />

Configuring the Network Metrics<br />

The network metrics for each NIC on the PC must be configured for optimal<br />

communications with the M-<strong>7600</strong> mercury analyzer.<br />

These instructions apply to the Microsoft Windows 7 and Windows XP<br />

operating systems.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

1 Power on the PC.<br />

2 Open the network connection dialog.<br />

WINDOWS 7:<br />

a) Open the Control Panel.<br />

b) Click Network and Internet | View network status and tasks.<br />

Figure 3-37 Network and Internet Settings (Windows 7).<br />

WINDOWS XP:<br />

a) Click Start > Control Panel.<br />

b) Click Network Connections.<br />

You should see two active networks (one for each card.).<br />

3 For each card, click the connection link (circled in red below).<br />

(WINDOWS XP: double-click the connection link.)<br />

Note: The network card connected to the M-<strong>7600</strong> will show No Internet<br />

Access, and probably show up as either an M-<strong>7600</strong> (if preconfigured by<br />

<strong>CETAC</strong>) or otherwise as an unidentified network, as seen in Figure 3-38.<br />

Figure 3-38 Network Connection Dialog for Windows 7.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

4 Click Properties.<br />

Figure 3-39<br />

Network Connection Properties Button.<br />

5 Select ‘Internet Protocol Version 4’ and click ‘Properties’.<br />

Figure 3-40<br />

IPv4 Properties Button.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

6 Click ‘Advanced’<br />

Figure 3-41<br />

IPv4 Advanced Button.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

7 Deselect ‘Automatic metric’ (see circled area in the image below), and specify a<br />

metric number. Specify ‘2’ for the card connected to the M-<strong>7600</strong> and ‘100’ for<br />

the card connected to the local area network.<br />

Figure 3-42<br />

Interface Metric for the M-<strong>7600</strong>.<br />

Setting the IP Address for the Secondary NIC<br />

If the PC was purchased from <strong>CETAC</strong>, it will be preconfigured to use an IP<br />

address of 192.168.0.149 for the M-<strong>7600</strong> mercury analyzer. In most cases, this<br />

address will work. If this address causes a conflict (for example, if the<br />

laboratory subnet is 192.168.0.*), or if you are configuring a secondary NIC in<br />

a PC not supplied by <strong>CETAC</strong>, set the address as follows:<br />

1 Choose an IP address for the secondary NIC.<br />

Choose an address that does not conflict with anything in use on the<br />

laboratory/company Local Area Network (LAN).<br />

Use a standard Ethernet cable to connect the secondary NIC directly to the M-<br />

<strong>7600</strong>. If there is any doubt about IP number conflict consult your network<br />

administrator.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

PC’s purchased from <strong>CETAC</strong> will come preconfigured in such a way that a<br />

conflict is unlikely, but reconfiguration may be required (the default IP address<br />

of the M-<strong>7600</strong> analyzer is 192.168.0.149.) If for example the subnet used in the<br />

lab consists of 192.168.0.*, then the secondary NIC could be configured to<br />

192.168.10.x allowing it to communicate with an analyzer configured to<br />

192.168.10.y, without conflicting with another device on the LAN.<br />

Ideally the secondary NIC can be configured to be on a subnet compatible with<br />

the M-<strong>7600</strong> default (i.e.192.168.0.*) and used. If this configuration is not<br />

acceptable for laboratory operation, see the next section.<br />

2 In the Internet Protocol version 4 properties dialog (pictured below) select<br />

‘Use the following IP address’, and specify a number on a subnet different than<br />

that used in your laboratory. Unless your network administrator indicates<br />

otherwise, the subnet mask should be 255.255.255.0, and the gateway, and<br />

DNS server can be left blank because they will not be used.<br />

Figure 3-43<br />

Setting the IP Address<br />

Changing the Subnet of the <strong>Mercury</strong> <strong>Analyzer</strong><br />

Ideally the secondary NIC can be configured to be on a subnet compatible with<br />

the M-<strong>7600</strong> default (192.168.0.*). If this configuration is not acceptable for<br />

laboratory operation, then the IP address used by theM-<strong>7600</strong> will need to be<br />

configured as described in the <strong>CETAC</strong> M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong> PC Setup Guide<br />

which is included with the mercury analyzer.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Connecting a Laptop Computer to the M-<strong>7600</strong><br />

Since a secondary network interface card cannot be installed in most laptop<br />

computers, an alternate configuration must be used.<br />

Option 1: Use a USB to TCP/IP Converter<br />

The easiest solution is to use a USB-to-TCP/IP converter (also called a USB<br />

LAN adapter). This converter will behave just like a secondary network<br />

interface card.<br />

Option 2: Use an Isolated Network<br />

If you don't need to connect the laptop to another network (including the<br />

laboratory network or the Internet), you can set up the network to<br />

communicate only with the M-<strong>7600</strong>. Set up the M-<strong>7600</strong> using the instructions<br />

for the secondary network card. Use an alternate means of communication,<br />

such as a flash drive or a USB connection, to transfer files and print results.<br />

Option 3: Use an Unallocated IP Address on the Network<br />

If your network uses static IP addresses, allocate a new address for the M-<br />

<strong>7600</strong>. If your network is managed by a network administrator or information<br />

technology professional, it is strongly recommended to ask that person to<br />

assign the address.<br />

If your network uses dynamic IP addresses (DHCP), it is usually possible to<br />

assign a static address to the M-<strong>7600</strong> while the other devices on the network<br />

continue to use DHCP. In this case, you must find a static address for the<br />

M-<strong>7600</strong> which will not conflict with other devices on the network. On many<br />

network routers, the DHCP IP addresses are restricted to a certain range. Note<br />

that this address range can be changed, so it is important to go into the<br />

router's configuration interface to verify the range. Choose an IP address above<br />

the address used by the router but below the DHCP range.<br />

For example, if the router is configured like this:<br />

Local IP Address: 192.168.1.1<br />

Subnet Mask: 255.255.255.0<br />

DHCP Starting IP Address: 192.168.1.100<br />

and if there are no other devices on the network with static IP addresses, then<br />

you can configure the M-<strong>7600</strong> to use:<br />

M-<strong>7600</strong> IP Address: 192.168.1.2<br />

M-<strong>7600</strong> Net Mask: 255.255.255.0<br />

M-<strong>7600</strong> Gateway: 192.168.1.1<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Step 9: Install the Gas-Liquid Separator (GLS)<br />

WARNING<br />

HANDLE WITH CARE<br />

Use care when handling the GLS. If the GLS breaks, there is a risk of cut<br />

from broken glass.<br />

Use only your fingers to tighten the fittings.<br />

1 Locate the gas-liquid separator (GLS).<br />

Liquid Mix (In)<br />

Gas Supply (In)<br />

Hg Vapor (Out, not<br />

connected until just<br />

before use)<br />

Drain (Out)<br />

Figure 3-44<br />

Gas-Liquid Separator (GLS).<br />

2 Locate the gas-liquid separator (GLS) and gently slide it into the holder with<br />

the drain and Hg vapor ports facing you. Raise it as far as it will go.<br />

Figure 3-45<br />

Placing the GLS.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

3 Rotate the GLS so that the ports face to the right and gently tighten the<br />

thumbscrew to temporarily hold it in position.<br />

Figure 3-46<br />

Tightening the GLS Thumbscrew.<br />

4 Locate the drip block in the completion kit and lower the drip block into place.<br />

The drip block slides over the pegs below the GLS.<br />

Figure 3-47<br />

Positioning the GLS drip block.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

5 Loosen the thumbscrew and lower the GLS into its final position, then gently<br />

tighten the thumbscrew. There should be space for the drain tube from the GLS<br />

to pass through the notch in the side of the drip tray.<br />

Figure 3-48<br />

Bottom of GLS.<br />

6 Route the liquid mix tube to the top of the GLS through the guides on the front<br />

of the mercury analyzer.<br />

Figure 3-49 Routing the Liquid Mix Tube to the GLS (view 1).<br />

Figure 3-50 Routing the Liquid Mix Tube to the GLS (view 2).<br />

55


Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

7 Connect the tube from the bottom of the GLS to the GLS SUPPLY fitting.<br />

Figure 3-51<br />

Ready to Connect the Gas Supply to the GLS.<br />

Figure 3-52<br />

Completed GLS Installation.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Step 10: Connect the Peristaltic Pump on the<br />

<strong>Mercury</strong> <strong>Analyzer</strong><br />

Figure 3-53<br />

Connected.<br />

Peristaltic Pump on the <strong>Mercury</strong> <strong>Analyzer</strong> After Tubing is<br />

Installing the Peristaltic Pump Tubing<br />

1 Release all four peristaltic pump channel clamps.<br />

2 Locate the peristaltic pump tubing in the completion kit. There are two sets of<br />

pump tubing.<br />

‣ The tubes with the yellow stops are for the sample and drain channels.<br />

‣ The tubes with the black stops are for the reagent channel.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

3 Using both hands, stretch a tube with yellow stops across channel 1, closest to<br />

the body of the M-<strong>7600</strong>. Keep the tension even between the two sides and<br />

insert the stops into the slots.<br />

Pressure Shoe<br />

Adjustable Clamp<br />

Roller Head<br />

Stop<br />

4 Install two more tubes with yellow stops, one in channel 2 and the second in<br />

channel 3, then one tube with black stops in channel 4.<br />

Note that the roller head moves clockwise.<br />

Inlet Side<br />

Figure 3-54<br />

Outlet Side<br />

Peristaltic Pump Tubing (Viewed from Front).<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Channel 1 2 3 4<br />

Yellow<br />

Black<br />

Inlet Side<br />

Figure 3-55<br />

Outlet Side<br />

Peristaltic Pump Tubing (Viewed from Left and Right Sides).<br />

Installing the Mixing Tee and Drain Tees<br />

1 Locate the larger (3/32" dia.) polypropylene tee fittings provided in the<br />

completion kit. Install these tees on either side of the back two channels<br />

(channel 1 and channel 2) of the pump.<br />

Large Tee<br />

Large Tee<br />

Figure 3-56<br />

Large Tee Fittings (Tubing removed from Ch 3-4 for clarity).<br />

2 In the completion kit, locate the 91 cm (three-foot) waste tube. Connect the tee<br />

on the right (outlet) side to the waste tube (1/8" o.d. Tygon ® tubing).<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

3 Connect the tee on the left (inlet) side to the drain tube coming from the GLS.<br />

Drain Tube<br />

Figure 3-57<br />

GLS Drain Tube.<br />

From Drain<br />

To Waste<br />

Figure 3-58<br />

Waste and Drain Connections.<br />

4 Find a Luer male barbed fitting (look for this in the 10 liter waste container).<br />

Replace one of the Luer caps on the waste container lid with the barbed fitting.<br />

Attach the other end of the waste tube to this fitting.<br />

To prevent pressure buildup in the 10-liter waste container, be sure that at<br />

least one of the two vents on the 10-liter waste container are open (uncapped)<br />

during operation.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

5 Route the 1/16" Teflon ® sample tube from the autosampler through the guide<br />

at the top of the mercury analyzer, then through the guide at the bottom.<br />

Trim the sample tube if necessary. This may be necessary with an ASX-260 or<br />

ASX-130 autosampler. Be careful to leave enough slack in the tube so that the<br />

sample probe is able to freely move to the most distant position without<br />

stretching or kinking the tube. On the other hand, if the sample tube is too long<br />

it can tangle, and a longer tube will require more time to transport the sample<br />

and more time to thoroughly rinse between samples.<br />

Figure 3-59<br />

Attaching the Sample Tube to the Side of the M-<strong>7600</strong>.<br />

6 Connect the sample tube to the inlet side of channel 3.<br />

From<br />

Sample<br />

Probe<br />

Figure 3-60<br />

Sample Probe Connection.<br />

7 Find the 23 inch (58 cm) length of 1/16" Teflon ® tubing inside the reagent<br />

bottle. This is the reagent uptake tube.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

8 Connect the reagent uptake tube to the inlet side of channel number four.<br />

When in use, to ensure that no precipitated solids are pumped through the<br />

system, the reagent tube should not touch the bottom of the reagent bottle.<br />

Reagent Uptake Tube<br />

(From Reagent Bottle)<br />

From Sample Probe<br />

Figure 3-61<br />

Reagent Connection.<br />

9 Locate the smallest (1/16" dia.) polypropylene tee provided in the completion<br />

kit. Install this tee on the output side of the pump. It connects the top two<br />

channels (channels 3 and 4).<br />

Liquid Mix<br />

Tube<br />

Figure 3-62<br />

Small Tee Fitting on Ch 3/4 Outputs.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

10 Connect the Liquid Mix tube to the small tee which you just installed.<br />

The Liquid Mix tube is a black tube which connects to the GLS, as shown in<br />

Figure 3-50 on page 55.<br />

Liquid Mix<br />

Tube<br />

Figure 3-63<br />

Liquid Mix Connection.<br />

Step 11: Power On and Verify Communication<br />

Once installation of the QuickTrace M-<strong>7600</strong> system is complete, it is<br />

important to verify that the system is installed correctly.<br />

CAUTION<br />

Attempting to use the QuickTrace M-<strong>7600</strong> before ensuring that all components<br />

are installed correctly may result in damage to the system.<br />

To Configure the Network Connection<br />

The <strong>CETAC</strong> M-<strong>7600</strong> mercury analyzer is controlled by a PC. <strong>CETAC</strong><br />

recommends that this PC be equipped with two network cards. One card is<br />

used for communication with your laboratory network, and the other card is<br />

used exclusively for communication with the M-<strong>7600</strong> mercury analyzer.<br />

In most cases, a PC is supplied with the mercury analyzer, and this PC has two<br />

network cards.<br />

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Chapter 3: Installing the <strong>Analyzer</strong><br />

NOTE<br />

In most cases, <strong>CETAC</strong> will pre-configure the network cards for your laboratory.<br />

If you were not able to supply the necessary network information to <strong>CETAC</strong>, or<br />

if you will be supplying your own PC, then you will need to set up the network<br />

cards yourself as described in this document.<br />

Refer to the M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong> PC Setup Guide and the QuickTrace<br />

Software <strong>Manual</strong> for instructions on how to configure the network settings on<br />

the PC and on the M-<strong>7600</strong>.<br />

To Power On the System for the First Time (PC Configured by<br />

<strong>CETAC</strong>)<br />

CAUTION<br />

When you turn off the QuickTrace M-<strong>7600</strong>, wait at least 15 seconds before<br />

turning it back on. Rapidly cycling power can cause the optical monitoring<br />

feedback system electronics to temporarily malfunction, potentially resulting in an<br />

optical performance error.<br />

1 Power on the PC, QuickTrace M-<strong>7600</strong> mercury analyzer, and the autosampler.<br />

2 Check to ensure that the communication cables are properly connected.<br />

3 Start the QuickTrace software.<br />

4 When the software is initializing, it will test the connections to the<br />

QuickTrace M-<strong>7600</strong> mercury analyzer and the autosampler.<br />

The QuickTrace M-<strong>7600</strong> software runs a test routine at startup to test the<br />

various interfaces throughout the system. The software will give a report on<br />

the status of the interface if there is a failure.<br />

To Power On the System for the First Time (Customer-<br />

Supplied PC)<br />

If you are supplying your own PC, you will need to set up drivers to<br />

communicate with the M-<strong>7600</strong> and the autosampler.<br />

CAUTION<br />

When you turn off the QuickTrace M-<strong>7600</strong>, wait at least 15 seconds before<br />

turning it back on. Rapidly cycling power can cause the optical monitoring<br />

feedback system electronics to temporarily malfunction, potentially resulting in an<br />

optical performance error.<br />

1 Power on the PC, QuickTrace M-<strong>7600</strong> mercury analyzer, and the autosampler.<br />

2 Check to ensure that the communication cables are properly connected.<br />

3 Run the USB device driver installation program. Navigate to<br />

C:\Program Files\QuickTrace\USB Drivers<br />

then double-click CDM2.02.04.<br />

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Chapter 3: Installing the <strong>Analyzer</strong><br />

4 Select All Programs | <strong>CETAC</strong> QuickTrace | Specify Installed Hardware.<br />

Figure 3-64<br />

Starting the Specify Installed Hardware Program.<br />

5 Select the M-<strong>7600</strong> analyzer.<br />

Figure 3-65<br />

Selecting the <strong>Analyzer</strong>.<br />

Once the M-<strong>7600</strong> is chosen the software will search the network for analyzers.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Figure 3-66<br />

Searching for the <strong>Analyzer</strong>s.<br />

6 When the search is complete, select the analyzer. The IP address and other<br />

communication parameters will be filled in automatically.<br />

Figure 3-67<br />

Selecting the <strong>Analyzer</strong>.<br />

7 Select the model of the autosampler you are using.<br />

66


<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Figure 3-68<br />

Selecting the Autosampler Model.<br />

8 Select the autosampler COM port.<br />

The autosampler is connected via USB, but the USB driver emulates a serial<br />

(COM) port. The driver automatically assigns a COM port number of COM3 or<br />

greater.<br />

Figure 3-69<br />

Selecting the Autosampler COM port.<br />

9 Start the QuickTrace software.<br />

10 When the software is initializing, it will test the connections to the<br />

QuickTrace M-<strong>7600</strong> mercury analyzer and the autosampler.<br />

The QuickTrace M-<strong>7600</strong> software runs a test routine at startup to test the<br />

various interfaces throughout the system. The software will give a report on<br />

the status of the interface if there is a failure.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

To Test the Autosampler<br />

1 In the QuickTrace software, click the Instrument Control button.<br />

Figure 3-70<br />

Instrument Control Button.<br />

2 Click the Autosampler button.<br />

Figure 3-71<br />

Autosampler Button.<br />

3 Click the buttons to turn the autosampler's peristaltic rinse pump on and off,<br />

move the probe (“sipper”) up and down, and move the probe to a sample vial<br />

and back.<br />

Refer to the QuickTrace software online help for more information on how to<br />

control the autosampler.<br />

Step 12: Fill the Rinse Solution Bottle<br />

1 Fill the rinse bottle with trace metal grade 1% HCl / 2% HNO 3 v/v.<br />

NOTE:<br />

When analyzing samples and standards of high concentration such as 20 ppb<br />

or greater use a stronger concentration of acid; such as 5% HCl / 2% HNO 3 or a<br />

similar mix but do not exceed 10% HNO 3 .<br />

2 Insert the rinse solution drain tube (from the autosampler rinse station drain<br />

port, via the peristaltic pump) about ¼ of the height of the rinse bottle.<br />

3 Insert the rinse solution supply tube (to the autosampler rinse station intake<br />

port, via the peristaltic pump) so that it is just above the bottom of the rinse<br />

bottle.<br />

The end of the drain tube must remain above the end of the supply tube.<br />

For help identifying the rinse solution drain and supply tubes, see Figure 3-10<br />

on page 30.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

Step 13: Fill the Reagent Bottle<br />

The reducing agent will be used with the QuickTrace M-<strong>7600</strong> system during<br />

operation of the system.<br />

The reducing agent is 10% SnCl 2 w/v (in 7% HCl v/v). To mix the reducing<br />

agent, perform the following steps under a hood:<br />

1 Add 100 g of SnCl 2 to the reagent bottle.<br />

2 Add 70 mL of trace metal HCl.<br />

3 Swirl and wait ~ 2 min or until SnCl 2 begins to dissolve.<br />

4 Add ~ 100 mL of DI water, swirl and wait ~ 2 min.<br />

5 Add ~ 100 mL of DI water, swirl and wait ~ 2 min.<br />

6 Fill with DI water to the shoulder of the rinse bottle.<br />

7 Cap until ready for use.<br />

Preserving the SnCl2<br />

‣ Cap the Luer fitting when not in use.<br />

‣ Refrigerate unused portions.<br />

NOTE<br />

All solutions must be room temperature prior to use.<br />

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Chapter 3: Installing the <strong>Analyzer</strong><br />

