CETAC M-7600 Mercury Analyzer Operator's Manual · Ultra-trace detection limits: < 0.5 ppt at 40 mL / min. carrier gas flow 1 Wide dynamic linear working range, ≅ 4 orders of magnitude.

CETAC M-7600 Mercury Analyzer

Manual Part Number 480195 Rev 2

Operator’s Manual

COPYRIGHT

© 2008, 2012 CETAC Technologies

480195 Rev 2 , October, 2012

CETAC Technologies authorizes its customers to reproduce, transmit, or store this document in its entirety, including this page, for the express purpose of installing, operating, or maintaining the product described herein.

CETAC Technologies Customer Service & Support 14306 Industrial Road Omaha, Nebraska 68144, USA Phone (800) 369-2822 (USA only) Phone (402) 733-2829 Fax (402) 733-1932 E-mail [email protected]

REVISIONS

CETAC Technologies strives to provide the scientific community with an unparalleled combination of effective technology and continuing value. Modular upgrades for existing instruments will continue to be a prime consideration as designs progress.

CETAC Technologies reserves the right to revise this document and/or improve products described herein at any time without notice or obligation. Warranty registration entitles the named owner exclusively to manual change pages/new editions as they are published.

TRADEMARK ACKNOWLEDGEMENTS

Windows is a registered trademark of Microsoft Corporation in the United States and other countries.

Nafion® is a registered trademark of DuPont (E.I. du Pont de Nemours and Company).

Perma Pure is a registered trademark of Perma Pure LLC.

DuPont™, Kapton®, Teflon®, Tefzel® and Viton® are trademarks or registered trademarks of E.I. du Pont de Nemours and Company.

PharMed and Tygon are registered trademarks of Saint-Gobain Performance Plastics.

Santoprene™ is a trademark of Exxon Mobil.

KIMWIPES is a registered trademark and KIMTECH SCIENCE is a trademark of Kimberly-Clark Worldwide, Inc

All other marks are the property of their respective owners.

Contents 1 Introduction .............................................................................................................. 7

Overview.................................................................................................................................... 7 About This Book ..................................................................................................................... 7

Who Should Use This Product ................................................................................... 7 Where to Go for More Information ................................................................................ 8 System Features ..................................................................................................................... 9 System Performance Characteristics .......................................................................... 10 Overview of the Mercury Analyzer .............................................................................. 11 Supplied Equipment ........................................................................................................... 13 Equipment and Supplies ................................................................................................... 14

Required Equipment and Supplies ........................................................................ 14 Recommended Supplies ............................................................................................. 15

2 Preparing for Installation ................................................................................. 17

Establishing Optimal Operating Conditions ............................................................ 17 Creating the Lab Environment ............................................................................... 17

Choosing a Location ............................................................................................................ 18 Space Requirements .................................................................................................... 18 Work Surface Requirements .................................................................................... 20

Ventilation Requirements ................................................................................................ 20 Power Requirements ......................................................................................................... 20 Unpacking the Mercury Analyzer ................................................................................. 21

3 Installing the Analyzer ....................................................................................... 25

Installation Overview......................................................................................................... 25 Step 1: Position the Mercury Analyzer and Autosampler.................................. 26 Step 2: Connect the Autosampler Peristaltic Pump to the Rinse Station .... 26 Step 3: Set Up the Autosampler ..................................................................................... 30 Step 4: Connect Power and Data Cables to the Back of the Mercury

Analyzer .......................................................................................................................... 39 Step 5: Connect the Carrier Gas Tubing ..................................................................... 40 Step 6: Install the Mercury Trap (KMnO4) ................................................................ 42 Step 7: Connect the Back of the Autosampler ......................................................... 44 Step 8: Connect to the Host Computer ....................................................................... 45

Summary ......................................................................................................................... 45 Installing a Secondary NIC in Your Own PC ...................................................... 45 Connecting the Communication Cables............................................................... 46 Configuring the Network Metrics .......................................................................... 46 Setting the IP Address for the Secondary NIC ................................................... 50 Changing the Subnet of the Mercury Analyzer................................................. 51 Connecting a Laptop Computer to the M-7600 ................................................ 52

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

M-7600 Mercury Analyzer Operator’s Manual

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Step 10: Connect the Peristaltic Pump on the Mercury Analyzer .................. 57 Installing the Peristaltic Pump Tubing ............................................................... 57 Installing the Mixing Tee and Drain Tees .......................................................... 59

Step 11: Power On and Verify Communication ...................................................... 63 To Configure the Network Connection ................................................................ 63 To Power On the System for the First Time (PC Configured by CETAC) 64 To Power On the System for the First Time (Customer-Supplied PC) ..... 64 To Test the Autosampler ........................................................................................... 68

Step 12: Fill the Rinse Solution Bottle ........................................................................ 68 Step 13: Fill the Reagent Bottle ..................................................................................... 69

Preserving the SnCl2 ................................................................................................... 69 Step 14: Adjust the Peristaltic Pump Tubing Clamp Tension (Optional) ... 70 Step 15: Check the Reagent Flow ................................................................................. 73 Step 16: Check the Sample Probe Flow ..................................................................... 73

4 Using the Analyzer ............................................................................................... 75

Theory of Operation ........................................................................................................... 75 Autosampler .................................................................................................................. 75 QuickTrace™ M-7600 Automated Mercury Analyzer .................................... 76

Software................................................................................................................................... 78 Preparing Reagents and Calibration Standards ..................................................... 79 Gas Parameters .................................................................................................................... 81 Starting the System............................................................................................................. 81

Mercury Vapor Lamp Warmup .............................................................................. 82 Turning Off the Mercury Vapor Lamp for System Warm-Up ..................... 82 System Warm-Up for Trace or Ultra-Trace Analysis ..................................... 82 System Warm-Up for ppb or Non-Ultra-Trace Analysis ............................... 83

Wetting the GLS .................................................................................................................... 84 Running the Interactive Demo ...................................................................................... 87 Overview of the CETAC QuickTrace™ Software ..................................................... 87

Learning More .............................................................................................................. 88 QuickTrace™ M-7600 Startup Summary ................................................................... 89 Setting Baseline Correction ............................................................................................ 91

Keeping an Instrument Log Book .......................................................................... 91 Viewing the Graphs ..................................................................................................... 92 Setting a One-Point Baseline ................................................................................... 92 Setting a Two-Point Baseline .................................................................................. 94

Summary of Gas and Liquid Flows for Analytical Ranges of the QuickTrace™ M-7600 ................................................................................................ 98

Placing the QuickTrace™ M-7600 in Standby Mode ......................................... 100 Cold Shutdown .................................................................................................................. 101

Summary of QuickTrace™ M-7600 Shut Down .............................................. 101

5 Maintaining the Mercury Analyzer ............................................................. 103

Maintenance Schedule ................................................................................................... 103 Daily Maintenance (Always Check Before Analysis) .................................... 103 Weekly Maintenance ................................................................................................ 104 Monthly Maintenance .............................................................................................. 104 Yearly Maintenance .................................................................................................. 104 Autosampler Yearly Maintenance....................................................................... 105

Removal or Inspection of the Sample Cell ............................................................. 105 Opening the Optics Access Panel ......................................................................... 105 Removing the Sample Cell ...................................................................................... 107