Step 14: Adjust the Peristaltic Pump Tubing Clamp<br />

Tension (Optional)<br />

The tension of the tubing in the mercury analyzer's built-in peristaltic pump<br />

affects how smoothly liquid will flow through the system.<br />

NOTE<br />

The clamps are preset at the factory to optimal tension. Perform the following<br />

steps only if you believe the clamps may need adjustment.<br />

1 Verify that the “11HG VAPOR12” tube is disconnected from the GLS vapor<br />

outlet.<br />

Figure 3-72<br />

Disconnecting the Hg Vapor Tube.<br />

2 Open the QuickTrace software.<br />

3 Open the QuickTrace hardware Controls (see the QuickTrace software manual)<br />

by clicking the Instrument button, or select Window|Instrument.<br />

Figure 3-73<br />

Instrument Control Button.<br />

4 With zero clamp tension on the tubing (screws nearly unscrewed), snap all<br />

four clamps into place and start the peristaltic pump.<br />

5 Set the gas pressure to 120 psi (825 kPa).<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

6 Set the analyzer gas flow to 100 mL/min.<br />

Figure 3-74<br />

Gas Flow Controls (Shown Before Setting to 100 mL/min.).<br />

CAUTION<br />

Read through steps 7-11 before proceeding. It is extremely important to set the<br />

peristaltic pump drain clamps in a timely fashion after the GLS begins to fill with<br />

liquid. Failing to do so can cause an overflow and spillage.<br />

WARNING<br />

CHEMICAL SPILL HAZARD<br />

Do not start liquid flow without the carrier gas being on and set to 100<br />

mL/min with and pressure set to 120 psi. Otherwise, fluid backfill can<br />

occur.<br />

Refer to the QuickTrace help or software manual for more information on<br />

instrument control.<br />

7 Place the autosampler sample probe into rinse station. Click the Up button,<br />

then the Park button. Visually verify the probe's movement.<br />

Figure 3-75<br />

Autosampler Button.<br />

8 Place a Kimwipes ® wiper at the GLS gas exit port to prevent any liquid from<br />

spilling onto the GLS mount.<br />

9 <strong>Manual</strong>ly increase the clamp tension on the Santoprene ® sample tubing<br />

(Channel three) until liquid uptake begins to flow with a jerky motion in the<br />

sample tube from the autosampler. Now rotate the tension screw ¼ turn past<br />

this point and verify that the flow is steady.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

10 Watch the liquid flow as it makes its way from the autosampler rinse station, to<br />

the pump, through the mixing tee, and to the Gas-Liquid Separator.<br />

The GLS will begin to fill with rinse solution.<br />

11 Increase the clamp tension on both of the drain tubing clamps (Channels one &<br />

two) until flow begins from the drain port of the GLS and the liquid level<br />

begins to drop.<br />

Do this quickly before the GLS fills to the point where fluid overflows the GLS.<br />

The GLS should slowly drain to empty, even though sample continues to be<br />

delivered to the top of the frosted center post. The GLS is intended to operate<br />

“empty” with only a thin film of liquid continuously wetting the frosted center<br />

post and exiting the drain.<br />

NOTE<br />

If GLS overflow occurs, the pump will stop. To restart the pump, simply click<br />

the Pump On button.<br />

12 Tighten both drain tube clamps equally to ensure even flow to each.<br />

Check this by observing the segmented flow at both drain tees. The rate of flow<br />

in and out should be balanced through both Santoprene drain tubes. Adjust the<br />

clamp tension to keep the GLS empty and to achieve a smooth, balanced,<br />

segmented flow. Unstable drain flow can cause baseline noise in the system.<br />

The drain tube tension should exactly match the sample flow tension.<br />

13 Start the SnCl 2 flow.<br />

‣ Place the SnCl 2 uptake tube in the reagent bottle<br />

‣ Close the Channel 4 clamp.<br />

‣ Increase the reagent clamp tension until reagent uptake begins in the tube.<br />

‣ Adjust the clamp so that the flow from the SnCl 2 bottle is smooth, with no<br />

jerks in the flow.<br />

14 Once liquid is running through the QuickTrace M-<strong>7600</strong>, note that the drain<br />

tubing clamp tension is properly adjusted by watching the flow through the<br />

Gas-Liquid Separator.<br />

The GLS should remain empty and liquid exiting the GLS should appear nearly<br />

motionless, with no flutter or instability.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

15 The flow into the GLS should be as smooth and pulse free as possible.<br />

View this closely at the top of the GLS frosted center post. The liquid should<br />

stream continuously from the capillary tip to the top of the post, and the liquid<br />

column spanning the gap between the capillary tip and post should be nearly<br />

“motionless,” with minimal fluctuation and no jerkiness or discontinuity. If this<br />

is not the case check that the “gap” between the bottom of the GLS capillary<br />

insert tube and the top of the GLS frosted center post is ~0.5 mm (range of 0.3-<br />

0.6 mm). If not, very carefully slide this insert up or down, as needed. Refine<br />

the clamp tension of the sample and reagent channels as needed to stabilize<br />

the liquid flow to the GLS.<br />

A flow check with a 10 mL graduated cylinder (less than 100 mm tall) and<br />

stopwatch should yield a sample uptake rate of ~15 mL/min, and a reagent<br />

uptake rate of ~5.7 mL/min. Check liquid flow stability at the drain exit of the<br />

GLS after final adjustments of clamp tension to sample and reagent pump<br />

tubing. The pump tension will not need further adjustments; do not adjust<br />

pump tension to compensate for worn pump tubing.<br />

NOTE:<br />

When properly adjusted the tension on the bottom three peristaltic pump<br />

tubes (channels 1-3) should be the same and the tension screw for the top<br />

pump tube (reagent tube, channel 1) should be screwed in 1 to 2 mm farther<br />

than the other channels.<br />

Step 15: Check the Reagent Flow<br />

1 Fill the 10 mL graduated cylinder with 10 mL DI water.<br />

2 Simultaneously place the reagent uptake tube in the graduated cylinder and<br />

start the stopwatch.<br />

3 After 30 seconds, remove the uptake tube from the cylinder.<br />

4 Measure the water remaining in the cylinder, and calculate the reagent flow<br />

rate.<br />

Step 16: Check the Sample Probe Flow<br />

1 Fill the 10 mL graduated cylinder with 10 mL DI water.<br />

2 Move the sample probe to the middle of the sample rack. (1:35 if set for a 60<br />

position rack).<br />

3 Position the graduated cylinder beneath the sample probe.<br />

4 Simultaneously click the Down button and start the stopwatch.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 3: Installing the <strong>Analyzer</strong><br />

5 After 30 seconds press the Up button.<br />

6 Measure the water remaining in the cylinder, and calculate the flow rate.<br />

7 Park the sample probe.<br />

NOTE:<br />

When properly adjusted the tension on the bottom three peristaltic pump<br />

tubes (channels 1-3) should be the same and the tension screw for the top<br />

pump tube (reagent tube, channel 1) should be screwed in 1 to 2 mm farther<br />

than the other channels.<br />

Once the clamp tension on the pump tubing is established, relieve their<br />

stretch:<br />

8 Unclamp reagent and sample clamps.<br />

9 Park the sample probe.<br />

10 Press the Up button to remove the sample probe from the rinse station.<br />

11 Remove the reagent uptake tube from the SnCl 2.<br />

12 Allow the waste tube to empty.<br />

13 Unclamp waste tube clamps.<br />

14 Turn the pump off using the software controls.<br />

Do not leave tubes clamped in place when the system is not being used. The<br />

next time the system is used, hook the tubes and close the quick-release<br />

mechanisms. No screw adjustments will be needed. Previous clamp tension is<br />

“remembered” as the quick release is engaged and disengaged.<br />

74


4 Using the <strong>Analyzer</strong><br />

Operation of the M-<strong>7600</strong> is mostly through the QuickTrace software<br />

interface.<br />

For a detailed description of the software see the QuickTrace help file and the<br />

QuickTrace mercury analyzer software manual.<br />

Theory of Operation<br />

Autosampler<br />

The autosampler is prepared for operation by loading sample vials of digested<br />

samples, into selected positions of the sample racks. Vials of calibration<br />

standards are placed in user-selected positions of the standards rack. Rinse<br />

solution, for sample-to-sample probe decontamination, fills the rinse station<br />

and re-circulates to the rinse bottle.<br />

After a method worksheet is prepared/loaded, the system is ready for<br />

unattended operation to begin. The autosampler operates under computer<br />

control to move the sample uptake probe to any sample position; the rinse<br />

station, reference standard, blank, etc., in a user-programmed sequence. The<br />

sample probe supplies the multi-channel peristaltic pump's sample inlet.<br />

For further information, see the Autosampler <strong>Operator's</strong> <strong>Manual</strong>.<br />

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Chapter 4: Using the <strong>Analyzer</strong><br />

QuickTrace M-<strong>7600</strong> Automated <strong>Mercury</strong> <strong>Analyzer</strong><br />

Figure 4-1<br />

QuickTrace M-<strong>7600</strong> Block Diagram.<br />

Sample Introduction & Stannous Chloride Reactor<br />

Refer to Figure 4-1 to trace the path of liquids through the M-<strong>7600</strong> System. An<br />

acidified digested aqueous sample from the autosampler is introduced, via<br />

peristaltic pump as Hg 2+ dissolved in solution. A reducing agent (10% stannous<br />

chloride in 7% HCl), is introduced via a parallel pump channel. The sample and<br />

reagent (SnCl 2) streams join at the mixing tee (1), and immediately enter the<br />

QuickTrace M-<strong>7600</strong> tubing reactor (“Liquid Mix”). Sn 2+ reduces Hg 2+ in<br />

solution to Hg 0 while the mixture is en route to the Gas-Liquid separator (GLS).<br />

At this stage and prior to the GLS, the analyte is present as a finely dispersed<br />

emulsion of liquid (metallic) Hg 0 micro-droplets, in excess SnCl 2 solution.<br />

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<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 4: Using the <strong>Analyzer</strong><br />

NOTE<br />

The <strong>CETAC</strong> QuickTrace M-<strong>7600</strong> mercury analyzer measures inorganic mercury<br />

(free Hg 2+ or HgCl 2 , which is subject to efficient stannous chloride reduction in<br />

the QuickTrace M-<strong>7600</strong> tubing reactor); using inorganic mercury standard<br />

solutions for instrument calibration. If insoluble mercury, bound mercury, or<br />

organomercurials are present in samples, an appropriate sample<br />

dissolution/digestion procedure will have to be employed to convert these<br />

other forms to free inorganic Hg 2+ or HgCl 2, prior to analysis with the<br />

QuickTrace M-<strong>7600</strong>.<br />

Gas-Liquid Separation<br />

The finely dispersed Hg 0 /SnCl 2 emulsion is introduced into the top of the GLS<br />

(Gas-Liquid Separator (2)). The Hg 0 /SnCl 2 emulsion flows over the frosted GLS<br />

center post in a relatively thin film, covering the entire post from top to<br />

bottom. A carrier gas simultaneously enters the bottom of the GLS tangentially<br />

(10). The carrier gas (Ar or N 2) swirls around the wetted center post and<br />

upwards toward the GLS gas exhaust port (11).<br />

Hg 0 droplets in the thin emulsion film quickly evaporate into the gas vortex<br />

surrounding the post. The carrier gas stream efficiently sweeps this Hg 0 vapor<br />

(along with some evaporated water) upward and out of the GLS gas exhaust<br />

(11), and on to the drying (12, 13) and optical section (14, 15) of the<br />

QuickTrace M-<strong>7600</strong> for an absorbency measurement.<br />

The liquid water, containing excess reducing agent, acid, any non-participating<br />

“spectator ions,” and reaction by-products, finally drains out the bottom of the<br />

GLS (3) and is pumped to waste (4), (channels one & two).<br />

NOTE<br />

The GLS operates “empty” with no liquid level. The liquid spreads out as a film<br />

that wets the center post. At the bottom of the post, the film collects at a<br />

single point and is then continuously pumped to waste, so the “liquid level”<br />

should not rise in the GLS.<br />

Carrier Gas<br />

Refer again to Figure 4-1 on page 76 to trace the path of the carrier gas. A<br />

clean, dry carrier gas, such as UHP N 2 or Argon, must be supplied to the back of<br />

the instrument. The gas passes through fixed restrictors to produce primary<br />

flow rates in the range of 30-1000 mL/min at 825 kPa (120 psig). The carrier<br />

gas first enters the reference cell (6) to facilitate measurement of the incident<br />

radiant power (P 0) at 253.7nm. It exits (7) and passes through the GLS (10) to<br />

pick up Hg 0 vapor from the reduced sample. The carrier gas and Hg 0 vapor exit<br />

the GLS (11) and enter (12) a Perma Pure ® drying cartridge where water<br />

vapor is removed by a Nafion ® membrane (13). For the Perma Pure ® dryer, an<br />

auxiliary sweep gas from a restrictor (5A) enters an auxiliary port (17) and<br />

selectively removes water vapor from the dryer cartridge at 18.<br />

Finally, the dry Hg 0 /carrier gas mixture exits the dryer (13) and enters the<br />

sample cell (14B) for measurement of transmitted radiant power (P) at 253.7<br />

nm.<br />

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Operator’s <strong>Manual</strong><br />

Chapter 4: Using the <strong>Analyzer</strong><br />

Ultimately, the gas stream (carrier gas and Hg 0 ) exits the sample cell (15) and<br />

is exhausted to a solid KMnO 4 trap (16) where Hg 0 is absorbed, and clean<br />

carrier gas passes to the lab atmosphere.<br />

Dryer Cartridge<br />

The mercury analyzer uses a Perma Pure ® DuPont Nafion ® -based dryer<br />

cartridge. Dryer cartridges typically last three to six months.<br />

The dryer cartridge contains Perma Pure ® dryer tubing which is made with a<br />

tubular DuPont Nafion ® membrane. The Nafion ® tubing is housed within an<br />

outer tube and coiled inside the cartridge. The argon or nitrogen carrier gas<br />

containing mercury and water vapor is swept along the inner Nafion ®<br />

membrane, allowing water vapor to permeate the membrane selectively,<br />

whereas the membrane is not permeable to mercury vapor. On the “waste” side<br />

of the membrane, a counter gas flow, split from the carrier gas supply,<br />

selectively sweeps the water vapor out of the system, whereas non-permeating<br />

mercury vapor proceeds to the sample cell.<br />

The Perma Pure ® dryer cartridge and associated plumbing is already preinstalled<br />

in your new QuickTrace M-<strong>7600</strong> factory shipment. No further<br />

installation is required.<br />

Optics and Cold Vapor AAS<br />

Refer again to Figure 4-1 on page 76 to trace the optical path of the<br />

QuickTrace M-<strong>7600</strong>. The Cold Vapor AAS (Atomic Absorption Spectrometry)<br />

process within the sample cell begins with a low pressure, high frequency,<br />

thermally stabilized, electro-optically regulated Hg vapor lamp, which<br />

produces the Hg emission spectrum. Emitted light is collimated (L 1) and<br />

projected in two parallel, isolated beams one each through the reference and<br />

sample cells. Absorbance of 253.7nm radiation by Hg 0 vapor (derived from the<br />

chemically reduced sample and GLS) occurs only in the sample cell. P is<br />

thereby decreased, relative to P 0.<br />

Light from the cells enter the binocular camera, where both collimated beams<br />

are independently focused (L 2) and filtered (F) before reaching the Charged<br />

Coupled Device (CCD) detector. Narrow band 254 +/- 2nm interference filters<br />

(F) remove all radiation but the strong 253.7 nm Hg 0 “resonance line” from<br />

both the sample (P) and reference (P 0) beams. By a photovoltaic effect, the CCD<br />

converts the light beams into electrical signals, proportional to radiant power<br />

(P and P 0). These outputs are processed to yield an electrical signal<br />

proportional to optical absorbance (Abs = -log (P/P 0)).<br />

Software<br />

In the host computer, the sample absorbance value is drift corrected, blank<br />

subtracted, if through blank is desired. The absorbance value is then measured<br />

against a calibration curve derived from previously obtained absorbance<br />

values of calibration standards.<br />

The QuickTrace software operates under a Windows environment. The<br />

QuickTrace software provides complete instrument, autosampler control.<br />

The QuickTrace software also provides a variety of EPA compliant quality<br />

control functions, display features, report generation and diagnostic routines.<br />

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Chapter 4: Using the <strong>Analyzer</strong><br />

The user interface is sufficiently powerful that it will satisfy the requirements<br />

of experienced technically advanced analysts and scientists.<br />

The reader is referred to the separate QuickTrace Help file and QuickTrace<br />

<strong>Mercury</strong> <strong>Analyzer</strong> Software <strong>Manual</strong> for a detailed description of the software<br />

features, functions, and operation instructions.<br />

Preparing Reagents and Calibration Standards<br />

Always use high purity gas, chemicals, acids, water, standards, and clean<br />

glassware for analysis. It may be necessary to acid wash and rinse all glassware<br />

more than once to eliminate contamination for the most sensitive mode of<br />

operation (


Operator’s <strong>Manual</strong><br />

Chapter 4: Using the <strong>Analyzer</strong><br />

NOTE<br />

The <strong>CETAC</strong> QuickTrace M-<strong>7600</strong> mercury analyzer measures inorganic mercury<br />

(free Hg 2+ or HgCl 2 , which is subject to efficient stannous chloride reduction in<br />

the QuickTrace M-<strong>7600</strong> tubing reactor). Inorganic mercury standard solutions<br />

are used for instrument calibration. If insoluble mercury, bound mercury, or<br />

organomercurials are present in samples, an appropriate sample<br />

dissolution/digestion procedure will have to be employed to convert these<br />

forms to free inorganic Hg 2+ or HgCl 2, prior to analysis with the QuickTrace M-<br />

<strong>7600</strong>. If it is desired to confirm the oxidative digestion procedure accuracy<br />

(recovery) regarding organomercurials, then organomercurial standards or<br />

appropriate standard reference materials would have to be carried through the<br />

digestion as “process standards”.<br />

WARNING<br />

ORGANOMERCURIAL EXPOSURE HAZARD<br />

The handling of organomercurial concentrates, which may be used in the<br />

preparation of process standards, presents a substantial (potentially lethal)<br />

safety hazard. Only an experienced, professionally trained organo-metallic<br />

chemist, knowledgeable and skilled specifically in the safe handling of<br />

organomercurials (using approved apparatus and approved protection<br />

measures in an approved facility) should attempt to prepare diluted<br />

organomercurial process standards from concentrates. Always be sure to<br />

obtain and carefully read the MSDS (Material Safety Data Sheets) before<br />

handling organomercurials!<br />

Always wear appropriate personal protective equipment when operating<br />

the mercury analyzer or handling organomercurials. At a minimum, you<br />

should wear eye protection, acid-resistant gloves, and a lab coat.<br />

NOTE:<br />

<strong>CETAC</strong> Technologies assumes no liability for the handling of organomercurial<br />

concentrates or the preparation, handling, or use of diluted organomercurial<br />

process standards.<br />

In most cases, <strong>CETAC</strong> Technologies recommends that samples be oxidized<br />

following standard, safe, well known, approved sample dissolution or digestion<br />

procedures, and that the QuickTrace M-<strong>7600</strong> instrument calibration<br />

standards be prepared only from inorganic mercury concentrates or diluted<br />

from commercially available inorganic mercury standard solution<br />

concentrates. Where possible, the recommended means of overall process<br />

(dissolution/digestion + QuickTrace M-<strong>7600</strong> analysis) validation should be<br />

through use of commercially available standard reference materials (SRM’s) of<br />

composition matching (or similar to) the samples and containing certified,<br />

known mercury levels in a concentration range similar to the samples. (Being<br />

by far the safest alternative, this SRM approach to overall process validation<br />

should be used whenever possible, and is nearly always preferred to preparing<br />

diluted process standards from hazardous organomercurial concentrates!)<br />

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Gas Parameters<br />

The QuickTrace M-<strong>7600</strong> has controls gas flow based on settings in the<br />

QuickTrace software. The user needs to adjust the method flow rate to<br />

achieve increased or decreased signal responses which are in part derived<br />

from gas flow rate.<br />

Carrier Gas<br />

Gas Pressure<br />

Gas Flow Rate<br />

N 2 UHP, high purity grade cylinder (dry,<br />

research grade) or Argon, high purity<br />

grade (supplied, for example, from a<br />

liquid Dewar boil-off or cylinder).<br />

120 psig (825 kPa)<br />

30-1000 mL/min<br />

For exact response versus gas flow parameters for your instrument, please<br />

consult the final test documentation, which accompanied the instrument.<br />

See Table 4-1 and Table 4-2 for a more complete listing of optimal instrument<br />

setups.<br />

Starting the System<br />

1 Power on the QuickTrace M-<strong>7600</strong>.<br />

2 Power on the autosampler.<br />

3 Open the QuickTrace software.<br />

The mercury vapor lamp automatically turns on when the QuickTrace<br />

software starts.<br />

4 Once the QuickTrace M-<strong>7600</strong> has powered up, and while the lamp is warming<br />

up, perform the following checks:<br />

‣ If this is the first time the instrument is started, check that the pump<br />

tubing is installed and tension is adjusted as described beginning on page<br />

70.<br />

‣ Check that supply gas is connected and 120 psig (825 kPa) pressure is<br />

applied to the unit.<br />

‣ If this is the first time the instrument is started, check that the KMnO 4 trap<br />

is filled as described on page 42.<br />

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NOTE:<br />

The mercury vapor trap will exhibit a noticeable brown color migrating toward<br />

the vapor exit port as the KMnO 4 is consumed. It may take a considerable<br />

amount of time to consume the entire amount of KMnO 4 . The reaction is the<br />

oxidation of Hg 0 to mercuric oxide with the KMnO 4 being reduced to<br />

manganese dioxide.<br />

<strong>Mercury</strong> Vapor Lamp Warmup<br />

The mercury vapor lamp automatically turns on when the QuickTrace<br />

software starts.<br />

The lamp will require 30-60 minutes to stabilize, as described in the following<br />

sections. Other instrument preparation may be performed during this time.<br />

Turning Off the <strong>Mercury</strong> Vapor Lamp for System Warm-Up<br />

If your intent is to only warm up the system and you are not going to analyze<br />

samples within the next hour it is recommended to navigate to instrument<br />

controls and turn off the mercury lamp.<br />

1 In the QuickTrace software, click the Instrument Control button.<br />

Figure 4-2<br />

Instrument Control Button.<br />

2 Click the Hg <strong>Analyzer</strong> button then click Lamp Off.<br />

Figure 4-3<br />

Turning Off the Lamp.<br />

System Warm-Up for Trace or Ultra-Trace Analysis<br />

For analysis in the trace to ultra-trace range (ppt), it is recommended to allow<br />

extra stabilization time as follows:<br />

1 Turn on the instrument and open the QuickTrace software.<br />

2 Navigate to instrument controls and turn off the mercury lamp.<br />

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3 Allow 2 hours for the instrument to stabilize.<br />

5 Turn on the lamp.<br />

4 Disengage the pressure shoe of the mercury analyzer's peristaltic pump.<br />

Disengaging the pressure shoe reduces wear on the peristaltic pump tubing<br />

while the pump stabilizes. Do not adjust the clamp tension.<br />

5 Run the peristaltic pump at the desired method rate.<br />

6 Allow 1 hour for the lamp and pump to stabilize.<br />

7 Proceed with liquid introduction to the system.<br />

System Warm-Up for ppb or Non-Ultra-Trace Analysis<br />

If the desired range is ppb or non-ultra-trace analysis the warm-up time from a<br />

warm start is just the lamp stabilization time. For a cold start in a non-trace<br />

range the system would need 30-60 minutes with the lamp and pump on at the<br />

desired rate to stabilize all parts of the system. For a warm start, allow 15-30<br />

minutes to stabilize the lamp.<br />

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Wetting the GLS<br />

At the beginning of each day or after any period of pump inactivity and prior to<br />

analysis ensure that the GLS center post is fully wetted.<br />

Refer to Figure 4-8 while reading the procedure below.<br />

1 Disconnect “11HG Vapor12” tube from the GLS vapor outlet.<br />

NOTE<br />

Always disconnect the Hg Vapor tube from the GLS when the system is not in<br />

use.<br />

Figure 4-4<br />

Disconnecting the Hg Vapor Tube.<br />

2 Set the gas to maximum flow. There are two ways to do this:<br />

‣ Click the Instrument Control button and set the flow rate to 1000 mL/min,<br />

or<br />

Figure 4-5<br />

Gas Flow Setting.<br />

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‣ Click the “Wet The Gas Liquid Separator Post” button. This will result in a<br />

gas flow of about 1000 mL/min with a pump rate of 100%.<br />

Figure 4-6<br />

Wet GLS Button.<br />

3 Check that the bottle supplying the autosampler rinse station is filled with<br />

clean trace metal grade acidified rinse solution.<br />

4 Place the reagent uptake tube in a beaker of DI water.<br />

5 If the peristaltic pump is not already on, turn it on.<br />

Figure 4-7<br />

Turning On the Pump.<br />

6 Engage the pressure shoe (quick release mechanism) on the peristaltic pump.<br />

7 Pinch the drain tube as shown in Figure 4-8. The drain tube runs from the GLS<br />

to the inlet side of the peristaltic pump.<br />

Pinch the Drain tube here<br />

Figure 4-8<br />

Pinching the Drain Tube.<br />

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8 With the drain tube pinched, the GLS should begin to fill with liquid. Once the<br />

liquid level rises, gas will bubble through it.<br />

9 Allow the GLS to fill until a gas bubble propels a “meniscus” upward to wet the<br />

post all along its length, including its top. (THE POST IS NOW WETTED.)<br />

10 When this happens, release (un-pinch) the drain tube. With the drain tube<br />

tension properly set and the drain tube un-pinched, the liquid will begin<br />

draining.<br />

11 Once the GLS has “emptied,” leave the pump running (keep liquid flowing) and<br />

reconnect “11HG Vapor12” tube to the GLS vapor outlet.<br />

12 Place reagent uptake tube in the SnCl 2.<br />

13 The post is now wetted and the QuickTrace M-<strong>7600</strong> is ready to run samples.<br />

The analyst may now operate the QuickTrace M-<strong>7600</strong> to perform analysis of<br />

samples. The help system built into the QuickTrace software has been<br />

developed specifically to assist the analyst in this task. Refer to the software<br />

manual, the online help, or the QuickTrace interactive demo to perform the<br />

desired analytical tasks.<br />

14 Once the analysis is finished, place the QuickTrace M-<strong>7600</strong> instrument in<br />

either Standby or Cold Shutdown condition (page 101).<br />

NOTE<br />

Concentration ranges greater than 20 ppb may require a higher percent acid in<br />

the rinse solution. A 5% HCl / 2% HNO 3 v/v should be sufficient for the highest<br />

concentration mode.<br />

NOTE<br />

If you don't want to consume stannous chloride reagent during a “standby”<br />

condition, you may alternatively keep the GLS center post wetted by<br />

immersing the reagent uptake tube in a beaker of deionized water (with the<br />

autosampler's sample probe also immersed in the autosampler rinse station).<br />

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Running the Interactive Demo<br />

The QuickTrace software comes with an interactive demonstration which will<br />

help you quickly understand the basic operation of the software.<br />

1 From the Start menu, select All Programs | <strong>CETAC</strong> QuickTrace | Interactive<br />

Demo.<br />

Figure 4-9<br />

Starting the Interactive Demo.<br />

Figure 4-10<br />

Interactive Demo Interface.<br />

Overview of the <strong>CETAC</strong> QuickTrace Software<br />

The QuickTrace software lets you create a method tailored to your analytical<br />

needs. You can specify a calibration, quality control limits with error actions<br />

and specific end-of-run routines such as automated standby, print or export<br />

routines.<br />

There are three basic parameters that affect the M-<strong>7600</strong>’s method ranges:<br />

‣ Gas flow rate<br />

‣ Sample peristaltic pump rate<br />

‣ Sample uptake rate<br />

By changing these basic parameters, you can set the QuickTrace M-<strong>7600</strong><br />

mercury analyzer to function in method ranges of ultra-trace to high µg/L<br />

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methods such as a high calibration standard of ~ 500 µg/L. These method<br />

ranges are guaranteed to exhibit at a minimum three orders of magnitude.<br />

The M-<strong>7600</strong> QuickTrace software comes with two basic templates or starter<br />

methods as described in “QuickTrace M-<strong>7600</strong> Startup Summary” on page 89.<br />

Follow these basic steps to create a new method based on one of the supplied<br />

templates:<br />

1 Open one of the supplied templates.<br />

The M-<strong>7600</strong> QuickTrace software comes with two basic templates or starter<br />

methods as described in “Summary of Gas and Liquid Flows for Analytical<br />

Ranges of the QuickTrace M-<strong>7600</strong>” on page 98.<br />

Click the File icon or the File menu and select New From… You will be asked to<br />

supply a name for the new method.<br />

Figure 4-11<br />

Creating a New Method Using the File Icon.<br />

Figure 4-12<br />

Creating a New Method Using the File Menu.<br />

2 Adjust the template to create a laboratory-specific method<br />

3 Perform the peak profile described in “Setting Baseline Correction” on page 91.<br />

4 After a successful peak profile, start the analytical sequence by selecting the<br />

green GO button, navigating to Analyze | Start Run, or typing Shift+Ctrl+F8.<br />

Learning More<br />

It is strongly recommended to navigate through the interactive demo, then<br />

view the help file or read the QuickTrace software manual to find out about<br />

more software features. In most cases, there are multiple ways to accomplish a<br />

given task.<br />

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QuickTrace M-<strong>7600</strong> Startup Summary<br />

1 Start the QuickTrace software.<br />

If the software was left open and in standby, open the instrument controls and<br />

start the autosampler rinse pump by clicking Pump On or Move Sipper to Park<br />

(either method will start the autosampler rinse pump).<br />

Figure 4-13<br />

Turning On the Pump.<br />

2 Turn on the lamp and initiate the carrier gas flow. A minimum of a 15-minute<br />

warm-up time is required.<br />

NOTE<br />

The lamp will automatically turn on when you start the QuickTrace software.<br />

Figure 4-14<br />

Turning On the Lamp and Carrier Gas.<br />

3 Clean and rinse the 2 L rinse bottle with DI water and refill with the desired<br />

trace metal grade HCl / HNO 3 solution.<br />

4 Place the autosampler rinse tubing into the rinse bottle.<br />

5 Prepare a fresh 10% SnCl 2. H 2O w/v 7% HCl v/v solution if old solution is<br />

yellow (oxidized) or precipitated. Prepare only what you need to complete the<br />

calibration and sample run including all QC checks and spikes. The reagent<br />

flow is ≈ 3.8 mL/min at 50% pump rate.<br />

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6 Verify that the sample capillary (inlet insert) is 0.5mm above the Gas-Liquid<br />

Separator (GLS) center post.<br />

7 Open the vents on the waste container.<br />

8 Inspect the peristaltic pump tubing for wear and flat spots (replace if<br />

necessary). If you remove any of the peristaltic pump tubes, do so one channel<br />

at a time, and be careful to return the tube to the appropriate pump channel.<br />

Do not lock the pressure shoes at this time.<br />

9 Place the reagent capillary in a beaker of DI water.<br />

10 Lock down the peristaltic pump pressure shoes.<br />

11 Inspect liquid flows. The GLS drain should be flowing smoothly with no build up<br />

or pulsing of liquid. The waste tube from the peristaltic pump to the waste<br />

container should be liquid/gas etc… with no vibration. If this is not the case<br />

upon inspection, stop immediately and change GLS drain tube and or waste tube.<br />

12 Wet the GLS center post as described on page 84.<br />

13 Inspect the rinse station for a convex liquid bubble adhering to the sample<br />

probe. If this is not the case, change the rinse pump peristaltic tubing.<br />

14 Open the appropriate worksheet (see the online help in the QuickTrace<br />

software) and set the gas pressure to match the method.<br />

You can also set the gas pressure by clicking on the Set Gas & Pump Speed icon.<br />

Figure 4-15<br />

Setting the Gas Pressure.<br />

15 Zero the QuickTrace M-<strong>7600</strong> using the auto zero.<br />

Figure 4-16<br />

Auto-Zero.<br />

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16 Peak profile the high standard and verify the baseline and sample integration<br />

times. Record µAbs and concentration of the peak profile standard in a daily<br />

instrument logbook. This operation should be performed on the highest<br />

standard.<br />

Figure 4-17<br />

Profiling the Highest Standard.<br />

17 Calibrate instrument and analyze samples.<br />

Setting Baseline Correction<br />

To guarantee a high quality result it is essential to always use the correct<br />

baseline correction.<br />

‣ For trace to ultra-trace levels (ng/L), use a two-point base line correction.<br />

‣ For µg/L levels, use a single point base line correction.<br />

Keeping an Instrument Log Book<br />

At a minimum, it is recommended that you record the following information in<br />

an instrument log book every day:<br />

‣ Date<br />

‣ Lamp current<br />

‣ Method<br />

‣ Response of highest calibration standard<br />

This will assist in troubleshooting any change in peak response.<br />

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Viewing the Graphs<br />

To scroll an absorbance/time graph, place the mouse pointer over the graph<br />

and hold the right mouse button.<br />

To zoom in on a graph, hold the left mouse button to draw a box from the<br />

upper-left to the lower-right corner of the region you wish to view.<br />

Setting a One-Point Baseline<br />

1 Examine the absorbance curve.<br />

The absorbance curve is displayed in the Method Editor after the peak profile<br />

has been performed.<br />

NOTE<br />

If you leave the method editor, the peak graph will not be retained. Make all<br />

your inspections and adjustments then save prior to exiting method editor. To<br />

save the adjustments, select File | Save, which will save the entire worksheet.<br />

2 Check “Baseline drift correction” to enable setting Baseline Point #1.<br />

Figure 4-18<br />

Typical Results from µg/L Settings.<br />

3 To set Baseline Point #1, place the end of the read about 4 seconds before the<br />

inflection point on the left side of the peak.<br />

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Figure 4-19<br />

Setting Baseline Correction Point #1 (µg/L).<br />

4 Zoom in on the graph to see the top of the peak, and record the peak height in<br />

the instrument log book.<br />

Figure 4-20<br />

10.0 µg/L Peak Profile Response With Baseline Correction.<br />

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Setting a Two-Point Baseline<br />

1 Examine the absorbance curve.<br />

The absorbance curve is displayed in the Method Editor after the peak profile<br />

has been performed.<br />

NOTE<br />

If you leave the method editor, the peak graph will not be retained. Make all<br />

your inspections and adjustments then save prior to exiting method editor. To<br />

save the adjustments, select File | Save, which will save the entire worksheet.<br />

2 Check “Baseline drift correction” to enable setting Baseline Point #1.<br />

3 Check “Two-point baseline correction” to enable setting Baseline Point #2.<br />

Figure 4-21<br />

Typical Results from ng/L Settings.<br />

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Chapter 4: Using the <strong>Analyzer</strong><br />

4 To set Baseline Point #1, place the end of the read about 4 seconds before the<br />

inflection point on the left side of the peak.<br />

Figure 4-22<br />

Setting Baseline Correction Point #1 (ng/L).<br />

5 Set Baseline Point #2 just after the signal returns to its baseline level on the<br />

right side of the peak.<br />

Figure 4-23<br />

Setting Baseline Correction Point #2 (ng/L).<br />

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Figure 4-24<br />

View of ng/L Baseline Correction Points.<br />

The software will average the baseline points and subtract that value from the<br />

peak height. The response will remain the same for each standard or duplicate<br />

sample and the drift correction will compensate for baseline drift, effectively<br />

zeroing out any instrument drift.<br />

For example, if the 100 ng/L response is 5000 units at time 0 and the baseline<br />

is at 0 the software will report 5000 units. If the baseline should drift over<br />

time, such as a baseline drift of 1000 units, and you analyze the 100 ng/L the<br />

response will be 6000 units. With baseline correction, the software will<br />

subtract the 1000-units drift from 6000 units and report a value of 5000 units<br />

or 100 ng/L. The same is true for a negative baseline drift.<br />

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Figure 4-25<br />

100 ng/L Peak Profile Response With Baseline Correction.<br />

6 Zoom in on the graph to see the top of the peak, and record the peak height in<br />

the instrument log book.<br />

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Summary of Gas and Liquid Flows for Analytical<br />