M-7600 Mercury Analyzer Operator's Manual

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Cleaning the Cell Windows ........................................................................................... 107 Quick Exposed Surface Cleaning ......................................................................... 107 Dismantling for Total Cleaning ........................................................................... 109

Cell Assembly...................................................................................................................... 109 Cleaning the Gas-Liquid Separator ........................................................................... 112 Changing the Cell Gas Tubing ...................................................................................... 113 Retubing the Gas-Liquid Separator .......................................................................... 115

GLS Inlet........................................................................................................................ 115 GLS Drain ..................................................................................................................... 116

Replacing the Perma Pure® Dryer Cartridge ........................................................ 117 GLS Overflow Recovery .................................................................................................. 119 Replacing the Hg Lamp Bulb ........................................................................................ 124

When to Replace or Service the Lamp .............................................................. 124 Cleaning the EOFM ................................................................................................... 124 Getting a Replacement Lamp ............................................................................... 125 Caring for the Lamp ................................................................................................. 126 Replacing the Lamp ................................................................................................. 126 Adjusting the Lamp Current ................................................................................. 129

Replacing the Fuse ........................................................................................................... 131

6 Troubleshooting the Mercury Analyzer .................................................... 133

Troubleshooting Communication Issues ............................................................... 133 Step 1: Check the Cable ........................................................................................... 133 Step 2: Use the IPSetup Tool to Check the Configuration .......................... 133 Step 3: Check the Subnet Configuration Using the Define QuickTrace

Hardware Tool .................................................................................................. 134 Step 4: Check for an IP address conflict ........................................................... 137 If the IPSetup Tool Does Not Find the M-7600 .............................................. 138 "Subnet of this PC and the M-7600 are Not Compatible" Error ............. 139

Cannot Zero Instrument ................................................................................................ 140 "Integration Adjustment Reached" Messages ...................................................... 140 Drifting Baseline ................................................................................................................ 140 Low Absorbance or No Mercury Response ........................................................... 141 No Liquid or Gas Flow .................................................................................................... 141

No Sample or Rinse Flow ....................................................................................... 141 No SnCl2 Flow ............................................................................................................. 142 No Drain Flow ............................................................................................................ 142 No Gas Flow or Low Gas Flow .............................................................................. 142

Double Peak with Low Absorbance .......................................................................... 142 Poor Reproducibility ....................................................................................................... 143 Noisy Baseline .................................................................................................................... 144 Bad DL .................................................................................................................................... 144 Sudden Standard Absorbance Rise During Run .................................................. 144 Poor Accuracy .................................................................................................................... 145 Returning the Product to CETAC for Service ........................................................ 146

Shipping the Product ............................................................................................... 146 Product Warranty Statement .............................................................................. 146 Returned Product Procedures .............................................................................. 147 Returned Product Warranty Determination ................................................. 147

7 Safety and Regulatory Information ............................................................. 149

Characteristics ................................................................................................................... 149 Environmental Characteristics ............................................................................ 149

M-7600 Mercury Analyzer Operator’s Manual

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Electrical Characteristics ....................................................................................... 150 Safety Notices ..................................................................................................................... 151

Replacement Parts .................................................................................................... 151 Chemical Hazards ...................................................................................................... 151 Power Cord Set Requirements .............................................................................. 151 Power Cord Safety Maintenance ......................................................................... 151 Grounding ..................................................................................................................... 152 Mains Disconnect ....................................................................................................... 152 Mechanical Hazards ................................................................................................. 152 Cleaning Instructions ............................................................................................... 153 Operating Environment .......................................................................................... 153 Explanation of Caution and Warning Notices ............................................... 154

Avertissements en Français ......................................................................................... 155 Electromagnetic Interference ..................................................................................... 156 Explanation of Regulatory Marks .............................................................................. 156

8 Glossary ................................................................................................................. 157

1 Introduction

Overview The CETAC QuickTrace™ M-7600 mercury analyzer measures trace levels of mercury in aqueous solution by Cold Vapor Atomic Absorption Spectrometry (CVAAS). CVAAS does not require heating the sample with a flame, plasma, or furnace. The mercury analyzer’s modular design permits remarkably easy maintenance access and a reduced countertop footprint. Sturdy construction, drift-stabilized double beam optics, thermal and electro-optical lamp stabilization, and an unusually stable “non-foaming” Gas-Liquid Separator (U.S. Patent #5,792,663) collectively afford exceptional structural integrity and signal stability. The QuickTrace™ M-7600 exhibits a high signal-to-noise ratio and ultra-trace detection limits for an absorbance system that is fully compliant with EPA CVAA methods such as 245.7, 245.1, 245.5, SW846 7470 and 7471.

About This Book This document describes the procedures for installing, using, and maintaining the analyzer.

This manual covers the following products:

CETAC QuickTrace™ M-7600 mercury analyzer

Who Should Use This Product

The primary audience for this manual consists of mercury detection and mercury measurement laboratory managers, chemists, technicians, field-service engineers and owners of the QuickTrace™ M-7600 mercury analyzer. To use this product effectively, you should have a basic knowledge of mercury analysis, at least a beginning level of computer experience, and a basic knowledge of chemical handling procedures including the handling of organomercurials.

Before operating the QuickTrace™ M-7600 analyzer, autosampler, or optional ADX-500 autodilutor, it is important to read this manual, the QuickTrace™ Software Manual, the Autosampler Operator’s Manual, and (if applicable) the ADX-500 Autodilutor Accessory Operator’s Manual.

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Chapter 1: Introduction

8

Where to Go for More Information In addition to this manual, you can refer to the following resources:

The QuickTrace™ Software Manual and built-in help

The M-7600 Mercury Analyzer PC Setup Guide

The CETAC Autosampler Operator’s Manual

The ADX-500 Autodilutor Manual (optional)

U.S. EPA Method 245.1; method for Hg determination in drinking water

U.S. EPA Method 245.7; Mercury in Water by Atomic Fluorescence Spectrometry

U.S. EPA, Office of Solid Wastes. SW846 Method 7470A; Mercury in Liquid Waste (Cold-Vapor Technique)

U.S. EPA, Office of Solid Wastes, SW846 Method 7471B; Mercury in Solid or Semisolid Waste (Cold-Vapor Technique)

American Society for Testing and Methods. ASTM D3223-91; Standard Test Method for Total Mercury in Water

The CETAC Technologies Web site: www.cetac.com

CETAC Technologies Customer Service and Support:

1 (800) 369-2822 (USA only)

1 (402) 733-2829

1 (402) 733-1932 (Fax)

E-mail: [email protected]

mailto:[email protected]�

CETAC QuickTrace™ M-7600 Mercury Analyzer


9

System Features The QuickTrace™ M-7600 incorporates the following features to form an automated, integrated mercury analysis system.

Computer-controlled four-channel high-performance peristaltic pump (12-roller pump head).

Ozone-free Hg Lamp. No lamp ventilation is needed.

Thermally controlled Hg lamp housing (for a stabilized Hg vapor lamp).

Stable high performance Gas-Liquid Separator (GLS). (U.S. Patent #5,792,663). Non-foaming/non-bubbling “thin liquid film” GLS design, which allows trouble-free direct analysis of blood, urine, and fish tissue digests as well as standard water and waste analysis.

Rigid, shock and vibration-isolated optical rail (mounting the Hg lamp, collimator lens, absorption tubes, camera, CCD detector, and A/D converter).