Ranges of the QuickTrace M-<strong>7600</strong><br />

RANGE #1: M-<strong>7600</strong> ng/L<br />


<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 4: Using the <strong>Analyzer</strong><br />

RANGE #2: M-<strong>7600</strong> µg/L<br />

0.1 – 20 µg/L Hg<br />

Gas Flow<br />

100 mL/min<br />

Peristaltic Pump Speed 50%<br />

Sample Flow Rate<br />

~5 mL/min<br />

ASX Rinse Pump Speed 50%<br />

Sample Time (for Liquid Uptake or autosampler “Sip”) 40 s<br />

Rinse Time<br />

95 s<br />

Read Delay<br />

52 s<br />

Replicate Read Time<br />

1.5 s<br />

Replicates 4<br />

Baseline Correction Method 1 point (20-25 s)<br />

Expected Results: 10 ppb | 7% HCl<br />

~150,000 µAbs<br />

Detection Limit (nominal):<br />

< 0.01 ppb<br />

Sample Throughput Rate (minutes/sample)<br />

~ 2.25 min/sample<br />

Table 4-2<br />

µg/L Parameters to Optimize<br />

Figure 4-27<br />

Typical Results from µg/L Settings.<br />

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Placing the QuickTrace M-<strong>7600</strong> in Standby Mode<br />

To prolong instrument life, do not leave the system fully on (with lamp on)<br />

overnight, or when not in use. However, to speed the next day’s startup, the<br />

QuickTrace M-<strong>7600</strong> can be left on with the lamp off overnight without<br />

significantly shortening its life.<br />

1 Turn the lamp off.<br />

Figure 4-28<br />

Turning Off the Lamp.<br />

NOTE<br />

The lamp will automatically turn off when you exit the QuickTrace software.<br />

2 When analysis is done for the day, rinse with 10% HNO 3 for several minutes<br />

through the reagent uptake tube.<br />

3 Rinse with deionized water through the reagent uptake tube for several<br />

minutes.<br />

NOTE<br />

Failure to perform this “shutdown rinse” may result in a system clog.<br />

4 Withdraw the reagent uptake tube.<br />

Secure the reagent uptake tube in a container that will keep it clean. A plastic<br />

re-sealable zipper storage bag, a plastic bottle, or a graduated cylinder with a<br />

plastic bag sealed over the top all work sufficiently.<br />

5 Remove the autosampler rinse supply tube from the bottle of rinse solution<br />

and allow the rinse station to run completely dry.<br />

Use the QuickTrace software controls to withdraw the autosampler probe<br />

from the rinse station when the rinse station becomes empty. Allow the drain<br />

and waste tubes to run completely dry.<br />

CAUTION<br />

Make sure the rinse return tube stays inside the bottle of rinse solution. Rinse<br />

solution may drain from the tubing while you are removing and wiping off the<br />

rinse supply tube.<br />

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6 Turn off both the M-<strong>7600</strong> peristaltic pump the autosampler peristaltic rinse<br />

pump.<br />

7 Release the M-<strong>7600</strong> peristaltic pump pressure shoes, and then lift the stops on<br />

the tubes out of the slots.<br />

8 Turn off the gas (main supply).<br />

9 Disconnect the Hg vapor tube from the GLS.<br />

Leave the system mains power on. The Hg lamp sent with the system has an<br />

operation life of ~5000 hours, but internal optical filter life may be<br />

substantially extended by turning off just the lamp whenever analyses are not<br />

being performed. Leaving the main power on leaves the lamp block heaters on,<br />

and consequently the lamp block remains thermally stable.<br />

To return the instrument to “run” status, simply turn the lamp on again, reestablish<br />

appropriate gas and liquid flows and operate the instrument<br />

normally. The system will be stable and ready to run within 5-10 minutes.<br />

If desired, exit the QuickTrace software, but leave the mains power on. This<br />

will also effectively keep the system in a warm start state.<br />

Cold Shutdown<br />

For a total system shutdown (to cold condition), prepare the pump tubing as<br />

you would for standby mode. Exit the QuickTrace software, shut down<br />

Windows and turn off the computer. Turn off the gas, autosampler, pump, and<br />

QuickTrace M-<strong>7600</strong> main power.<br />

Summary of QuickTrace M-<strong>7600</strong> Shut Down<br />

1 Place the reagent capillary in a beaker of 10% HNO 3 and cap the reagent bottle.<br />

Rinse the system for a minimum of ten minutes.<br />

2 Place the reagent capillary in a beaker of DI water and rinse the system for one<br />

minute.<br />

3 Remove reagent capillary from DI water.<br />

4 Remove the autosampler rinse supply tube from the bottle of rinse solution<br />

and allow the rinse station to run completely dry.<br />

Use the QuickTrace software controls to withdraw the autosampler probe<br />

from the rinse station. Allow the drain and waste tubes to run completely dry.<br />

CAUTION<br />

Make sure the rinse return tube stays inside the bottle of rinse solution. Rinse<br />

solution may drain from the tubing while you are removing and wiping off the<br />

rinse supply tube.<br />

5 Turn off both the M-<strong>7600</strong> peristaltic pump the autosampler peristaltic rinse<br />

pump.<br />

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6 Release the M-<strong>7600</strong> peristaltic pump pressure shoes, then lift the stops on the<br />

tubes out of the slots.<br />

7 Close the vents on the waste container.<br />

8 Disconnect the GLS exhaust tube from GLS.<br />

9 Turn off gas and lamp.<br />

10 If you are going to use the instrument the next day or in the near future, leave<br />

the instrument in this condition. It will then be ready for a warm start.<br />

11 If you are not going to be using the instrument in the near future then exit the<br />

QuickTrace software and turn off the autosampler and QuickTrace M-<strong>7600</strong>.<br />

NOTE<br />

Before shutting down the instrument to either Standby or Cold condition,<br />

remember to run 10% HNO 3 and deionized water through the SnCl 2 reagent<br />

tubes. This will clean out any chemicals from the peristaltic pump and sample<br />

tubing and prevent residue encrustation in the Gas-Liquid Separator and its<br />

drain. Remember to pump all tubes completely dry after rinsing.<br />

CAUTION<br />

Always remember to release all clamps and unhook the pump tubing from the<br />

peristaltic pump. Failure to release clamps and unhook the tubing when the pump<br />

is off, will cause tube fatigue and lead to poor results (bad RSD) when used for<br />

analysis the next time.<br />

102


5 Maintaining the<br />

<strong>Mercury</strong> <strong>Analyzer</strong><br />

Routine maintenance of the analyzer consists of daily and weekly cleaning of<br />

specific analyzer components. Routine maintenance also includes checking for<br />

leaks or other damage. Additional periodic maintenance tasks may be<br />

required, including replacement of the following analyzer components:<br />

peristaltic pump tubing, sample probe, rinse station tubing, GLS capillaries,<br />

GLS drain tubing and Perma Pure ® dryer cartridge.<br />

CAUTION<br />

Discharge static buildup and ground to the analyzer base or cabinet before<br />

performing any maintenance. Avoid touching the contacts on the communication<br />

ports.<br />

Maintenance Schedule<br />

Daily Maintenance (Always Check Before Analysis)<br />

‣ Ensure the autosampler rinse bottle is rinsed between analytical batches<br />

with small amounts 10% HNO 3 follow by DI water and refilled with<br />

acidified rinse solution. For concentration of standards and samples<br />

greater than 20 µg/L, a 5% HCl / 2% HNO 3 v/v should be sufficient. For<br />

trace to ultra-trace calibrations (such as 0 to 500 ng/L) a rinse solution of<br />

1% HCl / 1% HNO 3 v/v should be sufficient.<br />

‣ Ensure the rinse bottle tubes are completely submerged in rinse solution.<br />

The rinse station supply tubing should be at the bottom of the rinse bottle<br />

and the rinse station return tubing should be at the top of the rinse bottle.<br />

This will ensure that the rinse is a true recirculating rinse. Inspect the<br />

rinse station flow and ensure that the rinse is not removed via the sample<br />

probe faster than it is supplied. If the rinse station is being drained faster<br />

than the supply rate, you may need to adjust the autosampler pump rate in<br />

the method or change rinse pump tubing. Replace the autosampler rinse<br />

pump tubing periodically for best performance (See the Autosampler<br />

Operator’s <strong>Manual</strong>).<br />

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‣ Inspect the sample peristaltic pump tubing for fatigue and wear. Replace if<br />

too worn or fatigued.<br />

‣ If the pump tubing was left clamped overnight, install new tubing.<br />

‣ Pre-wet the GLS center post and be sure it remains completely wet during<br />

operation.<br />

‣ Check that the liquid flows, to and from the GLS, are smooth. Verify by<br />

close inspection the inlet to the GLS center post and drain exit points.<br />

‣ Be sure the waste bottle will not overflow during the run.<br />

‣ Check that the reagent bottle is sufficiently full for the number of samples<br />

to analyze.<br />

‣ Check that the SnCl 2 is fresh and not precipitated, crystallized, yellowed,<br />

or oxidized or that the small cap on reagent bottle was left open overnight.<br />

Replace if necessary.<br />

‣ For autosampler maintenance, see the appropriate autosampler Operator’s<br />

<strong>Manual</strong>.<br />

Weekly Maintenance<br />

‣ Remove the GLS and clean if residue is building up. See page 112 for<br />

instructions.<br />

‣ Clean the SnCl 2 reagent bottle weekly or before refilling.<br />

‣ Change the pump tubing if it is too worn, appreciably “flattened,” or left in<br />

place overnight.<br />

‣ Empty the waste bottle. Cap all Luer fittings to carry this bottle.<br />

‣ Check the cells and cell windows for cleanliness.<br />

Monthly Maintenance<br />

‣ Clean the GLS. See page 112 for instructions.<br />

‣ Clean the cells and cell windows. See page105 and following.<br />

‣ Replace the GLS inlet tubing and capillary insert. See page 115.<br />

‣ Replace the GLS drain tube. See page 116.<br />

‣ Check that the Perma Pure ® dryer cartridge is still good. A failing dryer<br />

cartridge may be indicated by loss of mercury absorbance sensitivity and<br />

an increase in the baseline of more than 3000 µabs during a short run of<br />

30 minutes or less. If the mercury absorbance for a given standard<br />

solution drops to 50% or more of its original value, change the cartridge.<br />

See page 117.<br />

Yearly Maintenance<br />

‣ Replace the Perma Pure ® dryer cartridge bi-yearly, or as needed. (See page<br />

117.) A failing dryer cartridge may be indicated by loss of mercury<br />

absorbance sensitivity and an increase in the baseline of more than<br />

3000 µabs during a short run of 30 minutes or less. If the mercury<br />

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absorbance for a given standard solution drops to 50% or more of its<br />

original value, change the cartridge.<br />

‣ Replace the 2-micron filter (See “Step 5: Connect the Carrier Gas Tubing”<br />

on page 40).<br />

Autosampler Yearly Maintenance<br />

‣ Replace the sample probe.<br />

‣ Replace the autosampler rinse peristaltic pump tubing.<br />

See the autosampler Operator’s <strong>Manual</strong>.<br />

Removal or Inspection of the Sample Cell<br />

Opening the Optics Access Panel<br />

1 Turn off power to the mercury analyzer and wait five minutes.<br />

2 Remove the four Philips screws which hold the access panel in place.<br />

Figure 5-1<br />

Screws for Optics Access Pane.<br />

WARNING<br />

For continued protection against hazards indicated on the warning labels,<br />

always retighten the screws securely after servicing.<br />

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3 Lift the access panel and set it aside.<br />

Figure 5-2<br />

Optical Access Panel of QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong>.<br />

4 Remove the thumbscrews on the optical cell clamps.<br />

Thumbscrews<br />

Cells<br />

Figure 5-3 Optical cabinet of QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong>.<br />

(Note that Viton ® tubing is always used for the carrier gas tubing; the color of<br />

the tubing in this figure has been modified to make it visible.)<br />

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Removing the Sample Cell<br />

Refer to Figure 5-3 and Figure 5-4. The cells are designed for simple removal<br />

and cleaning. When removing the cells, be careful to not touch the cell<br />

windows at the ends of the optical cells. If the cells and cell windows are dirty,<br />

use a clean foam swab and isopropyl alcohol (spectrophotometric grade only)<br />

to clean the surfaces (see page 107). If needed, the windows can be taken out<br />

by removing the end caps and the O-rings.<br />

Once the cell clamps have been removed, disconnect the carrier gas tubes from<br />

the cell end caps. Remove the cell end caps by holding the glass cell, pull, and<br />

rotate the end cap until it slides off the glass cell. Repeat this procedure for the<br />

reference cell. Inspect and/or clean the cell and its windows per the<br />

instructions beginning on page 107, or perform tubing maintenance as<br />

described in on page 113.<br />

Cleaning the Cell Windows<br />

Refer to Figure 5-4.<br />

There are two ways to clean cell windows:<br />

‣ Quick exposed surface cleaning (without dismantling).<br />

‣ Dismantling for total cleaning.<br />

The need for cleaning (or re-cleaning) is determined by close inspection of the<br />

window (D in Figure 5-4), visible through the hole in the window cap (A),<br />

while maintaining a low-angle total surface reflection of room light on the<br />

window. Any film, fingerprint, dust, or dirt will show up dramatically against<br />

the “white” background of a low-angle surface reflection of room light from the<br />

window.<br />

Quick Exposed Surface Cleaning<br />

Cleaning the exposed surface of the window requires the following: a clean<br />

foam swab, Kimwipes ® wipers, and a bottle of isopropyl alcohol (use only<br />

spectrophotometric grade).<br />

NOTE<br />

Do NOT use cotton swabs. They will leave small bits of lint, which can offset the<br />

absorbance baseline and add a great deal of noise, if the lint moves or flutters<br />

in the optical beam. Use only clean foam swabs. To pre-clean the foam swab,<br />

rinse in alcohol and dry with a KIMTECH SCIENCE KIMWIPES® delicate task<br />

wiper. Do not dip the swab in the alcohol supply (when new, the swabs may be<br />

dirty and contaminate the alcohol supply). Instead, squirt alcohol onto the<br />

swab with a wash-bottle that is for alcohol only and dry with the Kimwipes®<br />

wiper. Rinse and only lightly blot the swab with Kimwipes® wipers when<br />

cleaning; this will leave the swab moist with alcohol, which will be enough to<br />

clean the cell windows.<br />

Using the pre-cleaned, alcohol-moistened swab, gently swab the outside of the<br />

cell window. Wipe with a Kimwipes ® wiper and blow-dry with UHP Argon or<br />

Nitrogen. The blow-drying will also remove any lint or dust that may have<br />

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settled after cleaning. Re-check the surface reflection to see if the window is<br />

completely clean. If residue, fingerprints, or particles remain, repeat the<br />

process with another pre-cleaned alcohol-moistened foam swab until the<br />

windows are clean. If this quick procedure fails, it may be necessary to<br />

dismantle the assembly for more rigorous “total” cleaning, as described below.<br />

Figure 5-4 Cell assembly diagram.<br />

A - Window cap C - Phillips screws E - Cell end cap<br />

B - Window O-ring D - Sapphire windows F - Glass cell<br />

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Dismantling for Total Cleaning<br />

Refer again to Figure 5-4. Total cleaning requires a small Phillips screwdriver,<br />

clean Kimwipes ® wipers, isopropyl alcohol, and a clean plastic forceps.<br />

Carefully pull the cell end caps (E) off the cell (F), using a twisting motion, next<br />

remove the Phillips screws (C) and the window caps (A). This will allow the<br />

sapphire windows to be removed. Grip the window (D) with the forceps or<br />

wear powder free gloves when cleaning. Squirt the window with alcohol or use<br />

an alcohol wetted foam swab, then rub the surface of the window clean with a<br />

Kimwipes ® wiper. Rotate the forceps to a different position on the window and<br />

repeat the cleaning. Blow-dry with clean UHP Nitrogen or Argon.<br />

Clean the non-O-ring portion and gas ports of the end cap (E) with alcohol. Do<br />

not use alcohol to clean the O-ring (B). Do not handle the cleaned parts with<br />

your fingers; use clean forceps or powder free gloves. It will be necessary to<br />

blow dry the end cap; gas orifice and fitting with clean gas before assembly. Be<br />

sure not to touch the windows after cleaning.<br />

NOTE<br />

It is strongly recommended to clean both reference cell and sample cell at the<br />

same time. Be careful to keep the part orientation as originally supplied.<br />

Cell Assembly<br />

Reassemble the sapphire window (D), O-ring (B), and a window retainer (A)<br />

onto the cell end cap (E) with three flat-head Phillips screws (C), as shown in<br />

Figure 5-4. Be sure not to touch the clean O-ring (B). Handle it instead with<br />

clean forceps.<br />

Grip the cell (F) near one end and insert the cell into the open end of the cellend<br />

cap (E) with a pushing twisting motion. From Figure 5-5, which shows the<br />

“open” end, note that each cell end cap has two imbedded O-rings (A, B).<br />

Firmly push (with twisting motion) the cell into the open end of the cell end<br />

cap and continue pushing until both O-rings (A, B) are fully engaged.<br />

Figure 5-5<br />

A - O-ring<br />

Open End of Cell End Cap.<br />

B - O-ring<br />

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Inspect the assembled cell to determine that both O-rings (A, B) are fully<br />

engaged as shown in Figure 5-6. In Figure 5-6, shown without the window and<br />

cell cap, area “C” reveals no O-ring gap. This indicates that both O-rings A and B<br />

of Figure 5-5 are fully engaged. Figure 5-7, shown with window and cell cap,<br />

also reveals no O-ring gap at point C, (the boundary between the cell end (E)<br />

and the cell end cap.<br />

Figure 5-6 Engaged O-Ring. Shown without the window and cell cap.<br />

C - No gap visible<br />

Figure 5-7 Engaged O-Ring. Shown with the window and the cell cap.<br />

C - No O-ring visible D - Window O-ring E - Cell<br />

NOTE<br />

The O-ring “D” visible in Figure 5-7 seals against the cell window.<br />

If an O-ring is NOT engaged, as in Figure 5-6, the O-ring “B” Figure 5-8 is<br />

visible in the gap immediately at the end of the glass cell “E” Figure 5-8. This<br />

should look, instead like region “C” in Figures 5-5 and Figure 5-7. If the O-rings<br />

are not engaged correctly (as in Figure 5-8), then the system may drift and<br />

perform poorly. Assemble and attach the remaining cell end cap to the other<br />

end of the glass cell.<br />

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Figure 5-8 O-Ring NOT Engaged.<br />