Precise, self-aligning optical mounts, no optical alignment required, maximizing the convenience of instrument baseline zeroing. This design extends maintenance intervals without loss of performance.

Long path (220 mm) absorbance cells.

Hg lamp electro-optical feedback beam utilizing a high-performance solid-state detector for ultra-fine lamp stabilization.

Fixed optical interference filters, three each (254 ± 2 nm wavelength, 20% T, 12.7 mm dia.). No moving parts.

Standard Perma Pure® dryer cartridge eliminates the need for Mg(ClO4)2 drying agent.

Stabilized double beam optics - traditional double-beam (sample and reference) with a CCD detector.

Internal ADC (Analog-to-Digital Conversion).

High-rate data sampling.

Computer controlled system shutdown/standby routines.

Integrated optional autosamplers for accommodation of calibration standards and up to 720 samples.

Ethernet communications.

Gas exhaust Hg vapor safety trap (solid crystalline KMnO4).

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System Performance Characteristics Ultra-trace detection limits: < 0.5 ppt at 40 mL / min. carrier gas flow1

Wide dynamic linear working range, ≅ 4 orders of magnitude.

. (Direct steady state absorbance mode, without pre-concentration by gold amalgamation).

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

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

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

99% Confidence Accuracy @ 5 ppt; ±3.1%

99% Confidence Accuracy @ 20 ppt; ±4.3%

Sample Throughput < 3.5 min/sample at IDL

Ultra-low drift rates ≤ 300 µAbs/hr (after warm-up) raw uncorrected analog baseline on-screen drifts.

Ultra-low short-term absorbance noise ≤ 200 µAbs (10-5 Abs).

0.1% “raw” Hg lamp stability (single beam output).

Unusually fast washout ≈ 240 sec. from 1ppm Hg, at 1000 mL/min gas flow.

Mercury Response: ≥ 14,000 µAbs / ppb2

at 100 mL/min carrier gas flow.

1 One hour minimum warm-up using the standard Nafion® dryer and a gas flow equal to 40 mL/min along with prescribed tubing and reagents. Using pump speed, uptake and rinse times specified for standard Nafion® dryer in Table 4-1 (p. 72), and ≥12 s integration cycle selected on the "flattest" portion of the peak time profile. 2 Using prescribed tubing, reagents, and pump speed.



11

Overview of the Mercury Analyzer

Figure 1-1 M-7600 Mercury Analyzer—Front View.

Figure 1-2 M-7600 Mercury Analyzer—Front View with Autosampler.

Power and Status Lights

Peristaltic Pump

Autosampler (ASX-520 is shown)

Reagent Bottle

Rinse Bottle

Sample Probe

Perma Pure® Dryer Cartridge

Gas-Liquid Separator (GLS)

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Figure 1–2 M-7600 Mercury Analyzer —Back View of Complete System.

Figure 1-3 M-7600 Mercury Analyzer —Electrical Connectors.

The following components are located on the front of the mercury analyzer (see Figure 1-2).

POWER Indicator. The top blue LED indicates that the analyzer is connected to a power source and turned on.

LAMP ON Indicator. Indicates when the internal mercury vapor lamp is turned on.

OVER RANGE Indicator. Indicates that the internal mercury vapor lamp is drawing more than the recommended amount of current. This LED will glow for a few seconds while the mercury lamp warms up when the mercury analyzer is first turned on and the QuickTrace™ software is started or any time the lamp is off and then powered on via software controls.

Perma Pure® Dryer Cartridge. Uses a DuPont Nafion® membrane to remove humidity from the sample gas.

Gas-Liquid Separator (GLS).

Front Cover. Protects the GLS and dryer cartridge. An LED lamp illuminates the area behind the cover whenever the mercury analyzer is turned on.

M-7600 Power Switch

Autosampler Power Switch

Electrical Connectors

Autosampler Peristaltic Pump

Mercury Trap

M-7600 Power Switch

M-7600 Power Cord

Ethernet Port Auxiliary I/O Ports

Auxiliary Input Port

Auxiliary Power Ports



13

Peristaltic Pump. A four-channel peristaltic pump is built into the front of the mercury analyzer.

The following components are located on the back of the analyzer:

POWER Switch. Turns power to the M-7600 mercury analyzer on and off. This switch also controls power to the autosampler, when powered through the mercury analyzer.

Gas Ports. Gas inlet and exhaust ports.

Mercury Trap. The trap scrubs mercury from the exhaust gas.

The following electrical connectors are located on the back of the analyzer:

Ethernet Port. The Ethernet port is used to interface the mercury analyzer with the host computer.

Auxiliary Communication Ports. The two AUX I/O ports and one AUX INPUT port are reserved for use with other CETAC instruments.

Power Output Connectors. Provides power for the autosampler and for an optional auxiliary device.

Supplied Equipment The following standard components are supplied with the mercury analyzer:

M-7600 Mercury Analyzer.

CD. The CD contains:

QuickTrace software This manual Other application-specific information

Gas-Liquid Separator.

Perma Pure® Dryer Cartridge. Uses a DuPont Nafion® membrane to remove humidity from the sample gas. The cartridge is pre-installed in the mercury analyzer.

KMnO4 Absorbent Trap. This scrubs mercury from the exhaust gas. The KMnO4 is not included.

Bottles. One reagent bottle and one rinse bottle are provided.

PCI Ethernet Adapter Board.

Power Cord and Cables. An Ethernet cable, a power cord for the mercury analyzer, and a power cord for the autosampler are supplied.

Depending on how the system was ordered, the following optional equipment may be supplied:

Computer. The mercury analyzer may be ordered with a computer which is pre-configured with the QuickTrace™ software.

CETAC ASX-520/260/130 Autosampler.

CETAC ADX-500 Autodilutor.

ENC-500 Enclosure.

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The computer, autosampler, and optional accessories have their own manuals (printed or on CD-ROM). Before using the equipment, read those manuals to understand the precautions you must take to avoid possible hazards.

Equipment and Supplies

Required Equipment and Supplies

Inert Gas Regulator.

Two-stage, 10-200 psig (70-1380 kPa) secondary pressure gauge, with plumbing couple for either a cylinder or Dewar capable of delivering 150 psig (1040 kPa).

AC Power Strip.

Surge protected with six outlets, 15-20 A.

Cylinder or Dewar, UHP Nitrogen or Argon Gas.

Ultra-high purity, dry, research grade N2 or 99.999% purity Ar. The QuickTrace™ M-7600 has a user replaceable 2-micron filter, which prevents damage from particulates to the internal gas control components.

Mercury Standard Solution.

1000 ppm (minimum order quantity).

Hydrochloric Acid Trace Metal Grade (37%).

Trace metal HCl will be used in the preparation of Hg standards, SnCl2 reagent and in some method applications. If an application is more demanding, a better grade of acid may be needed (for example, double distilled).

Nitric Acid Trace Metal Grade (68-70%).

Trace metal HNO3 will be used in sample preparation, cleaning glassware (lab glassware and the QuickTrace™ Gas-Liquid Separator) and added to the QuickTrace™ rinse solution to help maintain the cleanliness of the system during operation.

Stannous Chloride (Crystals, Di-Hydrate).

Two 500g containers minimum order, “suitable for Hg determination.” The stock SnCl2 is introduced into the QuickTrace™ at a steady flow rate and therefore any mercury contamination will be negated during the instrument zero.

Potassium Permanganate. Solid, Crystalline.

The least expensive available grade at a minimum quantity is sufficient unless it is also to be used for oxidative sample preparation. This low-grade reagent stock is sufficient to fill a safety trap for retention of Hg vapor exhaust from the instrument.

2-propanol. High Purity, “Spectrophotometric” Grade.

2-propanol will be used for cleaning the optical cells and cell windows.

WARNING



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KIMTECH SCIENCE™ KIMWIPES® Delicate Task Wipers.

Additional Chemical Compounds.

The sample preparation procedures of the intended analytical method may require additional chemical compounds. Refer to published method specifications.

Recommended Supplies

Volumetric flasks 100 mL class A (TC) six each.

Volumetric flasks 1000 mL class A (TC) two each.

Precision air displacement micropipettes, 10 to 10,000 µL (TD).

Replacement tips for micropipettes.

Disposable plastic dropping pipettes.

Graduated cylinders, 10 and 100 mL.

Polypropylene or polyethylene bottle with Cap, 1 L.

Weighing balance, top loading, 0.1 g readability (or better), any available capacity will work (1.1 kg capacity is good).

Laboratory scoopula and large spatula.

Stopwatch (for measuring liquid uptake rates).

Stirring rod.

Powder funnel, wide bore stem, small overall size.

Wrenches, adjustable 12" and 6".

Screw drivers:

1 small Phillips 1 medium Phillips 1 long-shank medium flat-blade 1 small thin flat-blade

Deionized water.

Flow meter 0 – 1,500 mL/min. with 1 mL/min. readability, calibrated to user’s choice of carrier gas (Ar or N2).

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2 Preparing for Installation

Installing the analyzer requires preparation. Before you install the analyzer, you should evaluate the physical arrangement of the laboratory to choose a suitable location. Once you choose a location, you must carefully unpack the analyzer prior to beginning the installation.

This chapter discusses what requirements must be met when you choose a location. It also describes how to unpack the equipment before installation.

Establishing Optimal Operating Conditions The mercury analyzer operates reliably even under less than ideal conditions. It is not, however, indestructible. Malfunction or damage can occur if specific operating conditions are not met. Meeting these conditions requires that you create the proper lab environment, replace analyzer components that wear out under normal use, and purchase the appropriate supplies for use with the analyzer.

NOTE

Damage or malfunction that results from unsatisfactory operating conditions may constitute misuse and abuse and be excluded from warranty coverage.

Creating the Lab Environment

To create satisfactory operating conditions in your lab environment, follow these guidelines:

Operate the analyzer in a conventional lab environment where the temperature is 60–90 °F (15–32 °C), the humidity is 20–70% non-condensing, and the unit is not exposed to excessive flammable or corrosive materials.

Avoid rough handling of the analyzer. If possible, do not expose the analyzer to vibration or shock.

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Chapter 2: Preparing for Installation

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Protect the analyzer from long-term exposure to condensation, corrosive materials, solvent vapor, continual standing liquids.

Observe the same general electrostatic discharge precautions as with any other integrated circuit electronic devices. Low humidity environments, especially when combined with static-generating materials, require maximum care.

Discharge static buildup and ground to the analyzer base or cabinet before performing any maintenance. Do not touch or short-circuit bare contacts or connectors.

Avoid using the analyzer if strong electromagnetic interference or radio frequency interference is present. Interference fields can cause erratic operation of the analyzer.

Choosing a Location

Space Requirements

The QuickTrace™ M-7600 Mercury Analyzer System includes the base unit, PC with monitor, reagent and rinse bottles, and an optional autosampler.

A typical system requires a minimum footprint for countertop installation of 183cm (6’) X 31cm (2’) X 91cm (3’) (W x D x H). A floor space of 1’ (30cm) X 1’ (30cm) is required for the liquid waste receptacle. The space for the waste can be directly below the analyzer, or directly in front of the lab bench and in line with the peristaltic pump.

Figure 2-1 Footprint of QuickTrace™ M-7600 Mercury Analyzer with ASX-520 Autosampler.

CAUTION

86 cm (34 inches) 183 cm (6 feet)



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Figure 2-4 Dimensions of the QuickTrace™ M-7600 Mercury Analyzer.

The work surface should be at least 61 cm (24 inches) deep if it is accessible from both front and back. If the work surface is against a wall, it should be at least 76 cm (30 inches, if possible) deep. If possible, allow at least 15 cm (6 inches) behind the system for cable egress, ventilation, and access to the power switches.

20 cm (7.9 inches)

56 cm (22.0 inches)

46 cm (18.1 in)

71 cm (28 inches) 142 cm (56 inches)

71 cm (28 inches) 142 cm (56 inches)

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Always position the equipment so that it is easy to disconnect the power cord.

Work Surface Requirements

The analyzer must be placed on a sturdy countertop or table. It is not recommended to place the analyzer on a wheeled cart or folding table.

If the analyzer is to be used in an earthquake zone, choose a location or secure it so that it will not fall and cause injury or damage during an earthquake.

Ventilation Requirements During operation, the QuickTrace™ M-7600 internally contains trace amounts of mercury vapor. To prevent inhalation of the vapor, the QuickTrace™ M-7600 uses a solid KMnO4 absorbent trap located on the back of the instrument. This trap absorbs the mercury vapor prior to final exhaust; therefore no extra ventilation is required beyond that of a standard laboratory environment.

INHALATION HAZARD Gases exhausting from the QuickTrace™ M-7600 cabinet prior to the external Hg vapor trap (affixed to the rear cabinet panel) contain traces of mercury vapor and will cause injury if inhaled. Do not run the QuickTrace™ M-7600 unless exhausted gas is properly “scrubbed” or removed. Fill, maintain, and use the provided KMnO4 absorbent trap or run a transfer line to a fume hood.

The ambient temperature should be kept as stable as possible. Locating the QuickTrace™ M-7600 directly in the path of an air conditioner or heater vent may cause baseline drift, and is not recommended.

NOTE

Due to the likelihood of accelerated damage from corrosion and dust, locating the QuickTrace™ M-7600 in a fume hood with stagnant air automatically voids the warranty.

Power Requirements The QuickTrace™ M-7600 mercury analyzer includes a built-in switching power supply which supports line voltages in the range 100-240 VAC at frequencies of 50-60 Hz. See “Electrical Characteristics” on page 150 for detailed power requirements.

The autosampler is powered by the M-7600's AUX POWER output. See the autosampler manual for more details.

The power requirements for the computer can be found on the label affixed to the bottom of the computer, or in the computer manual which can be found on the computer CD.

Place the QuickTrace™ M-7600 within 1.2 meters of a standard power outlet. Ensure that you position the analyzer so that the location where the power supply cord plugs into it is easily accessible (is not blocked) and it can be

WARNING



21

quickly disconnected if needed. In case of hazard, the analyzer should be disconnected from the power source.

Three power outlets may be required, one each for the QuickTrace™ M-7600 mercury analyzer, computer, and monitor. (An AC surge protected power strip with six or more outlets will suffice).

The supplied power cord meets the requirements of the country where the instrument was purchased. If the instrument is to be used in a country other than the one specified at the time of ordering, obtain a new power cord set that meets the requirements of that country.

SHOCK HAZARD This equipment is designed for connection to a grounded (earthed) outlet. The grounding type plug is an important safety feature. For continued protection against electrical shock or damage to the instrument, do not disable this feature.