B - O-ring is visible E - Cell end<br />

An alternate means of checking complete engagement of all O-rings in both<br />

cells is to measure the overall length of the fully assembled cell with a ruler. If<br />

the overall assembled cell length is: 8 29/32 inches (226.5mm), then both O-<br />

rings are engaged; 8 31/32 inches (228mm) indicates one O-ring is not<br />

engaged; 9 1/32 inches (229.5mm) indicates that two O-rings are not engaged<br />

(one in each end).<br />

CAUTION<br />

The glass tubing is sufficiently thick-walled that there is almost no danger of<br />

breakage (provided you have gripped near the end being inserted). However, for<br />

maximum safety, grip the glass tube with a sufficient thickness of cloth or paper<br />

towel to protect your hands in the unlikely event of glass breakage. Never insert or<br />

try to use a cracked or chipped glass tube.<br />

Once the cell has been completely assembled, with both O-rings fully engaged,<br />

place the cell on a flat surface with both cell end cap “flats” facing downward.<br />

Rotationally adjust the cells until both “flats” are flat against the surface and<br />

parallel with each other. Recheck O-ring engagement (as above) and re-inspect<br />

both windows under low-angle reflection illumination to verify that no<br />

residual dust, lint, fingerprints, or other smudges exist on the windows. If both<br />

windows are “clean”, attach the appropriate Viton ® interconnect tubing and<br />

reinstall the cells.<br />

To reinstall the clean (and/or re-tubed) sample cell, first check that the two<br />

cell holder “flats” are parallel to each other. A simple check will reveal both cell<br />

end cap flats to be completely “tight down” against a flat surface with no gap<br />

visible between the end cap and the flat surface, when parallel.<br />

Finally, reconnect the tubing and the optical cabinet cover.<br />

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Chapter 5: Maintaining the <strong>Mercury</strong> <strong>Analyzer</strong><br />

Cleaning the Gas-Liquid Separator<br />

Periodically it will be necessary to clean the Gas-Liquid Separator. Try<br />

pumping 10% HNO 3 through the system for 30 minutes continuously, followed<br />

by a deionized water rinse. For more aggressive cleaning, disconnect all tubing<br />

from the GLS. Be careful not to pull hard on the tubing; this can break the glass<br />

side arms off. Instead, use a fingernail to gently work the tubing off the glass<br />

arms.<br />

GLS Retainer<br />

Thumbscrew<br />

Figure 5-9<br />

Removing the GLS.<br />

Refer to Figure 5-9. After removing the drip tray, loosen the white, plastic<br />

retainer screw, and carefully remove the GLS by rotating the vapor outlet to the<br />

front and slide the GLS down through the clamp and exiting at the clamp<br />

bottom.<br />

Once the GLS is removed, place it in a beaker containing 50% HNO 3 v/v in DI<br />

water. If an ultrasonic bath is available, place the beaker in the bath, sonicate<br />

for 30 minutes, rinse both inside and outside with DI water, then repeat the<br />

cleaning with fresh acid. If an ultrasonic bath is not available, let the GLS soak<br />

for two hours in the 50% HNO 3. If excessively dirty immerse the GLS in a<br />

mixture of 20% nitric and 20% sulfuric acid and heat on a hot plate for several<br />

hours or until clean.<br />

Finally, rinse with DI water and dry. Reassemble GLS as shown on page 115.<br />

Tighten the plastic screw finger tight only.<br />

WARNING<br />

INHALATION HAZARD<br />

Hot concentrated acids may cause severe burns, severe fume inhalation<br />

trauma and/or death. They should be handled only by professionally<br />

trained chemists, who employ proper safety precautions and equipment<br />

(hoods, goggles, gloves, tongs, etc.).<br />

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Changing the Cell Gas Tubing<br />

Begin by opening the optical access panel as shown on page 106.<br />

Next, replace the tubing. The replacement tubes, which are in the cell gas<br />

tubing kit, are labeled and precut to length. See Figure 5-10 for label<br />

designations. Match these numbers and letters with the existing tubing to see<br />

where each labeled tube should go. It is best to replace one tube at a time.<br />

Figure 5-10<br />

Tubing Diagram and Connection Table.<br />

To remove an old tube from a plastic connector, grip it near its connector and<br />

pull firmly. For glassware, it is better to slit the old tube with a razor blade or<br />

sharp knife, before removing. Alternatively, you may use the edge of a<br />

fingernail to ease the tube off its glass arm.<br />

A simple way to avoid making wrong connections is to remove only one tube at<br />

a time, and replace this tube with the appropriate, labeled new one, before<br />

proceeding to the next tube.<br />

Drying cartridges are replaced as assemblies (replacements with tubing<br />

already attached).<br />

When finished, be sure no tubing is pinched when the covers are replaced.<br />

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Replace the Tygon ® drain waste as described on page 59.<br />

Sample in and drain tubes need to be replaced monthly. If needed, a cell gas<br />

tubing kit is available from <strong>CETAC</strong> with the correct labeled tubing included,<br />

pre-cut to the correct length.<br />

NOTE:<br />

Do not use waste tubing other than that provided by <strong>CETAC</strong>. The interior<br />

diameter and length (3 feet) of the drain tube are optimized for maximum<br />

system stability, and should not be altered. Other tubes are similarly optimized<br />

and substitutions/alterations should not be made.<br />

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Retubing the Gas-Liquid Separator<br />

This procedure should be followed once a month, unless the samples are<br />

excessively “dirty,” in which case the procedure should be followed more often,<br />

as needed. Improper installation can damage the GLS, so it is recommended to<br />

read the entire procedure before beginning.<br />

This procedure shows the drain tubing being installed after the GLS is<br />

mounted on the instrument. Alternatively, the capillary, liquid mix tube, and<br />

drain tube can be installed prior to the GLS being installed in its mount.<br />

GLS Inlet<br />

Refer to Figure 5-11. Note tubing routing and then remove all tubing, drain<br />

sleeve (J), inlet capillary (C) and silicone sleeve (D) from the GLS using the<br />

same procedure as for Viton ® tubing above.<br />

A – Liquid mix tube<br />

B – Capillary heat-shrink<br />

C – Teflon capillary<br />

D – Silicon inlet sleeve<br />

E – Sample inlet guide<br />

F – Hg vapor outlet<br />

G – Frosted center post<br />

H – Carrier gas inlet<br />

I – Teflon drain tubing<br />

J – Silicon drain sleeve<br />

Figure 5-11<br />

Assembled Gas-Liquid Separator.<br />

1 Select a new translucent white silicone inlet sleeve (D), and push it down over<br />

the glass sample inlet guide (E) until ≈ 6mm (1/4 inch) of silicone tubing<br />

protrudes above the top of the glass inlet guide (E).<br />

2 Select a replacement GLS Teflon inlet capillary assembly, (C). Carefully direct<br />

the capillary end of the insert into the top protruding end of the silicone tube<br />

(D), and GENTLY push straight down.<br />

The capillary insert (C) should go down inside the inlet guide (E). Continue<br />

pushing gently downward until the exposed capillary end (C) protrudes below<br />

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the glass guide (E). Stop pushing when the bottom edge of the capillary is<br />

about 0.5 mm (range of 0.3 - 0.6 mm) above the top of the GLS frosted center<br />

post (G).<br />

CAUTION<br />

The capillary insert should not touch the GLS center post. Pushing the capillary too<br />

far can damage the GLS.<br />

3 Select a replacement liquid mix tube (A). Carefully slide the end of the Viton ®<br />

liquid inlet tube labeled "2


<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

Chapter 5: Maintaining the <strong>Mercury</strong> <strong>Analyzer</strong><br />

Replacing the Perma Pure ® Dryer Cartridge<br />

Replace this cartridge if mercury absorbance diminishes to less than 50% of<br />

original value.<br />

14<br />

11<br />

Hg Vapor<br />

12<br />

Sample Gas<br />

18<br />

17<br />

Dryer Supply<br />

Dryer Exhaust<br />

Figure 5-12 Perma Pure ® Cartridge. (The numbers in this figure refer to<br />

the labels which are attached to each tube.)<br />

1 Open the instrument front door for access to the dryer cartridge.<br />

2 Disconnect the Hg vapor tube (labeled “11>Hg Vapor>12”) from the GLS arm<br />

(11).<br />

Figure 5-13<br />

Disconnecting the Hg Vapor Tube.<br />

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3 Disconnect the sample gas tube (labeled “>Sample Gas>14”) from the bulkhead<br />

(14).<br />

Figure 5-14<br />

Disconnecting the Sample Gas Tube.<br />

4 Disconnect the dryer gas supply tube (labeled “


<strong>CETAC</strong> QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong><br />

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6 Pull the Perma Pure ® dryer forward to detach it from the two black clamps and<br />

set aside.<br />

7 Install a new Perma Pure ® dryer cartridge and reattach tubes described above.<br />

(When reconnecting Luer lock fittings, be careful not to kink the tubing, which<br />

could cause gas flow constriction.) Remember to route the dryer tube (“18


Operator’s <strong>Manual</strong><br />

Chapter 5: Maintaining the <strong>Mercury</strong> <strong>Analyzer</strong><br />

exhaust.” If liquid has passed through the system, then proceed with the below<br />

corrective action steps.<br />

3 Remove the sample cell, GLS, and Perma Pure ® cartridge (with all tubing still<br />

attached). Place all parts on a clean lab cloth (or equiv.) on the lab bench.<br />

4 Dismantle the sample cell completely. See page 109.<br />

CAUTION<br />

Do NOT remove the cell window blocks over the optical rail if the cell is wet or full<br />

of water. Do this instead outside the instrument to avoid spillage onto the optical<br />

components.<br />

5 Dump out all water and brine from the sample cell glass tube.<br />

6 Rinse the sample cell glass tube with deionized water and oven dry.<br />

Alternatively, dry by rinsing with alcohol (recommended spectophotometric<br />

isopropyl alcohol (isopropanol)) and blowing dry with clean air, nitrogen, or<br />

argon.<br />

You can supply drying gas from the argon carrier gas source by simply<br />

disconnecting the instrument gas supply and turning down the gas pressure to<br />

create a low flow.<br />

WARNING<br />

The flow used for drying of the optical components must be less than 100<br />

mL/min or extremely low psig such as < 5 psi. If a flow greater than this is<br />

used, the gas could blow the optical parts from your grip and cause<br />

personal injury.<br />

7 Rinse and all remaining cell holder parts, fittings and transfer tubing with<br />

deionized water. Dry these parts by rinsing with alcohol (recommended<br />

spectophotometric isopropyl alcohol (isopropanol)) and blowing dry with<br />

clean air, argon, or nitrogen. Inspect closely to be sure all water, and/or all<br />

residual alcohol is completely eliminated from all fittings, tubes, parts, and gas<br />

ports.<br />

When you re-assemble the cell components and install the cleaned cells, use<br />

new or clean, dry reference and sample cell tubing.<br />

CAUTION<br />

Do not oven dry any of the parts except for the sample cell glass tube. Instead, use<br />

the alcohol rinse/blow-dry procedure. Excessive heat could damage these parts.<br />

8 Clean the sapphire window first with water and then as described on page<br />

109.<br />

9 Reassemble the window and cell end caps. Handle the window with clean<br />

forceps or hold by the edge with fingertips while wearing gloves (verify<br />

cleanliness by inspection with low-angle room light reflection).<br />

10 Install the glass tube into the cell end caps, and seat firmly to fully engage both<br />

O-rings.<br />

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11 For Perma Pure ® dryer cartridges that have gotten wet, if not already<br />

disconnected, disconnect the cartridge “sample gas” from sample cell. Attach a<br />

10 mL Luer lock syringe filled with DI water to tube 14 and gently push the<br />

water through the dryer cartridge. The water will exit through the cartridge at<br />

tube 11 (Figure 5-12, tube numbered 11). Hold tube 11 so it is positioned over<br />

an empty beaker (do not pull on tube 11 because it may disconnect from the<br />

cartridge and render it useless). Repeat the flushing procedure again followed<br />

by a syringe filled with air, which will flush the water out of the dryer<br />

cartridge. Next, adjust carrier gas flow to 40 mL/min. Reconnect tube 11 to the<br />

GLS. Turn on the gas and allow GLS and cartridge to blow dry for one hour<br />

with flowing gas. Be sure to engage all peristaltic pump tube clamps before<br />

initiating gas flow (otherwise the gases will leak out the pump tubing and<br />

bypass the dryer cartridge).<br />

12 Turn off gas!<br />

13 Reattach the cartridge sample outlet tube to the QuickTrace M-<strong>7600</strong> SAMPLE<br />

IN gas port, verify that the gas path tubing is correctly installed, and close the<br />

front door.<br />

See Figure 5-10 on page 113 for the gas path tubing. At this point, all of the<br />

tubing should be attached except for the final tube end labeled “18GAS<br />

EXHAUST”.<br />

NOTE:<br />

More than likely, water saturation of the Perma Pure® dryer will destroy it,<br />

making replacement necessary. However, if the overflow accident is quickly<br />

caught, cleaning and drying the Nafion® membrane in the dryer immediately<br />

(per above procedures) may save it.<br />

14 Determine whether any rinse solution (acidic stannous chloride dissolved in<br />

water) got past the sample cell (during the original accident), and into any<br />

portion of the remaining gas exhaust tubes and KMnO 4 trap.<br />

Determine this by dismantling all fittings “en route” and inspecting for the<br />

presence of any liquid or salt encrustation in any of the fittings or tube ends.<br />

Make sure to check the dark purple potassium permanganate powder to see if it<br />

is wet or no longer “free flowing” in any part of the trap tube.<br />

15 If no undesirable conditions are found in the above plumbing inspection,<br />

reconnect all the system plumbing and check the gas flow. The gas flow that<br />

exits the GLS should exit the exhaust fitting on the rear of the system at rate<br />

equal to the GLS exhaust rate less 1 to 2 mL/min due to internal Perma Pure ®<br />

dryer restrictions. As an example, if the flow out of GLS is 100 mL/min the flow<br />

out of the exhaust port should be ~ 98 mL/min. Be sure all peristaltic pump<br />

tubes are engaged by their clamps before checking gas flow (otherwise the<br />

gases will leak out the pump tubing and bypass the flow meter).<br />

16 If any undesirable condition was found during the above plumbing inspection<br />

proceed to the next step. Otherwise, skip to step 25.<br />

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17 Remove the potassium permanganate mercury trap from the rear of the<br />

instrument.<br />

WARNING<br />

POISON HAZARD<br />

The mercury vapor trap contains potassium permanganate (KMnO 4 ) and<br />

may contain mercury. Handle and dispose of the used KMnO 4 according to<br />

your laboratory’s procedures and your country’s hazardous waste<br />

regulations.<br />

If it is completely dry, simply set it aside.<br />

If the vapor trap is wet:<br />

1. Empty the KMnO 4 and dismantle the trap.<br />

2. Remove the glass wool plugs.<br />

3. Rinse all parts, fittings and tubes with deionized water and then<br />

Hydroxylamine Hydrochloride. The Hydroxylamine Hydrochloride will<br />

clean any remaining purple color from the vapor trap.<br />

4. Dry by means of rinsing with alcohol and blowing dry with clean air,<br />

argon, or nitrogen.<br />

5. Reinstall loose glass wool plugs into the endcaps.<br />

6. Install one cap, and refill tube body with potassium permanganate<br />

powder (crystals). Gently tap the tube as you fill it to settle the<br />

KMnO 4.<br />

7. Install the remaining end cap and set the trap aside.<br />

Do not reinstall the mercury vapor trap on the QuickTrace M-<strong>7600</strong><br />

instrument at this time.<br />

18 It is still necessary to rinse residual acidic stannous chloride brine out of<br />

remaining internal and external gas exhaust tubing. Refer to Figure 5-10.<br />

Locate the sample cell exit. Disconnect the exhaust tube at the sample cell.<br />

19 Connect the sample cell exhaust tube to a 10 mL syringe filled with water to<br />

perform a water flush of the internal and external exhaust tubes and port.<br />

20 Place the disconnected tubing from the KMnO 4 vapor trap into a waste<br />

receptacle (>100 mL) immediately under the “gas exhaust” fitting on the rear<br />

of the instrument. Alternatively, use the appropriate Luer fittings and hook<br />

another transfer tube from the rear gas exhaust fitting to the drain bottle on<br />

the floor.<br />

21 Using the syringe, push 50 to 100 mL of deionized water through the exhaust<br />

tube, until it all passes through to the waste collection receptacle. This will<br />

wash all residual perchlorate salt encrustation and/or acidic stannous chloride<br />

brine out of the internal gas exhaust tubes and fittings.<br />

22 Dry all of the tubing. To do this, engage the peristaltic pump tubing with all<br />

connections to the GLS and gas ports connected and allow gas to flush through<br />

the system until the exhaust tubing is dry.<br />

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23 Reinstall all covers and close all doors.<br />

24 Initiate a reasonable gas flow, then pump rinse solution through the GLS<br />

continuously, and let the system “purge,” “dry” and thermally stabilize for a<br />

period of 90 minutes.<br />

25 Reinstall the permanganate trap onto the back of the instrument.<br />

26 Operate instrument normally.<br />

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Replacing the Hg Lamp Bulb<br />

The effect of lamp current on data quality (absorbance and noise) is minimal<br />

over the range 2 – 15 mA. When a lamp is new, the normal operating lamp<br />

current is 2 – 5 mA. As the lamp ages, the lamp current will automatically<br />

adjust to maintain constant emission intensity reaching the EOFM<br />

filter/detector.<br />

WARNING<br />

ULTRAVIOLET RADIATION HAZARD<br />

Before opening the cover, turn off the power switch and disconnect the<br />

power cord. Sustained exposure of eyes to UV rays emitted from the lamp<br />

may result in permanent eye injury.<br />

When to Replace or Service the Lamp<br />

If the OVER RANGE indicator on the front of the mercury analyzer remains<br />

illuminated for more than 15 minutes when the mercury analyzer is turned on,<br />

it is time to consider replacing the lamp. The OVER RANGE indicator is<br />

illuminated whenever the current through the lamp exceeds a certain<br />

threshold.<br />

Cleaning the EOFM<br />

The electro-optical feedback monitor (EOFM) monitors the output of the lamp<br />

and adjusts the lamp current to ensure constant light intensity as the lamp<br />

ages. A filter ensures that the lamp output is measured only at the correct<br />

wavelength.<br />

Use a dentist mirror and flashlight to check that the EOFM filter is not<br />

“smudged.” Refer to Figure 5-18. If it's clean, order a replacement lamp.<br />

If the EOFM filter is dirty, clean in place using the cell cleaning procedure. If the<br />

OVER RANGE indicator continues to stay on, or if you need greater absorbance<br />

sensitivity than the old “high current” lamp can provide, replace the lamp.<br />

Lamp<br />

Assembly<br />

Cells<br />

Detector<br />

Assembly<br />

Figure 5-18<br />

M-<strong>7600</strong> Optical Rail.<br />

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Figure 5-19<br />

Lamp Assembly with Cover Removed (Side View).<br />

Lamp Block (Lamp is<br />

inserted from the other<br />

side of the bulkhead)<br />

EOFM Block<br />

EOFM Filter<br />

(Faces the lamp)<br />

Figure 5-20<br />

Lamp Assembly with Cover Removed (Side View).<br />

Getting a Replacement Lamp<br />

Lamps may be ordered from <strong>CETAC</strong> Technologies by visiting www.cetac.com.<br />

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Caring for the Lamp<br />

CAUTION<br />

Do not touch the glass part of the lamp. Fingerprints may damage the lamp.<br />

If it becomes necessary to clean the bulb, follow the same procedure as for<br />

cleaning the cell windows on page 107.<br />

Replacing the Lamp<br />

WARNING<br />

BURN HAZARD<br />

Turn off power and allow the mercury analyzer to cool for at least five<br />

minutes before touching the lamp.<br />

1 Turn off the mercury analyzer and disconnect the power cord.<br />

2 Allow the instrument to cool five minutes.<br />

3 Remove the cabinet screws from the electrical cabinet cover of the<br />

QuickTrace M-<strong>7600</strong> and remove the cover.<br />

Figure 5-21<br />

Location of Screws for Access to Lamp.<br />

4 Lift the right side of the gasket away from the sheet-metal divider to free the<br />

yellow lamp cord. It is not necessary to completely remove the gasket.<br />

Yellow Lamp Cord<br />

Gasket<br />

Figure 5-22<br />

Lifting the Gasket.<br />

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5 Locate the “heavy” yellow/orange colored lamp cord, on the right-hand side of<br />

the cabinet interior. Trace the cord backward and unplug it from the lamp<br />

controller board. Squeeze the lever on the bottom of the connector to release<br />

it.<br />

Figure 5-23<br />

Unplugging the Lamp Cord.<br />

6 On the top surface of the lamp block, push back the edge of the gray foam.<br />

Under the edge of this foam is a small Allen set screw. Insert the lamp<br />

replacement tool (a 0.050 inch Allen wrench, supplied with the M-<strong>7600</strong><br />

completion kit) into the setscrew head and loosen the screw.<br />

Figure 5-24<br />

Loosening the Set Screw.<br />

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7 Grab the old bulb where it attaches to its yellow cord and pull it straight out.<br />

The bulb will slide out easily.<br />

Lamp Bulb – DO NOT TOUCH<br />

Alignment Mark<br />

Figure 5-25<br />

Removing or Inserting the Lamp.<br />

8 Clean the new bulb by wiping clean with a Kimwipes ® wiper or optical tissue<br />

moistened with high purity (spectrophotometric grade) isopropanol, and blow<br />

dry with argon gas. Don't touch the bulb face, once it is clean.<br />

9 Holding it by the base, carefully insert the bulb into the lamp block until it<br />

stops.<br />

10 Rotate the bulb base until the mark on the lamp body faces straight up.<br />

Light output from the lamp is asymmetric—it is stronger toward the positive<br />

side of the lamp.<br />

11 Hold this position carefully while tightening the Allen set screw.<br />

12 Plug the yellow lamp cord into the lamp controller board.<br />

13 Replace the gasket. Start on the left end and work it onto the edge of the sheet<br />

metal.<br />

14 Replace the cover.<br />

15 Check the lamp current as described in the next section.<br />

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Adjusting the Lamp Current<br />

The lamp current can be adjusted using a potentiometer on the back of the<br />

instrument.<br />

Note that the effect of lamp current on data quality (absorbance and noise) is<br />

typically minimal when a lamp is new. As the lamp ages, the lamp current will<br />

automatically adjust to maintain constant emission intensity reaching the<br />

EOFM filter/detector.<br />

A new lamp needs a minimum of a 30 minute warm up time before final<br />

adjustment. After installation of the new lamp, the lamp current will<br />

automatically return to a value similar to the initial set up value.<br />

1 Make sure the mercury analyzer is turned on and that it is connected to the PC.<br />

2 Move the PC's display so that you can see it while you are behind the mercury<br />

analyzer.<br />

3 Exit the QuickTrace software, if it is running.<br />

4 Run the M-<strong>7600</strong> Lamp Current Configuration Tool. On the taskbar navigate to<br />

Start | All Programs | <strong>CETAC</strong> QuickTrace | M-<strong>7600</strong> Lamp Current Configuration<br />

Tool.<br />

5 Click Search for <strong>Analyzer</strong>s.<br />

Figure 5-26<br />

Searching for the <strong>Analyzer</strong>.<br />

6 Select the analyzer (if more than one is found) and click Connect.<br />

If you see an “analyzer in use” error, double-check to make sure that the<br />

QuickTrace software is not running.<br />

7 Allow 30 minutes for the lamp to warm up.<br />

8 While the lamp is warming up, remove the LAMP ADJUST access panel on the<br />

back of the instrument.<br />

9 Click Check Lamp Current.<br />

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10 Locate the mA ADJ potentiometer and use a small flat-blade screwdriver<br />

(jewelers screwdriver) to adjust the lamp current.<br />

Figure 5-27<br />

Adjusting the Lamp Current.<br />

‣ Begin by rotating the potentiometer fully clockwise until the OVER RANGE<br />

LED lights, then counterclockwise until the lamp current reads < 0.5 mA. At<br />

this point, the lamp is ready for adjustment.<br />

‣ Adjust the lamp current potentiometer until the marker is in the center<br />

(the green region) of the scale.<br />

‣ Clockwise will increase the current and counter-clockwise will decrease<br />

the current.<br />

‣ After each adjustment, click Check Lamp Current.<br />

‣ Let the voltage stabilize and make fine adjustments until the system<br />

stabilizes.<br />

11 Reinstall the cover and begin using the mercury analyzer.<br />

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Replacing the Fuse<br />

WARNING<br />

FIRE AND SHOCK HAZARD<br />

Replace only with the specified fuse. Using an incorrect fuse may cause fire<br />

or personal injury.<br />

Two fuses are located in the power supply, just above the power cord<br />

connector. Use a 5 A, 250 V, SLOBLO, 5x20 mm cylindrical fuse.<br />

1 Disconnect the power cord.<br />

2 Inspect all of the equipment which is plugged into the power supply for<br />

moisture or other conditions which might pose a hazard and cause the new<br />

fuse to blow.<br />

3 Using your fingernails or a small, flat-blade screwdriver, squeeze the ends of<br />

the fuse holder.<br />

M-<strong>7600</strong><br />

Power Switch<br />

Fuses<br />

4 Pull the fuse holder out.<br />

Figure 5-28<br />

Removing the Fuse Holder.<br />

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5 Replace the blown fuse with a new one of the same size, type, and rating.<br />

Figure 5-29 Fuse.<br />

6 Press the fuse holder back in until it clicks into place.<br />

7 Plug the power cord back in.<br />

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6 Troubleshooting the<br />

<strong>Mercury</strong> <strong>Analyzer</strong><br />

This chapter explains how to troubleshoot mercury analyzer problems. If you<br />

cannot solve a problem using the steps given in this chapter, you should<br />

contact <strong>CETAC</strong> Technologies Customer Service and Support.<br />

Troubleshooting Communication Issues<br />

If the QuickTrace cannot connect to the analyzer:<br />

Step 1: Check the Cable<br />

Check that the PC is connected directly to the M-<strong>7600</strong> with a standard Ethernet<br />

cable. To eliminate the possibility of an IP address conflict with another device<br />

on the company network, disconnect the PC from the company network while<br />

troubleshooting.<br />

Step 2: Use the IPSetup Tool to Check the Configuration<br />

Figure 6-1<br />

IPSetup Tool.<br />

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IPSetup a product of Netburner, Inc. IPSetup.exe is installed in the following<br />

folder:<br />

C:\Program Files\QuickTrace\IPSetup<br />

On the right hand side of the window will be a list of all Netburner-based<br />

devices (like the M-<strong>7600</strong>) that the program could find on the network. If you<br />

select one such device, its current IP configuration will appear on the left hand<br />

side of the window. These settings can be changed, and the changes applied<br />

simply by clicking on the “Set ” button in the middle. (The gateway and DNS<br />

settings are not necessary if the M-<strong>7600</strong> is connected directly to the PC, and<br />

can be left at 0.0.0.0 or any other legal value.) After making a change this way,<br />

turn the M-<strong>7600</strong> off, wait 15 seconds, then turn it back on.<br />

If no device is detected by the IPSetup tool then it is likely that either the<br />

device is not powered, or it is not connected to the network that the computer<br />

running IPSetup is connected to. It should be noted that IPSetup uses UDP, so if<br />

the M-<strong>7600</strong> is not directly connected to the PC, a router or bridge could be<br />

blocking UDP broadcasts.<br />

Step 3: Check the Subnet Configuration Using the Define<br />

QuickTrace Hardware Tool<br />

Once we know the device is connected to the network, and powered on we<br />

have to make sure the device is on a logical subnet that our PC can<br />

communicate with.<br />

1 To start <strong>CETAC</strong>'s Define QuickTrace Hardware tool, click Start | All Programs |<br />

<strong>CETAC</strong> Technologies | QuickTrace | Define QuickTrace Hardware.<br />

If the instrument is seen and connected to, then subnet compatibility is<br />

assured. Skip to “Step 4: Check for an IP address conflict” on page 137.<br />

If the instrument is not detected, then we’ll have to look at the IP address of<br />

the device.<br />

2 Open the Windows network connections dialog.<br />

For Windows 7, open the Windows Control Panel and select Network and<br />

Internet | Network and Sharing Center | View network status and tasks.<br />

Figure 6-2<br />

Network and Internet Settings (Windows 7, View by Category).<br />

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For Windows XP, open the Windows Control Panel and select Network<br />

Connections. Note that the remainder of the instructions below assume<br />

Windows 7.<br />

3 Click on the connection name (shown in blue).<br />

Figure 6-3 Network Connections in the Windows Control Panel.<br />

The network status will pop up.<br />

4 Click Properties.<br />

Figure 6-4<br />

Network Connection Properties Button.<br />

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5 Select ‘Internet Protocol Version 4’ and click ‘Properties’.<br />

Figure 6-5<br />

IPv4 Properties Button.<br />

6 Click Internet Protocol Version 4 (under XP there is no 4/6) and then click<br />

Properties.<br />

You will see a dialog that shows the TCP/IP setup for the connection.<br />

Figure 6-6<br />

IP Address and Subnet Mask.<br />

Subnet masks are often 255.255.255.0 and if this is the case, then you have to<br />

make sure that the first 3 sets of numbers for each device match (192.168.1 in<br />

this example; note that this is not the default value) and that the last numbers<br />

are different. The network administrator is in charge of allocating IP<br />

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addresses, and should be consulted if there’s any doubt about what number(s)<br />

to use. Once this configuration has been achieved, Define QuickTrace Hardware<br />

should be able to connect to the M-<strong>7600</strong> – this will result in the device IP<br />

configuration appearing as seen below.<br />

Figure 6-7<br />

Example of Network Settings for the <strong>Mercury</strong> <strong>Analyzer</strong>.<br />

Step 4: Check for an IP address conflict<br />

Checking for an IP address conflict is an important diagnostic step. A symptom<br />

of an IP address conflict might be that the M-<strong>7600</strong> works fine when the<br />

computer is not connected to the company network, but fails to connect, or<br />

fails intermittently when connected to the network.<br />

1 Determine the IP address of the M-<strong>7600</strong> using the IPSetup tool, then power off<br />

the M-<strong>7600</strong>.<br />

2 Open a command prompt (found under the “Accessories” folder on the Start<br />

menu.)<br />

Figure 6-8<br />

Opening a Command Prompt Window.<br />

3 Type the following command to change to the Windows system folder:<br />

CD \Windows\System32<br />

4 Type<br />

ping <br />

In our working example that would be ping 192.168.1.148. If a device<br />

with that address exists on the network (and is therefore in conflict with our<br />

M-<strong>7600</strong>) it will respond as seen at the top of the screen capture below with<br />

“Reply from : bytes= 32 time …” If there is no device with that IP<br />

address you’ll get a response that indicates “Destination host unreachable” as<br />

seen below for the ping 192.168.1.149 command.<br />

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Figure 6-9<br />

Example “Ping” Commands.<br />

If there’s a conflict, contact the network administrator for another IP address<br />

that can be used instead.<br />

If the IPSetup Tool Does Not Find the M-<strong>7600</strong><br />

1 Reset the IP configuration on the M-<strong>7600</strong> by holding down the recessed IP<br />

RESET button on the back of the analyzer as the analyzer is powered on.<br />

Continue to hold the button for about 5-10 seconds after you turn on the M-<br />

<strong>7600</strong>. This will reset the IP address to 192.168.0.149 with a netmask of<br />

255.255.255.0.<br />

2 Run IPSetup again. You should now be able to see the device and configure it.<br />

If IPSetup still cannot see the device and configure it:<br />

3 Switch the PC network interface to a compatible IP address (for example,<br />

192.168.0.100). See “Step 3: Check the Subnet Configuration Using the Define<br />

QuickTrace Hardware Tool” on page 134.<br />

4 Run Define QuickTrace Hardware to set the desired IP address.<br />

5 Turn the M-<strong>7600</strong> off, wait 15 seconds, then turn it back on.<br />

6 Set the PC’s network interface to a compatible setting.<br />

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"Subnet of this PC and the M-<strong>7600</strong> are Not Compatible" Error<br />

The ‘Define QuickTrace Hardware’ application may display the following<br />

message:<br />

Figure 6-10<br />

Error Message: Incompatible Subnet<br />

This means that the subnet configured for the secondary network card in the<br />

PC is not compatible with the subnet of the IP address configured for the M-<br />

<strong>7600</strong>. Click Yes to see what IP addresses are currently set:<br />

Figure 6-11<br />

Configuration Information for an Incompatible Subnet<br />

The address of the secondary network card should show up as "Interface 1."<br />

(The interface metrics you set earlier force this network card to be listed first.)<br />

In this example, the subnet of the M-<strong>7600</strong> is set to 11 and the subnet of the<br />

network card is set to 0. Since the laboratory network has a subnet of 0, a<br />

possible solution is to change the IP address of the secondary card to<br />

192.169.11.156.<br />

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Cannot Zero Instrument<br />

Perform the following steps:<br />

‣ Be sure instrument is fully warmed up with the peristaltic pump running<br />

at the method rate. The warm up time is dependent on the chosen method:<br />

ultra-trace may need at least 1 hour with the lamp and pump on; a normal<br />

µg/L range may only need 15 to 30 minutes. See “Starting the System” on<br />

page 81.<br />

‣ Check that both cells (sample & reference) and cell end caps are clean and<br />

“dry” (no liquid or dried stannous chloride obstructing the gas flow or the<br />

optical beam). See page 107 for cleaning instructions.<br />

‣ Check that both cell windows are clean. See page 107 for cleaning<br />

instructions.<br />

"Integration Adjustment Reached" Messages<br />

These messages can result if the M-<strong>7600</strong> power is cycled too rapidly. If this<br />

happens, the lamp current can get "stuck" at 6.5 mA. Always allow at least 15<br />

seconds before turning the M-<strong>7600</strong> back on.<br />

1654: Upper limit integration adjustment reached<br />

Cleaning the optics is recommended.<br />

This message means too little light is reaching the detector, and the system<br />

cannot compensate by increasing the integration period.<br />

‣ Turn the M-<strong>7600</strong> off. Wait at least 15 seconds, then turn it back on.<br />

‣ Clean the sample cells.<br />

‣ Check the lamp and replace it if needed.<br />

1655: Lower limit integration adjustment reached<br />

Contact <strong>CETAC</strong> technical support.<br />

This message means too much light is reaching the detector, and the system<br />

cannot compensate by decreasing the integration period.<br />

‣ Turn the M-<strong>7600</strong> off. Wait at least 15 seconds, then turn it back on.<br />

‣ Check that the sample cells are installed.<br />

‣ Adjust the lamp current.<br />

Drifting Baseline<br />

The system might not be thermally stable because of insufficient warm up<br />

time. Wait longer.<br />

‣ Check that gas pressures are stable and correct. Variable gas flow can<br />

cause the baseline to drift. Check that no stannous chloride encrustation<br />

exists in gas tubes/fittings after a GLS overflow accident. See “Removal or<br />

Inspection of the Sample Cell” on page 105.<br />

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‣ Check that the gas hoses are not pinched.<br />

‣ Check that the lamp block heater works. The lamp block should be hot<br />

(50°C) to touch. Turn the lamp power off. Remove lamp-housing cover and<br />

touch the lamp block momentarily to verify that it is hot.<br />

‣ With the Hg lamp off, check that the EOFM filter is not dirty (inspect it<br />

with a dentist’s mirror and low angle flashlight).<br />

‣ Check that the lamp current is not too high using the QuickTrace M-<strong>7600</strong><br />

instrument controls. High current indicates a worn-out lamp, if all the<br />

windows and optics are clean.<br />

‣ Replace the Perma Pure ® dryer cartridge.<br />

Low Absorbance or No <strong>Mercury</strong> Response<br />

‣ Ensure the Hg lamp is on.<br />

‣ Check all liquid uptake rates and gas flow. If there is no liquid or gas flow,<br />

see page 141.<br />

‣ Check that the reagent tube is in the reagent bottle.<br />

‣ Check that SnCl 2 is active, not empty, not oxidized or precipitated.<br />

‣ Check that standards have the correct Hg concentrations in them.<br />

‣ Check the liquid tubes for kinks or clogs.<br />

‣ Check that standards have 7% HCl in them.<br />

‣ Check the gas flow at the GLS outlet.<br />

‣ Check the gas flow at the sample cell outlet.<br />

‣ Check that the gas flow at the KMnO 4 trap outlet; does not drop in<br />

pressure or flow, this indicates an upstream block or a leak.<br />

‣ Check all plumbing connections for correct location and proper seal.<br />

‣ Replace the Perma Pure ® dryer cartridge.<br />

‣ Mechanically block the sample beam optical path (such as with a business<br />

card) and see if absorbance goes full scale (≥ 8,000,000 µabs). This task<br />

can be accomplished in instrument controls by starting the strip chart<br />

recorder.<br />

‣ Reboot the system: shut down the software, and power down the<br />

QuickTrace M-<strong>7600</strong> and autosampler. Restart, and check the signal.<br />