Do not apply power to the power supply until ready to operate the analyzer.

Unpacking the Mercury Analyzer Inspect external packaging upon receipt for signs of shipping damage. Inspect all items during unpacking and notify the carrier immediately of any concealed damage.

If the system is shipped or removed from storage during cold weather, allow the packaged equipment to equilibrate to room temperature before opening and exposing to warm, humid air. It is usually sufficient to provide four to eight hours for this purpose.

EQUIPMENT DAMAGE FROM CONDENSATION If condensation forms on or inside the analyzer, allow it to dry thoroughly before connecting it to a power source and operating it. Failure to do so may cause equipment damage.

1 Remove the packing checklist from the shipping container, and check off items against it. Leave accessories in the packing until you are ready to install them.

NOTE

Keep the factory packaging for use in case the product ever needs to be returned or shipped to another location.

2 Open the box which contains the M-7600.

WARNING

CAUTION

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3 Remove the upper piece of foam.

Figure 2-5 Opening the Box and Removing the Packaging.

4 Ask an assistant to help you lift the M-7600 from the box.

LIFTING HAZARD Two people are required to lift the M-7600 when it is in an awkward position such as in its box. Lifting should be done with a person situated on either end of the instrument.

Figure 2-6 Lifting the M-7600 Mercury Analyzer.

WARNING



23

5 Remove the piece of foam from inside the door of the M-7600.

Figure 2-7 Removing Foam from the Door.

6 Store the packaging in case you need to ship the mercury analyzer in the future.

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3 Installing the Analyzer

Installation Overview

Figure 3-1 Front View of QuickTrace™ M-7600 with Autosampler.

Figure 3-2 Rear View of QuickTrace™ M-7600 with Autosampler.

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Chapter 3: Installing the Analyzer

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Step 1: Position the Mercury Analyzer and Autosampler

1 Position the mercury analyzer.

Keep in mind the factors listed in “Choosing a Location” on page 18. You will need easy access to the back of the analyzer as you make the connections.

2 Place the autosampler next to the QuickTrace™ M-7600 mercury analyzer.

Leave a 1-centimeter gap so that vibration from the autosampler will not be transmitted directly to the mercury analyzer, and to facilitate passage of tubing.

Step 2: Connect the Autosampler Peristaltic Pump to the Rinse Station It is easiest to connect the rinse station tubing to the autosampler's built-in peristaltic pump before other cables and tubing get in the way.

In most cases, rinse solution will be “recycled” by returning it to the rinse solution bottle. If necessary, rinse solution can be pulled from a fresh bottle and used solution returned to a waste container.

Note that rinse solution flows up through the rinse station.

Figure 3-3 Autosampler Rinse Station.

Rinse Drain Port

Rinse Intake Port



27

1 The tubing from the output of the pump to the rinse station intake port is pre-connected at the factory.

Figure 3-4 Pump Output to Rinse Intake Port.

2 Locate in the completion kit the 6 mm (¼") OD Tygon® tubing. The tubing will need to be cut to the appropriate lengths.

3 Cut a 38 cm (15") length of tubing. This will run between the drain port of the rinse station and the rinse input of the peristaltic pump.

4 Connect one end to the input of the outer pump channel.

The pump rotates counterclockwise, so the inputs are on the top and the outputs are on the bottom.

Figure 3-5 Pump Input Connection from Rinse Drain.

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5 Connect the other end to the drain of the rinse station.

Remove the rinse station and press the tubing very firmly so that it completely covers the barb of the fitting. It helps to use your other hand to apply counter-pressure.

Figure 3-6 Rinse Station Drain Connection.

Figure 3-7 Replacing the Rinse Station.



29

Figure 3-8 Rinse Station in Place.

6 Cut an approximately 102 cm (40 inch) length of tubing to connect the input of the pump to the bottle of rinse solution. The tubing should be long enough to reach the bottom of the rinse bottle. This tube will draw rinse solution from the bottle.

7 Connect one end of this tube to the remaining input channel of the pump.

Figure 3-9 Pump Input Connection.

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8 Cut an approximately 86 cm (34 inch) length of tubing to extend from the remaining pump output to the bottle of rinse solution. The tubing should extend a few inches inside the rinse bottle, but should remain above the liquid surface. This is the rinse solution drain tube.

Figure 3-10 Pump Output Connection and Liquid Flow Direction.

SHOCK HAZARD In the steps which follow, pay attention to keep the tubing below all of the wires. Move the tubing, if necessary, so that any leaking liquid will not be directed onto electrical cables or connectors.

Step 3: Set Up the Autosampler

Ensure the power cord is not connected before proceeding with installation.

See the Autosampler Operator’s Manual, included on the CD, for additional instructions and safety information. You may also refer to the printed Z-Drive Assembly Quick Installation Guide which comes with the autosampler for more information on installing the Z-drive assembly.

WARNING

WARNING



31

The Z-drive is driven by a length of cable (line) which is made of solid Nylon 101 (or in some cases, PEEK.)

Do not allow the cable to bend sharply. Avoid pushing up on the slider or pushing on the Z-drive cable.

Do not tighten the thumbscrews with anything other than your fingers.

1 Locate the Z-drive assembly.

Figure 3-11 Z-Drive Assembly (Appearance May Vary Slightly Depending on Autosampler Model).

2 Slide the Z-drive assembly onto the autosampler arm.

Figure 3-12 Sliding the Z-Drive Onto the Arm of the Autosampler.

CAUTION

CAUTION

Sleeve (Protects Z-Drive Cable)

Sample Probe Home flag

Y-Axis Slider

Z-Axis Slider

Sample Tube

Z-Drive Cable

Guide Block

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3 Slide the Z-drive assembly onto the Y-axis leadscrew nut (the black block which moves back and forth along the arm). Lift the bushings with your fingernails to get them over the edge of the leadscrew nut.

Figure 3-13 Lifting the Bushings Over the Edge of the Leadscrew Nut.

4 Secure the Z-drive assembly to the Y-axis leadscrew nut by tightening the thumbscrews with your fingers. Never use tools to tighten the thumbscrews.

Figure 3-14 Tightening the Thumbscrews.



33

5 Slide the cable onto the rotor on the back of the autosampler (Figure 6).

Figure 3-15 Sliding Z-Drive Cable into Rotor Groove.

6 Secure the guide block to the back of the autosampler with 2 black-capped thumbscrews (Figure 7). Note that it is important to install the guide block in the correct orientation.

Figure 3-16 Securing Block to Back of Autosampler.

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7 Turn the rotor clockwise as far as it will go. This will raise the Z-drive to its highest position. (To avoid damaging the drive cable, always raise or lower the Z-drive by moving the rotor, rather than by pushing or pulling on the Z-drive itself.)

Figure 3-17 View of Rotor with Z-Drive at Highest Position.

8 Gently move the Z-axis slider until the gap between the slider and cap is approximately 2 mm (3/32").

With the Z-drive in its highest position, there should be a gap between the Z-axis slider and the top cap of the Z-drive of approximately 2 mm (~ 3/32 inch). If this is not the case, see the Autosampler Operator's Manual for instructions on how to adjust the Z-drive travel.

Figure 3-18 View of Gap Between Probe Bracket and Cap.