No Liquid or Gas Flow<br />

No Sample or Rinse Flow<br />

‣ Increase the tension on the sample pump tubing to start flow.<br />

‣ Be sure the sample, SnCl 2, and “Liq. Mix” tubes are not pinched off<br />

anywhere and restricting flow.<br />

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‣ Ensure the rinse station is filled with acidified rinse.<br />

‣ Ensure all pump tubing is centered in clamps.<br />

‣ Check for clogs in sample tubing.<br />

‣ Check for kinks in the autosampler sample probe and in the reagent<br />

uptake tube.<br />

‣ Check for excessive pump tubing wear. Replace if needed.<br />

No SnCl2 Flow<br />

‣ Increase tension on the reagent pump tubing to start flow.<br />

‣ Check to see that no precipitate has formed and clogged the reagent<br />

uptake and/or pump tubing.<br />

‣ Check for excessive pump tubing wear. Replace if needed.<br />

No Drain Flow<br />

‣ Increase tension on the drain pump tubing to start flow.<br />

‣ Check that there is no clogging of the drain outlet tubing of the Gas-Liquid<br />

Separator. If clogged, clean or replace the drain outlet tubing.<br />

‣ Be sure the drain tube is not pinched off and restricting flow. Ensure it is<br />

not pinched under the autosampler foot.<br />

‣ Check that the vent port on the waste bottle is open, and that the bottle is<br />

not overflowing.<br />

No Gas Flow or Low Gas Flow<br />

‣ Check that the in-line gas filter is not clogged. Remove the threaded<br />

connection downstream from the filter and check for gas flow at the filter<br />

outlet.<br />

‣ Check that all gas supply tubes are connected correctly.<br />

‣ Check that no gas tube is kinked or pinched.<br />

‣ Be sure that the KMnO 4 trap is not packed too tightly (with either the glass<br />

wool plugs or the reagent crystals) and restricting flow. Repack if too tight.<br />

‣ Check for leaks/clogs throughout the gas system, especially after a GLS<br />

overflow accident. Check flow after each fitting/component to isolate the<br />

bad section.<br />

Double Peak with Low Absorbance<br />

This may indicate a problem with not enough (or none at all) reagent<br />

(stannous chloride) uptake. Check the following items:<br />

‣ The reagent uptake tube is in the reagent bottle (rather than sitting in a<br />

deionized water container or loose in air).<br />

‣ There is liquid in the reagent bottle.<br />

‣ The reagent uptake tube is submerged below the liquid level.<br />

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‣ The liquid is 10% stannous chloride solution in 7% HCl.<br />

‣ The reagent is not “old,” precipitated, yellowed, or otherwise oxidized (for<br />

example, by leaving the bottle open overnight).<br />

‣ There is no clog, kink, pinch, or other obstruction in the reagent-tubing<br />

pathway.<br />

‣ The reagent liquid uptake rate is at least 1.5 mL/min at ~ 30% pump rate.<br />

‣ The autosampler sample probe tubing is the standard i.d. optimized for<br />

the mercury system: 1.0 mm i.d. (marked with a double blue band).<br />

‣ The sample uptake is at least 4.5 mL/min at ~ 30% pump rate.<br />

‣ The autosampler probe, reagent uptake tube, QuickTrace M-<strong>7600</strong> mixing<br />

tee and GLS liquid/mix capillary inlet is not under pressure from a partial<br />

clog.<br />

Poor Reproducibility<br />

‣ Always be sure to matrix match standards and samples as closely as<br />

possible (excluding the 7% HCl in the standards), and rinse solution<br />

should also be acidified.<br />

‣ Inspect the liquid flow into and out of the Gas-Liquid Separator. If either<br />

the sample in or waste out is pulsing, adjust the clamp tension on the<br />

corresponding tubing in the peristaltic pump to smooth out flows. If<br />

unable to stop the pulsing, check to see if the pump tubing is worn out. If<br />

so, replace the pump tubing. Be sure to check all the pump tubes.<br />

‣ Ensure the center post is fully “wet.” If partially dry anywhere on post<br />

surface, wet the post. See page 84.<br />

‣ Check to see if the reagent tube is in the reagent bottle.<br />

‣ Ensure that the stannous chloride has not been emptied or oxidized. Old<br />

SnCl 2 can lead to poor results. Replace if yellow, precipitated, or just too<br />

old.<br />

‣ Ensure that the autosampler rinse station and rinse bottle are filled with<br />

acidified rinse.<br />

‣ Inspect both cell windows for fingerprints, films, or debris. If dirty, clean<br />

the windows following the procedure on page 107.<br />

‣ Make sure gas pressure to the QuickTrace M-<strong>7600</strong> is 120 psig (825 kPa).<br />

‣ Check the output gas flow after the KMnO 4 gas trap with a flow meter (to<br />

check this flow, all pump tubes must be clamped or plugged). This gas flow<br />

should be the same as set in the software. Check all the seals and<br />

recalibrate if necessary. Note calibration and flow stability.<br />

‣ Check the gas flow at the GLS exit.<br />

‣ Check the gas flow at the sample cell exit.<br />

‣ Check that the optimal instrument settings are employed. See “Using the<br />

<strong>Analyzer</strong>” beginning on page 75, the QuickTrace M-<strong>7600</strong> help file, or the<br />

QuickTrace M-<strong>7600</strong> <strong>Mercury</strong> <strong>Analyzer</strong> Software <strong>Manual</strong> for more details.<br />

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‣ Check that the peristaltic pump rollers are not severely worn. Inspect all<br />

rollers with tubing removed. Roller facets should not be “grooved.” All<br />

rollers should spin freely when turned by sliding your thumb quickly<br />

across them. None should feel “gritty” or slow in spinning. Replace the<br />

head if any one of the 12 rollers are grooved or fail to move freely.<br />

‣ Ensure the baseline is not drifting severely. (See page 140).<br />

‣ Check that the raw analog system noise is ≤ 400 µAbs peak to peak. If not,<br />

call <strong>CETAC</strong> Support.<br />

Noisy Baseline<br />

‣ Check that flows into and out of the Gas-Liquid Separator are not pulsing.<br />

Pulsation indicates improperly adjusted pump clamps.<br />

‣ Make sure the gas pressures are correct.<br />

‣ Be sure the SnCl 2 is fresh and not oxidized or precipitated.<br />

‣ Ensure the cell windows are clean.<br />

‣ Check that the EOFM filter is clean. Turn the Hg lamp off and ensure that<br />

the EOFM filter is not dirty (inspect it with a dentist’s mirror and low<br />

angle flashlight).<br />

‣ Check that nothing has been spilled on the binocular camera lenses. Turn<br />

the Hg lamp off and ensure that the camera lenses are not dirty (inspect<br />

them with a dentist’s mirror and low angle flashlight). Call <strong>CETAC</strong><br />

Customer Service and Support if the camera lenses are dirty.<br />

Ensure the lamp current is not excessive. For more information see “Adjusting<br />

the Lamp Current” on page 129.<br />

Bad DL<br />

‣ Check Low Absorbance. See “Low Absorbance or No <strong>Mercury</strong> Response”<br />

on page 141 and “Double Peak with Low Absorbance” on page 142.<br />

‣ Check noisy baseline. See page 144.<br />

Sudden Standard Absorbance Rise During Run<br />

‣ Ensure the rinse bottle has acidified rinse.<br />

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Poor Accuracy<br />

‣ Verify good reproducibility (typically ~1% RSD on standard replicates).<br />

‣ If reproducibility is poor, see “Noisy Baseline” on page 144.<br />

‣ Be sure the standards contain 7% HCl (v/v).<br />

‣ Be sure the samples are properly digested.<br />

‣ Utilize an appropriate process standard to validate digestion and<br />

container storage.<br />

‣ Check process (digestion blanks, containers, and rinse solution) for<br />

mercury contamination.<br />

‣ Check standard solution accuracy, and all gravimetric/volumetric process<br />

steps and equipment for accuracy and calibration.<br />

‣ If very low samples are run immediately following high samples or<br />

standards, the rinse time may not have been long enough and the result<br />

may be reading low. (Increase rinse times when sample and/or standard<br />

concentrations are widely spread).<br />

Be sure that the rinse solution contains at least 1% HCl / 1% HNO 3. If it only<br />

contains deionized water, very low samples (acidified) may read erroneously<br />

high if they immediately follow the high standard or a high sample, regardless<br />

of allocated deionized water rinse time. The problem is avoided by a acidified<br />

rinse solution in the rinse solution bot<br />

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Returning the Product to <strong>CETAC</strong> for Service<br />

Refer to the following information if you need to return the product to <strong>CETAC</strong><br />

Technologies for service.<br />

Shipping the Product<br />

Follow these guidelines when shipping the product:<br />

‣ Use the original packing materials. If the original shipping materials are<br />

not available, place a generous amount of shock-absorbing material<br />

around the instrument and place it in a box that does not allow movement<br />

during shipping. Seal the box securely.<br />

‣ Contact <strong>CETAC</strong> Technologies before shipping the product.<br />

‣ Pre-pay all shipping expenses including adequate insurance.<br />

‣ Write the following information on a tag and attach it to the product:<br />

• Name and address of the owner<br />

• Product model number and serial number<br />

• Description of service required or failure indications<br />

‣ Mark the shipping container as FRAGILE.<br />

‣ In all correspondence, refer to the instrument by model name or number<br />

and full serial number.<br />

‣ Do not return products which are contaminated by radioactive<br />

materials, infectious agents, or other materials constituting health<br />

hazards to <strong>CETAC</strong> employees.<br />

Product Warranty Statement<br />

NOTE<br />

Contact <strong>CETAC</strong> Technologies or refer to the warranty card which came with<br />

your product for the exact terms of your warranty. The following copy is<br />

provided for your convenience, but warranty terms may be different for your<br />

purchase or may have changed after this manual was published.<br />

<strong>CETAC</strong> TECHNOLOGIES warrants that for (1) one year from the date of<br />

shipment of any <strong>CETAC</strong> unit manufactured or supplied by <strong>CETAC</strong> and found in<br />

the reasonable judgment of <strong>CETAC</strong> to be defective in material or workmanship<br />

will be repaired by <strong>CETAC</strong> without charge for parts and labor.<br />

The unit, including any defective part, must be returned to <strong>CETAC</strong> within the<br />

warranty period. The expense of returning the unit to <strong>CETAC</strong> for warranty<br />

service will be paid for by the buyer. <strong>CETAC</strong>’s responsibility in respect to<br />

warranty claims is limited to making the required repairs or replacements, and<br />

no claim of breach of warranty shall be cause for cancellation or recession of<br />

the contract of sale of any unit.<br />

Products may not be returned which are contaminated by radioactive<br />

materials, infectious agents or other materials constituting health hazards to<br />

<strong>CETAC</strong> employees.<br />

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This warranty does not cover any unit that has been subject to misuse, neglect,<br />

negligence or accident. The warranty does not apply to any damage to the unit<br />

that is the result of improper installation or maintenance, or to any unit that<br />

has been operated or maintained in any way contrary to the operating or<br />

maintenance instructions as specified in the <strong>CETAC</strong> Instruction and Operations<br />

<strong>Manual</strong>. The warranty does not cover any unit that has been altered or<br />

modified so as to change its intended use. Any attempt to repair or alter any<br />

<strong>CETAC</strong> unit by anyone other than by <strong>CETAC</strong> authorized personnel or agents<br />

will void this warranty.<br />

In addition, the warranty does not extend to the repairs made necessary by the<br />

use of parts, accessories, or fluids which are either incompatible with the unit<br />

or adversely affect its operation, performance or durability.<br />

<strong>CETAC</strong> reserves the right to change or improve the design of any unit without<br />

assuming any obligation to modify any unit previously manufactured.<br />

THE FOREGOING EXPRESS WARRANTY IS IN LIEU OF ALL OTHER<br />

WARRANTIES, EXPRESSED OR IMPLIED INCLUDING WARRANTIES OF<br />

MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE.<br />

<strong>CETAC</strong>’S OBLIGATION UNDER THIS WARRANTY IS STRICTLY AND<br />

EXCLUSIVELY LIMITED TO THE REPAIR OR REPLACEMENT OF DEFECTIVE<br />

PARTS, AND <strong>CETAC</strong> DOES NOT ASSUME OR AUTHORIZE ANYONE TO ASSUME<br />

FOR THEM ANY OTHER OBLIGATION.<br />

<strong>CETAC</strong> ASSUMES NO RESPONSIBILITY FOR INCIDENTAL CONSEQUENTIAL OR<br />

OTHER DAMAGES (EVEN IF ADVISED OF SUCH POSSIBILITY), INCLUDING BUT<br />

NOT LIMITED TO, LOSS OR DAMAGE OF PROPERTY, LOSS OF REVENUE, LOSS<br />

OF USE OF THE UNIT, LOSS OF TIME, OR INCONVENIENCE.<br />

This warranty and all matters arising pursuant of it shall be governed by the<br />

laws of the State of Nebraska, United States.<br />

Returned Product Procedures<br />

Claims for shipment damage (evident or concealed) must be filed with the<br />

carrier by the buyer. <strong>CETAC</strong> must be notified within ninety (90) days of<br />

shipment of incorrect materials. No product may be returned, whether in<br />

warranty or out of warranty, without first obtaining approval from <strong>CETAC</strong>. No<br />

replacements will be provided, nor repairs made, for products returned<br />

without such approval. Any returned product must be accompanied by a<br />

return authorization number. The expense of returning the unit to <strong>CETAC</strong> for<br />

service will be paid by the buyer. The status of any product returned later than<br />

thirty (30) days after issuance of a return authorization number will be subject<br />

to review. Shipment of repaired products will generally be made forty-eight<br />

(48) hours after the receipt.<br />

Do not return products which are contaminated by radioactive materials,<br />

infectious agents, or other materials constituting health hazards to <strong>CETAC</strong><br />

employees.<br />

Returned Product Warranty Determination<br />

After <strong>CETAC</strong>’s examination, warranty or out of warranty status will be<br />

determined. If a warranted defect exists, the product will be repaired at no<br />

charge and shipped prepaid back to the buyer. If the buyer desires an air<br />

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freight return, the product will be shipped collect. Warranty repairs do not<br />

extend the original warranty period.<br />

If an out of warranty defect exists, the buyer shall be notified of the repair cost.<br />

At such time the buyer must issue a valid purchase order to cover the cost of<br />

repair and freight, or authorize the products to be shipped back as is, at the<br />

buyer’s expense. Failure to obtain a purchase order number approval within<br />

fifteen (15) days of notification will result in the products being returned as is,<br />

at the buyer’s expense.<br />

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Chapter 7: Safety and Regulatory Information<br />

7 Safety and Regulatory<br />

Information<br />

Review this product and related documentation to familiarize with safety<br />

markings and instructions before you operate the instrument.<br />

Characteristics<br />

Environmental Characteristics<br />

Operating Temperature +5° C to +40° C (+41° F to +104° F)<br />

Non-Operating Temperature +0° C to +55° C (+32° to +131° F)<br />

Operating Altitude<br />

Relative Humidity<br />

Non-Operating Relative Humidity<br />

Up to 2,000 m (6,562 ft)<br />

0% to 80% non-condensing for<br />

temperatures up to 31° C, decreasing<br />

linearly to 50% at 40° C<br />

0% to 95% non-condensing<br />

Pollution Degree Pollution Degree 2<br />

Normally no pollution or only dry, nonconductive<br />

pollution occurs. The<br />

pollution has no influence. Occasionally,<br />

however, a temporary conductivity<br />

caused by condensation may be<br />

expected.<br />

Table 7-1: Environmental Characteristics for Safe Operation<br />

For indoor use only.<br />

Avoid sudden, extreme temperature changes which could cause condensation<br />

on circuit boards in the product.<br />

These environmental characteristics indicate the conditions for safe<br />

operation. See “Establishing Optimal Operating Conditions” on page 17<br />

for the recommended environment for the best experimental results.<br />

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Electrical Characteristics<br />

Power requirements<br />

M-<strong>7600</strong> <strong>Mercury</strong><br />

<strong>Analyzer</strong><br />

Input:<br />

AC Voltage, Frequency, and Current<br />

100-240 V ~<br />

50-60 Hz<br />

3 A<br />

Installation Category: CAT II (Line voltage in appliance and<br />

to wall outlet)<br />

AUX POWER Outputs:<br />

24 V DC, max 3.33 A each connector, max 6 A total<br />

Table 7-2: Power Requirements<br />

Input and output connectors<br />

Connector<br />

AUX INPUT<br />

Description and characteristics<br />

Trigger signal input, reserved for future use. Connect only<br />

as instructed by <strong>CETAC</strong> Technologies. (Max 28V DC)<br />

ETHERNET Ethernet connection. (Max 5V)<br />

Table 7-3: Electrical Input and Output Connectors on the <strong>Analyzer</strong><br />

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Safety Notices<br />

WARNING<br />

INJURY HAZARD<br />

If the equipment is used in a manner not specified by <strong>CETAC</strong> Technologies,<br />

the protection provided the equipment may be impaired.<br />

Repair or service that this not covered in this manual should only be<br />

performed by qualified personnel.<br />

Replacement Parts<br />

Except as otherwise noted, all replacement parts must be obtained from <strong>CETAC</strong><br />

Technologies. Visit www.cetac.com for a current list of available spare parts.<br />

Chemical Hazards<br />

WARNING<br />

POISON HAZARD<br />

Do not prepare organomercurial concentrates unless you are qualified to<br />

do so. Improper handling can result in injury or death.<br />

The handling of organomercurial concentrates which may be used in the<br />

preparation of process standards presents a substantial (potentially lethal)<br />

safety hazard. Only an experienced, professionally trained organo-metallic<br />

chemist, knowledgeable and skilled specifically in the safe handling of<br />

organomercurials (using approved apparatus and approved protection<br />

measures in an approved facility) should attempt to prepare diluted<br />

organomercurial process standards from concentrates.<br />

<strong>CETAC</strong> Technologies assumes no liability for the handling of organomercurial<br />

concentrates or the preparation, handling, or use of diluted organomercurial<br />

process standards. Instead, <strong>CETAC</strong> Technologies recommends use of<br />

appropriate standard reference materials to validate sample preparation<br />

(dissolution/digestion) and use of inorganic mercury standards for instrument<br />

calibration.<br />

Power Cord Set Requirements<br />

The power cord set supplied with your instrument meets the requirements of<br />

the country where you purchased the instrument.<br />

If you use the instrument in another country, you must use a power cord set<br />

that meets the requirements of that country.<br />

Power Cord Safety Maintenance<br />

The operator should check the power/signal supply cord condition. The<br />

equipment should not be operated if the mains inlet is cracked or broken. Any<br />

obvious damage to the case (from a drop or fall) should be checked by service<br />

personnel for loose or damaged parts. See individual parts lists for approved<br />

replacement parts<br />

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Grounding<br />

This equipment is designed for connection to a grounded (-earthed) outlet.<br />

The grounding type plug is an important safety feature. To reduce the risk of<br />

electrical shock or damage to the instrument, do not disable this feature.<br />

See “Power Requirements” on page 20 and “Electrical Characteristics” on page<br />

150 for more information.<br />

Mains Disconnect<br />

The power switch on the rear panel is not the mains disconnect. Power mains<br />

disconnect is accomplished by unplugging the power cord at the power supply<br />

or at the wall outlet. Ensure the power cord is easily accessible and removable,<br />

in the event of an emergency which requires immediate disconnection.<br />

WARNING<br />

SHOCK HAZARD<br />

Ensure that power cord is disconnected before removal of any covers.<br />

Mechanical Hazards<br />

1<br />

Figure 7-1<br />

Overview of Mechanical Hazards.<br />

WARNING<br />

1 –PINCH HAZARD<br />

Keep fingers, hair, and loose clothing away from moving parts when the<br />

system is powered on.<br />

Additional hazards related to the autosampler are described in the<br />

autosampler <strong>Operator's</strong> <strong>Manual</strong>.<br />

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Cleaning Instructions<br />

For additional cleaning information, see “cleaning” in the index.<br />

To clean the exterior surfaces of the instrument, complete the following steps:<br />

1 Shut down and unplug the instrument.<br />

2 Wipe the instrument exterior surfaces only using a towel dampened with a<br />

lab-grade cleaning agent.<br />

3 Repeat step 2, using a towel dampened with clear water.<br />

4 Dry the instrument exterior using a dry towel.<br />

WARNING<br />

SHOCK HAZARD<br />

Do not allow any liquid to enter the instrument cabinet or come into<br />

contact with any electrical components. The instrument must be<br />

thoroughly dry before you reconnect power, or turn the instrument on.<br />

Operating Environment<br />

WARNING<br />

SHOCK HAZARD<br />

To reduce the risk of fire hazard and electrical shock, do not expose the<br />

unit to rain or humidity. To reduce the risk of electrical shock, do not open<br />

the cabinet. All maintenance is to be performed by an Authorized <strong>CETAC</strong><br />

Service Provider.<br />

Protection provided by the equipment may be impaired if the equipment is<br />

used in a manner not specified by the manufacturer.<br />

WARNING<br />

SHOCK HAZARD<br />

Equipment is not intended for wet locations. Miscellaneous liquids in the<br />

equipment could cause hazardous conditions.<br />

WARNING<br />

EXPLOSION HAZARD<br />

Do not operate in an explosive atmosphere.<br />

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Explanation of Caution and Warning Notices<br />

Warning symbol marked on equipment. This symbol means “Attention! Refer<br />

to the manual.”<br />

Pinch Point – Keep hands, hair, and clothing clear of moving parts.<br />

Lifting Hazard – Single person lift could cause injury. Use assistance when<br />

moving or lifting.<br />

WARNING<br />

The WARNING notice denotes a hazard. It calls attention to a procedure,<br />

practice, or the like, that, if not correctly performed or adhered to, could<br />

result in personal injury. Do not proceed beyond a WARNING notice until<br />

the indicated conditions are fully understood<br />

CAUTION<br />

The CAUTION notice indicates an action which must be taken to prevent<br />

equipment damage or a serious loss of data. Do not proceed beyond a CAUTION<br />

notice until the indicated conditions are fully understood and met.<br />

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Chapter 7: Safety and Regulatory Information<br />

Avertissements en Français<br />

This section provides French translations of notices which may appear on the<br />

instrument or on other instruments used as part of the measurement system.<br />

AVERTISSEMENT<br />

POUR UNE PROTECTION CONTINUÉ CONTRE LES RISQUES<br />

D’INCENDIE, REMPLACER UNIQUEMENT PAR DES FUSIBLES<br />

DE MÊME TYPE ET AMPÈRAGE.<br />

AVERTISSEMENT<br />

POUR LA PROTECTION PERMANENTE<br />

CONTRE UN CHOC ÉLECTRIQUE, UNE<br />

BRÛLURE DES YEUX (RADIATION UV) OU DE<br />

LA PEAU, LAISSER LE COUVERCLE<br />

HERMÉTIQUEMENT FERMÉ LORSQUE<br />

L’APPAREIL EST SOUS TENSION.<br />

LAISSER REFROIDIR 5 MINUTES (APPAREIL<br />

ÉTEINT) AVANT D’ENLEVER LE COUVERCLE.<br />

AVERTISSEMENT<br />

SURFACES CHAUDES, LAISSER LE<br />

COUVERCLE HERMÉTIQUEMENT FERMÉ.<br />

POUR ACCÉDER, METTRE LA TEMPÉRATURE DU FOUR À<br />

ZÉRO, OUVRIR LE COUVERCLE ET LAISSER REFROIDIR 5<br />

MINUTES AVANT DE TOUCHER LA VERRERIE OU TOUTE<br />

SURFACE MÉTALLIQUE INTÉRIEURE.<br />

AVERTISSEMENT<br />

TOUT CONTACT AVEC LES HAUTES TENSIONS PEUT<br />

ENTRAINER LA MORT OU DES BLESSURES SÉVÈRES. CE<br />

PANNEAU NE DOIT ÊTRE ENLEVE QUE PAR UN<br />

RÉPARATEUR QUALIFIÉ.<br />

155


Operator’s <strong>Manual</strong><br />

Chapter 7: Safety and Regulatory Information<br />

Electromagnetic Interference<br />

FEDERAL COMMUNICATIONS COMMISSION (FCC) NOTICE<br />

This equipment has been tested and found to comply with the limits for a Class A digital device,<br />

pursuant to Part 15 of the FCC Rules. These limits are designed to provide reasonable protection<br />

against harmful interference in a commercial installation.<br />

This equipment generates, uses, and can radiate radio frequency energy and, if not installed and<br />

used in accordance with the instructions, may cause harmful interference to radio<br />

communications. Operation of this equipment in a residential environment is likely to cause<br />

harmful interference, in which case the user will be required to correct the interference at his<br />

expense.<br />

MODIFICATIONS<br />

The FCC requires the user to be notified that any changes or modifications made to this device that<br />

are not expressly approved by <strong>CETAC</strong> Technologies may void the user's authority to operate the<br />

equipment.<br />

CABLES<br />

Connections to this device must be made with shielded cables with metallic RFI/EMI connector<br />

hoods to maintain compliance with FCC Rules and Regulations.<br />

CANADIAN NOTICE<br />

This digital apparatus does not exceed the Class A limits for radio noise emissions from digital<br />

apparatus as set out in the interference-causing equipment standard entitled "Digital Apparatus"<br />

ICES-001 of the Department of Communications.<br />

AVIS CANADIEN<br />

Cet appareil numerique respecte les limites de bruits radioelectriques applicables aux appareils<br />

numeriques de Classe A prescrites dans la norme sur le materiel brouilleur: "Appareils<br />

Numeriques," NMB-001 edictee par le ministre des Communications.<br />

Explanation of Regulatory Marks<br />

Do not dispose in domestic household waste.<br />

The affixed label indicates that you must not discard this<br />

electrical/electronic product in domestic household waste, in compliance<br />

with the European Waste Electrical and Electronic Equipment Directive<br />

(WEEE, 2002/96/EC).<br />

For instructions on how to return end-of-life equipment, producer-supplied<br />

electrical accessories, or auxiliary items for proper disposal please contact<br />

the supplier or importer. In the event a supplier cannot be reached, contact<br />

<strong>CETAC</strong> Technologies customer service department at 1 (800) 369 2822.<br />

The CE mark is a registered trademark of the European Community. This CE<br />

mark shows that the product complies with all the relevant European Legal<br />

Directives.<br />

156


8 Glossary<br />

A Amperes, electrical current<br />

AAS Atomic Absorption Spectrometry<br />

Abs Absorbance (-log 10 T or 2-LOG 10 %T)<br />

ADC or A/D Analog-to-digital converter<br />

ADX-500 Optional autodilutor accessory<br />

ASX-500 A <strong>CETAC</strong> ASX-500 series autosampler, such as the ASX-510<br />

autosampler or ASX-520 autosampler<br />

Bar Unit of pressure. 1 bar = 100 kPa ≈ 14.5 psi<br />

Ar Argon carrier gas, chemical formula<br />

CH 3 HgCl Methyl mercuric chloride (or “methyl mercury”), chemical formula<br />

of a common organo-mercurial<br />

CLP Contract Laboratory Protocol (analysis protocol of U.S. EPA)<br />

cm Centimeter (10 -2 meter), unit of length<br />

Cold Vapor Direct Atomic Absorption Spectrometric analysis (at 253.652 nm) of<br />

Direct AAS or<br />

“head-space” gas from a stannous chloride or stannous sulfate<br />

CVAAS<br />

reactor using neither flame, nor plasma, nor furnace nor any other<br />

electro-thermal atomizer. CVAAS works only for the element<br />

mercury (Hg)<br />

Dia. Diameter<br />

DL Detection limit. Smallest statistically detectable concentration,<br />

where the absorbance, Abs (produced by that concentration),<br />

equals 3 times the standard deviation σ of the blank Abs<br />

DSP Digital Signal Processor<br />

ea. Each<br />

EOFM Electro-Optic Feedback Module; used to stabilize the Hg lamp<br />

EPA U.S. Environmental Protection Agency<br />

EPA-245.1 The standard EPA method of water quality analysis for measuring<br />

mercury (Hg)<br />

ETFE Ethylenetetrafluoroethylene (Tefzel), a polymeric tubing material<br />

157


Operator’s <strong>Manual</strong><br />

Chapter 8: Glossary<br />

g Gram, unit of mass or “weight”<br />

GCU Gas Control Unit, sets and regulates carrier gas flow rate<br />

GLS Gas-Liquid Separator<br />

HCl Hydrochloric Acid, chemical formula<br />

Hg <strong>Mercury</strong>, chemical symbol<br />

Hg 0<br />

Hg 2+<br />

<strong>Mercury</strong>, elemental (reduced) state<br />

Mercuric ion, mercury in +2 (oxidized) state, typically HgCl 2<br />

HgCl 2 Mercuric chloride, chemical formula<br />

HNO 3 Nitric acid, chemical formula<br />

Host The computer that controls operation of the instrument .<br />

Computer<br />

i.d. Inside diameter<br />

IDL Instrument Detection Limit. DL in ultra-clean, high purity acid media<br />

(for example, 7% HCl, “Ultrex II” grade). IDL is generally measured<br />

under “favorable” operating conditions and does not involve<br />

sample digestion or preparation steps. IDL indicates what the<br />

instrument is capable of doing, if not subjected to contamination,<br />

digestion loss, storage loss, or other sample collection/preparation<br />

errors or limitations<br />

KMnO 4 Potassium permanganate, chemical formula of oxidizing reagent,<br />

and mercury exhaust trap agent<br />

L Liter, unit of volume<br />

LED Light-Emitting Diode<br />

QuickTrace<br />

system<br />

The entire mercury analyzer system including the QuickTrace,<br />

autosampler, peristaltic pump, etc.<br />

mA Milliamperes (10 -3 amperes), electrical current<br />

MDL Method Detection Limit; DL measured under actual reagent purity,<br />

sample preparation, and storage conditions for samples, reagents,<br />

and containers in question. Calibration standards are generally<br />

prepared in the sample media and are carried through all sample<br />

digestion/preparation, storage and transfer steps, etc., as are<br />

samples. In the presence of significant contamination, small<br />

concentration detectability gets worse and the actual MDL should<br />

be redefined as 1/3 the contamination, but not less than the<br />

statistical MDL!<br />

mL Milliliter (cubic centimeter, cc, 10 -3 L), unit of volume<br />

mm Millimeter (10 -3 meter), unit of length<br />

MSDS Material Safety Data Sheet specifying chemical hazard type and<br />

level<br />

N 2 Nitrogen carrier gas, chemical formula<br />

Nafion® DuPont's porous polymer membrane which passes water vapor, but<br />

not Hg vapor.<br />

nm Nanometer (10 -9 meter), wavelength unit.<br />

158


ng Nanogram (10 -9 gram), mass or weight unit<br />

o.d. Outside diameter<br />

P Transmitted radiant power, photon flux at sample detector (after<br />

passing through sample)<br />

P 0 Incident radiant power, photon flux at reference detector (before<br />

passing through sample)<br />

PC Personal Computer<br />

PEEK Polyetheretherketone; a machined polymeric construction material<br />

Perma Pure Brand name of the dryer tubing which uses a DuPont Nafion®<br />

membrane.<br />

pg Picograms (10 -12 g), mass or weight unit<br />

PID Proportional Integral Differential. Description of a type of precision<br />

heater control device<br />

ppb Parts per billion (ng/mL, 10 -9 -6 g/mL, µg/L, 10 g/L), concentration<br />

unit<br />

ppm Parts per million (µg/mL, 10 -6 -3 g/mL, mg/L, 10 g/L), concentration<br />

unit<br />

ppt Parts per trillion (pg/mL, 10 -12 g/mL, ng/L, 10 -9 g/L), concentration<br />

unit<br />

psi Pounds per square inch. Pressure. 1 psi ≈ 0.068 bar. 1 bar = 100 kPa<br />

psig Pounds per square inch, gauge reading (above atmospheric<br />

pressure)<br />

PTU Precision-Timed Uptake<br />

Pump or PP Peristaltic Pump<br />

P-P Peak to Peak. A description of how signal noise is measured (One<br />

method)<br />

RMS Root Mean Square. A description of how signal noise is measured.<br />

RMS = 0.707 of peak amplitude (another method), approximately<br />

one standard deviation unit<br />

RSD Relative Standard Deviation. A measure of data precision or<br />

reproducibility<br />

SCR Stannous Chloride Reactor<br />

Sn Tin, chemical symbol. Typically as SnCl 2 reagent<br />

SnCl 2 Stannous chloride, chemical formula of reducing agent<br />

SRM Standard Reference Material, containing a certified, known mercury<br />

level<br />

T Transmittance (P/P 0 ), often %T or percent transmittance (P/P 0 x<br />

100%)<br />

TC “To Contain” Designation of a type of volumetric flask calibrated to<br />

accurately contain a specified volume of liquid<br />

TD “To Deliver” Designation of a type of volumetric flask or pipet<br />

calibrated to accurately deliver a specified volume of liquid<br />

159


Operator’s <strong>Manual</strong><br />

Chapter 8: Glossary<br />

UHP Ultra High Purity<br />

UV Ultraviolet; short wavelength region of spectrum below 370 nm<br />

(such as 253.7 nm)<br />

VAC Volts Alternating Current<br />

VDC Volts Direct Current<br />

XS A substantial concentration “excess” of one chemical reactant (over<br />

another)<br />

µg Micro-gram (10 -6 g), unit of mass or weight<br />

µL Micro-liter (10 -6 L), unit of volume<br />

µAbs Micro-absorbance units. (10 -6 Abs)<br />

160


Index<br />

autosampler<br />

data cables, 44, 46<br />

placement, 26<br />

power, 40<br />

probe installation, 36<br />

rinse solution, 79<br />

rinse station, 26<br />

sample tube, 61<br />

Z-drive, 31<br />

avertissements, 156<br />

avis Canadien, 157<br />

baseline correction, 91<br />

bulb. See lamp<br />

cleaning, 154<br />

cold shutdown, 101<br />

condensation. See humidity<br />

dimensions, 18<br />

disposal, 157<br />

dryer cartridge<br />

inspecting, 104<br />

Nafion membrane, 78<br />

overflow cleaning, 119<br />

replacing, 117<br />

water damage, 121<br />

earthing, 21<br />

earthquake precautions, 20<br />

electrical characteristics, 151<br />

EOFM, 124<br />

Ethernet setup, 45<br />

exhaust, 42<br />

FCC notice, 157<br />

footprint, 18<br />

fuse, 131<br />

gas pressure<br />

maximum, 42<br />

minimum, 70<br />

range 1, 98<br />

range 2, 99<br />

GLS<br />

cleaning, 112<br />

inspecting flow, 90<br />

installing, 53<br />

overflow, 71<br />

overflow recovery, 119<br />

parts of, 115<br />

tubing, 115<br />

wetting, 72, 73, 84<br />

grounding, 21<br />

hazards, 153<br />

chemical burn, 42, 71, 119<br />

electrical, 154<br />

inhalation, 20, 112<br />

mechanical, 153<br />

organomercurial, 80<br />

poison, 152<br />

humidity, 21, 150, 154<br />

ICES 001, 157<br />

installation category, 151<br />

integration limits, 140<br />

interference, 157<br />

IP address, 137<br />

IP Address, 50<br />

IP RESET button, 138<br />

IPSetup, 133<br />

LAMP ON indicator, 12<br />

lamp, mercury vapor<br />

current, 140<br />

replacement, 124<br />

warm-up, 82<br />

lamps<br />

power, 12<br />

LEDs. See lamps<br />

lifting, 22<br />

log book, 91<br />

mains disconnect, 153<br />

mercury vapor trap, 82<br />

inspecting, 43<br />

installing, 42<br />

refilling, 122<br />

Nafion. See dryer cartridge<br />

network setup, 45, 63<br />

OVER RANGE indicator, 12, 124<br />

over voltage category, 151<br />

PC setup, 63<br />

Perma Pure. See dryer cartridge<br />

physical characteristics, 18<br />

pollution degree, 150<br />

power<br />

requirements, 20, 151<br />

power cord, 152<br />

POWER indicator, 12<br />

reagent uptake tube, 61<br />

161


Index<br />

reducing agent, 69<br />

regulatory notices, 150<br />

return procedure, 147<br />

safety information, 150<br />

service, 147<br />

SnCl2, 69<br />

standby, 100<br />

supplies, 14<br />

temperature<br />

recommended, 17<br />

safe operating, 150<br />

tubing<br />

cell gas, 113<br />

kinks, 21<br />

unpacking, 21<br />

uptake tube (reagent), 61<br />

vibration, 20<br />

warranty, 147<br />

WEEE notice, 157<br />

work surface requirements, 20<br />

162


<strong>Manual</strong> Part Number 480195 Rev 2<br />

Printed in USA

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