2 mm (3/32”)

Stator Stop

Rotor Pin



35

9 Hold the cable flat against the rotor and secure the cable by tightening thumbscrew on the rotor. Maintain the 2 mm (~ 3/32 inch) gap while the rotor pin is making contact with the stator stop (full clockwise rotation of rotor). The thumbscrew should be as tight as possible using just your fingers.

Figure 3-19 Securing Cable to Rotor.

10 Rotate the rotor back and forth to ensure that it moves freely. Ensure that the full width of the cable is under the clamp.

Figure 3-20 Verifying Cable Movement and Cable Clamp.

Clamp

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11 Insert the clamp into the slot in the Z-drive. Slide the probe into the Z-drive, through the hole in the clamp, and tighten the clamp with your fingers.

Figure 3-21 Tightening the Clamp Which Holds the Probe to the Z-Drive.

If the clamp doesn't tighten enough to hold the probe in place, reverse the orientation of the knurled nut:

Figure 3-22 Clamp Oriented Correctly.

12 Loosen the clamp and adjust the position of the probe so that it is about 2 mm (3/32 inch) above the top of the rinse station when the Z-drive is in its highest position.

You can use a large coin, such as a U.S. quarter, to help measure this gap. The exact distance is not critical, but the probe needs to be high enough that it will not hit anything when it moves from place to place.

Threads Visible

Lip Without Threads

Hole for Sample Probe



37

Figure 3-23 Probe Position with Z-Drive in Highest Position.

13 Center the probe over the rinse station and rotate the rotor counterclockwise to lower the probe into the rinse station.

14 Use the provided spiral wrap to secure the sample tube to the Z-drive cable about 5 cm (2 inches) above the top of the Z-drive. There should be just a little curve to the free sample tube when the probe is lowered, and a loop when the probe is raised.

The sample tube should naturally curve away from the probe so that it won't rub or get caught. If necessary, loosen the probe and rotate it so that the sample tube looks like the pictures below:

Figure 3-24 Securing the Sample Tube.

2 mm

Slight Curve Away from

Probe

Loop

Spiral Wrap

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15 Use the other spiral wrap to secure the sample tube to the cable at its highest point.

Figure 3-25 Securing the Sample Tube.

16 Moisten a Kimwipes wiper with 10% HNO3 and wipe the probe to remove any oil. This is needed so that aqueous samples do not adhere to the probe causing sample-to-sample contamination or rinse contamination.

17 The Z-drive assembly and sample probe are now properly installed on the autosampler.



39

Step 4: Connect Power and Data Cables to the Back of the Mercury Analyzer

1 Locate the plastic shipping bag labeled “Completion Kit – QuickTrace™ M-7600.” It contains various power and data cables, small parts, tubing, fittings, computer CD-ROM, etc.

You will be locating supplies from in kit for throughout the installation process. It is recommended to leave the parts in this bag, in their original packaging, until you need them.

2 Place the autosampler power switch in the OFF position.

3 Place the mercury analyzer power switch in the OFF position.

Figure 3-26 Power Switch

4 Connect the line cord to the connector on the back of the mercury analyzer.

If the cord is not of the correct type for your country, contact CETAC Technologies. See “Power Cord Set Requirements” on page 151.

Figure 3-27 Power Cord Connected to Mercury Analyzer

5 Connect the power cord into a grounded surge protected power strip.

6 Plug the surge protected power strip into the AC outlet receptacle.

Do not turn on the power switches yet.

M-7600 Power Switch

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7 Connect the 5-pin end of the autosampler power cable to the back of the mercury analyzer.

Figure 3-28 Autosampler Power Cable Connected to Mercury Analyzer.

8 Plug one end of the Ethernet cable into the mercury analyzer.

Figure 3-29 Ethernet Cable Connected to Mercury Analyzer.

Step 5: Connect the Carrier Gas Tubing

1 In the completion kit bag, find the brass 2-micron gas filter, with associated brass Swagelok™ fittings, and a short section of ETFE tubing (attached to the filter).

2 Determine how far the QuickTrace™ M-7600 is located from the gas supply (UHP nitrogen or argon). Allow a generous service loop of 1/8" nylon tubing from the roll provided the likely event of system placement changes or maintenance. This will allow the system to be slid forward for cell maintenance without disconnecting the gas tubes.



41

3 Connect one end of this tube to the gas inlet side of the 2-micron brass filter and tighten the Swagelok™ fitting securely.

Figure 3-30 Completed Assembly of Gas Inlet Tubing with Filter.

NOTE:

A 2-micron in-line filter must always be used. The 2-micron filter has been selected for minimal pressure drop and minimal flow fluctuation. Do not substitute other filters.

4 Connect the ETFE tube into the bulkhead fitting labeled “GAS INLET.” Make sure that the flow arrow on the gas filter is pointing in the direction to the gas in fitting.

Tighten the fitting as tight as you can get it using your fingers. (This fitting needs to be very secure, but do not use pliers to tighten it.)

Figure 3-31 Carrier Gas Inlet Tubing Connected to Mercury Analyzer.

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5 Connect the other end of the nylon tube to the gas supply regulator, using ¼" NPT 1/8" Swagelok™ fitting provided.

Exceeding 825 kPa (120 psig) gas supply pressure to the QuickTrace™ M-7600 may rupture the bulkhead fittings, causing the unit to malfunction.

Use only “research-grade”, “dry” UHP Nitrogen or Argon. Do not use “welding” grade gases - these may permanently damage the QuickTrace™ M-7600.

Step 6: Install the Mercury Trap (KMnO4) A tube filled with crystalline potassium permanganate will serve as the mercury vapor trap. The vapor trap will clean the QuickTrace™ M-7600 exhaust vapors, to prevent the release of mercury vapor into the lab atmosphere.

INHALATION HAZARD Do not operate the mercury analyzer unless the mercury trap is in place and functioning correctly.

1 In the plastic bag labeled “Completion Kit - QuickTrace M-7600,” find the polyethylene tube with a seven inch (17.8 cm) length of dark Viton® tubing attached to one end.

2 Remove one end cap from the polyethylene tubular body. Do NOT remove the heatshrink wrapped Luer fitting from the end cap.

3 Inspect both end cap interiors to ensure that the ends are lightly plugged with fine glass wool. If not, lightly pack a small, loose wad of fine glass wool into the small i.d. section of each cap. Pack enough glass wool to stop the potassium permanganate from filtering through, but not restrict the gas flow.

4 Put on protective eyewear and gloves.

5 With the glass wool in place, use a powder funnel to fill this tube with dry crystalline solid potassium permanganate (KMnO4). While filling, have one end fully capped, hold the other end straight upward, and use the powder funnel to guide the KMnO4 crystals into the tube. Fill to the top, tapping a finger lightly on the tube to settle the KMnO4, and finally place the end cap on securely.

CHEMICAL BURN HAZARD Be sure to wear protective eyewear and safety gloves when handling chemicals.

6 Snap the filled mercury trap into the black holders.

CAUTION

CAUTION

WARNING

WARNING



43

7 Attach the black Viton® tube with fitting to the connection labeled “GAS EXHAUST.”

Figure 3-32 KMnO4 Absorbent Trap Connected to Mercury Analyzer.

The mercury vapor trap needs to be cleaned and refilled when the brown color approaches the open end. This is the formation the MnO2 as the KMnO4 is reduced. The potassium permanganate may last at least one year depending on frequency of use, except in the unlikely event of a major overflow accident in the QuickTrace™ M-7600.

NOTE

So long as the KMnO4 is dry, free flowing (not caked), dark purple crystals, it is perfectly OK.

POISON HAZARD The mercury vapor trap contains potassium permanganate (KMnO4) and may contain mercury. Handle and dispose of the used KMnO4 according to your laboratory’s procedures and your country’s hazardous waste regulations.

WARNING

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Step 7: Connect the Back of the Autosampler

1 Connect one end of the USB cable to the autosampler.

Figure 3-33 USB Cable Connected to Autosampler.

2 Connect the power cable to the autosampler.

This is the cable which was connected in step 7 on page 40. The autosampler will be powered by the automatic switching power supply within the M-7600.

Figure 3-34 Power Cable Connected to Autosampler.



45

Step 8: Connect to the Host Computer The CETAC M-7600 mercury analyzer is controlled by a PC through an Ethernet connection.

CETAC recommends that this PC be equipped with two network cards. One card is used for communication with your laboratory network, and the other card is used exclusively for communication with the M-7600 mercury analyzer.

In most cases, a PC is supplied with the mercury analyzer, and this PC has two network cards.

NOTE

In most cases, CETAC will pre-configure the network cards for your laboratory. If you were not able to supply the necessary network information to CETAC, or if you will be supplying your own PC, then set up the network cards yourself as described below. If the PC is already set up, skip to “Step 9: Install the Gas-Liquid Separator (GLS)” on page 53.

If you wish to use a laptop computer or if you cannot install a secondary network card, see “Connecting a Laptop Computer to the M-7600” on page 52.

The information in this section is also supplied in the CETAC M-7600 Mercury Analyzer PC Setup Guide which is included with the mercury analyzer.

Summary

Primary NIC Secondary NIC

Connects to Laboratory network 192.168.0.149 (address of the M-7600)

Interface Metric 100 2

Default IP Address Obtain automatically 192.168.0.100 (address of the PC)

Installing a Secondary NIC in Your Own PC

Most PC’s come with a single network interface, but a secondary network interface card (NIC) can easily be installed in most desktop and tower PCs. To install the second NIC:

1 Power off the PC.

2 Install secondary network interface card (NIC), following the manufacturer's instructions.

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

3 Install all of the PC peripherals such as the keyboard, mouse, and monitor.

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Connecting the Communication Cables

Figure 3-35 PC Before Connection to the M-7600.

1 Connect the USB cable from the autosampler to the computer.

2 Connect the Ethernet cable from the mercury analyzer to the computer.

Figure 3-36 PC After Connection to the M-7600.

Configuring the Network Metrics

The network metrics for each NIC on the PC must be configured for optimal communications with the M-7600 mercury analyzer.

These instructions apply to the Microsoft Windows 7 and Windows XP operating systems.

Power Cord

Keyboard and Mouse

Monitor (Cable Not Shown)

USB to Autosampler

Ethernet to M-7600



47

1 Power on the PC.

2 Open the network connection dialog.

WINDOWS 7:

a) Open the Control Panel.

b) Click Network and Internet | View network status and tasks.

Figure 3-37 Network and Internet Settings (Windows 7).

WINDOWS XP:

a) Click Start > Control Panel.

b) Click Network Connections.

You should see two active networks (one for each card.).

3 For each card, click the connection link (circled in red below). (WINDOWS XP: double-click the connection link.)

Note: The network card connected to the M-7600 will show No Internet Access, and probably show up as either an M-7600 (if preconfigured by CETAC) or otherwise as an unidentified network, as seen in Figure 3-38.

Figure 3-38 Network Connection Dialog for Windows 7.

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4 Click Properties.

Figure 3-39 Network Connection Properties Button.

5 Select ‘Internet Protocol Version 4’ and click ‘Properties’.

Figure 3-40 IPv4 Properties Button.



49

6 Click ‘Advanced’

Figure 3-41 IPv4 Advanced Button.

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7 Deselect ‘Automatic metric’ (see circled area in the image below), and specify a metric number. Specify ‘2’ for the card connected to the M-7600 and ‘100’ for the card connected to the local area network.

Figure 3-42 Interface Metric for the M-7600.

Setting the IP Address for the Secondary NIC

If the PC was purchased from CETAC, it will be preconfigured to use an IP address of 192.168.0.149 for the M-7600 mercury analyzer. In most cases, this address will work. If this address causes a conflict (for example, if the laboratory subnet is 192.168.0.*), or if you are configuring a secondary NIC in a PC not supplied by CETAC, set the address as follows:

1 Choose an IP address for the secondary NIC.

Choose an address that does not conflict with anything in use on the laboratory/company Local Area Network (LAN).

Use a standard Ethernet cable to connect the secondary NIC directly to the M-7600. If there is any doubt about IP number conflict consult your network administrator.



51

PC’s purchased from CETAC will come preconfigured in such a way that a conflict is unlikely, but reconfiguration may be required (the default IP address of the M-7600 analyzer is 192.168.0.149.) If for example the subnet used in the lab consists of 192.168.0.*, then the secondary NIC could be configured to 192.168.10.x allowing it to communicate with an analyzer configured to 192.168.10.y, without conflicting with another device on the LAN.

Ideally the secondary NIC can be configured to be on a subnet compatible with the M-7600 default (i.e.192.168.0.*) and used. If this configuration is not acceptable for laboratory operation, see the next section.

2 In the Internet Protocol version 4 properties dialog (pictured below) select ‘Use the following IP address’, and specify a number on a subnet different than that used in your laboratory. Unless your network administrator indicates otherwise, the subnet mask should be 255.255.255.0, and the gateway, and DNS server can be left blank because they will not be used.

Figure 3-43 Setting the IP Address

Changing the Subnet of the Mercury Analyzer

Ideally the secondary NIC can be configured to be on a subnet compatible with the M-7600 default (192.168.0.*). If this configuration is not acceptable for laboratory operation, then the IP address used by theM-7600 will need to be configured as described in the CETAC M-7600 Mercury Analyzer PC Setup Guide which is included with the mercury analyzer.

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Connecting a Laptop Computer to the M-7600

Since a secondary network interface card cannot be installed in most laptop computers, an alternate configuration must be used.

Option 1: Use a USB to TCP/IP Converter

The easiest solution is to use a USB-to-TCP/IP converter (also called a USB LAN adapter). This converter will behave just like a secondary network interface card.

Option 2: Use an Isolated Network

If you don't need to connect the laptop to another network (including the laboratory network or the Internet), you can set up the network to communicate only with the M-7600. Set up the M-7600 using the instructions for the secondary network card. Use an alternate means of communication, such as a flash drive or a USB connection, to transfer files and print results.

Option 3: Use an Unallocated IP Address on the Network

If your network uses static IP addresses, allocate a new address for the M-7600. If your network is managed by a network administrator or information technology professional, it is strongly recommended to ask that person to assign the address.

If your network uses dynamic IP addresses (DHCP), it is usually possible to assign a static address to the M-7600 while the other devices on the network continue to use DHCP. In this case, you must find a static address for the M-7600 which will not conflict with other devices on the network. On many network routers, the DHCP IP addresses are restricted to a certain range. Note that this address range can be changed, so it is important to go into the router's configuration interface to verify the range. Choose an IP address above the address used by the router but below the DHCP range.

For example, if the router is configured like this:

Local IP Address: 192.168.1.1 Subnet Mask: 255.255.255.0 DHCP Starting IP Address: 192.168.1.100

and if there are no other devices on the network with static IP addresses, then you can configure the M-7600 to use:

M-7600 IP Address: 192.168.1.2 M-7600 Net Mask: 255.255.255.0 M-7600 Gateway: 192.168.1.1



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

HANDLE WITH CARE Use care when handling the GLS. If the GLS breaks, there is a risk of cut from broken glass.

Use only your fingers to tighten the fittings.

1 Locate the gas-liquid separator (GLS).

Figure 3-44 Gas-Liquid Separator (GLS).

2 Locate the gas-liquid separator (GLS) and gently slide it into the holder with the drain and Hg vapor ports facing you. Raise it as far as it will go.

Figure 3-45 Placing the GLS.

WARNING

Gas Supply (In)

Drain (Out)

Hg Vapor (Out, not connected until just before use)

Liquid Mix (In)

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3 Rotate the GLS so that the ports face to the right and gently tighten the thumbscrew to temporarily hold it in position.

Figure 3-46 Tightening the GLS Thumbscrew.

4 Locate the drip block in the completion kit and lower the drip block into place. The drip block slides over the pegs below the GLS.

Figure 3-47 Positioning the GLS drip block.



55

5 Loosen the thumbscrew and lower the GLS into its final position, then gently tighten the thumbscrew. There should be space for the drain tube from the GLS to pass through the notch in the side of the drip tray.

Figure 3-48 Bottom of GLS.

6 Route the liquid mix tube to the top of the GLS through the guides on the front of the mercury analyzer.

Figure 3-49 Routing the Liquid Mix Tube to the GLS (view 1).

Figure 3-50 Routing the Liquid Mix Tube to the GLS (view 2).

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7 Connect the tube from the bottom of the GLS to the GLS SUPPLY fitting.

Figure 3-51 Ready to Connect the Gas Supply to the GLS.

Figure 3-52 Completed GLS Installation.



57

Step 10: Connect the Peristaltic Pump on the Mercury Analyzer

Figure 3-53 Peristaltic Pump on the Mercury Analyzer After Tubing is Connected.

Installing the Peristaltic Pump Tubing

1 Release all four peristaltic pump channel clamps.

2 Locate the peristaltic pump tubing in the completion kit. There are two sets of pump tubing.

The tubes with the yellow stops are for the sample and drain channels. The tubes with the black stops are for the reagent channel.

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3 Using both hands, stretch a tube with yellow stops across channel 1, closest to the body of the M-7600. Keep the tension even between the two sides and insert the stops into the slots.

4 Install two more tubes with yellow stops, one in channel 2 and the second in channel 3, then one tube with black stops in channel 4.

Note that the roller head moves clockwise.

Figure 3-54 Peristaltic Pump Tubing (Viewed from Front).

Inlet Side Outlet Side

Pressure Shoe

Adjustable Clamp

Roller Head

Stop



59

Figure 3-55 Peristaltic Pump Tubing (Viewed from Left and Right Sides).

Installing the Mixing Tee and Drain Tees

1 Locate the larger (3/32" dia.) polypropylene tee fittings provided in the completion kit. Install these tees on either side of the back two channels (channel 1 and channel 2) of the pump.

Figure 3-56 Large Tee Fittings (Tubing removed from Ch 3-4 for clarity).

2 In the completion kit, locate the 91 cm (three-foot) waste tube. Connect the tee on the right (outlet) side to the waste tube (1/8" o.d. Tygon® tubing).

Black

Yellow

Inlet Side Outlet Side

Channel 1 2 3 4

Large Tee Large Tee

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3 Connect the tee on the left (inlet) side to the drain tube coming from the GLS.

Figure 3-57 GLS Drain Tube.

Figure 3-58 Waste and Drain Connections.

4 Find a Luer male barbed fitting (look for this in the 10 liter waste container). Replace one of the Luer caps on the waste container lid with the barbed fitting. Attach the other end of the waste tube to this fitting.

To prevent pressure buildup in the 10-liter waste container, be sure that at least one of the two vents on the 10-liter waste container are open (uncapped) during operation.

From Drain

To Waste

Drain Tube



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5 Route the 1/16" Teflon® sample tube from the autosampler through the guide at the top of the mercury analyzer, then through the guide at the bottom.

Trim the sample tube if necessary. This may be necessary with an ASX-260 or ASX-130 autosampler. Be careful to leave enough slack in the tube so that the sample probe is able to freely move to the most distant position without stretching or kinking the tube. On the other hand, if the sample tube is too long it can tangle, and a longer tube will require more time to transport the sample and more time to thoroughly rinse between samples.

Figure 3-59 Attaching the Sample Tube to the Side of the M-7600.

6 Connect the sample tube to the inlet side of channel 3.

Figure 3-60 Sample Probe Connection.

7 Find the 23 inch (58 cm) length of 1/16" Teflon® tubing inside the reagent bottle. This is the reagent uptake tube.

From Sample Probe

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8 Connect the reagent uptake tube to the inlet side of channel number four.

When in use, to ensure that no precipitated solids are pumped through the system, the reagent tube should not touch the bottom of the reagent bottle.

Figure 3-61 Reagent Connection.

9 Locate the smallest (1/16" dia.) polypropylene tee provided in the completion kit. Install this tee on the output side of the pump. It connects the top two channels (channels 3 and 4).

Figure 3-62 Small Tee Fitting on Ch 3/4 Outputs.

Reagent Uptake Tube (From Reagent Bottle)

From Sample Probe

Liquid Mix Tube



63

10 Connect the Liquid Mix tube to the small tee which you just installed.

The Liquid Mix tube is a black tube which connects to the GLS, as shown in Figure 3-50 on page 55.

Figure 3-63 Liquid Mix Connection.

Step 11: Power On and Verify Communication Once installation of the QuickTrace™ M-7600 system is complete, it is important to verify that the system is installed correctly.

Attempting to use the QuickTrace™ M-7600 before ensuring that all components are installed correctly may result in damage to the system.

To Configure the Network Connection

The CETAC M-7600 mercury analyzer is controlled by a PC. CETAC recommends that this PC be equipped with two network cards. One card is used for communication with your laboratory network, and the other card is used exclusively for communication with the M-7600 mercury analyzer.

In most cases, a PC is supplied with the mercury analyzer, and this PC has two network cards.

CAUTION

Liquid Mix Tube

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NOTE

In most cases, CETAC will pre-configure the network cards for your laboratory. If you were not able to supply the necessary network information to CETAC, or if you will be supplying your own PC, then you will need to set up the network cards yourself as described in this document.

Refer to the M-7600 Mercury Analyzer PC Setup Guide and the QuickTrace™ Software Manual for instructions on how to configure the network settings on the PC and on the M-7600.

To Power On the System for the First Time (PC Configured by CETAC)

When you turn off the QuickTrace™ M-7600, wait at least 15 seconds before turning it back on. Rapidly cycling power can cause the optical monitoring feedback system electronics to temporarily malfunction, potentially resulting in an optical performance error.

1 Power on the PC, QuickTrace™ M-7600 mercury analyzer, and the autosampler.

2 Check to ensure that the communication cables are properly connected.

3 Start the QuickTrace™ software.

4 When the software is initializing, it will test the connections to the QuickTrace™ M-7600 mercury analyzer and the autosampler.

The QuickTrace™ M-7600 software runs a test routine at startup to test the various interfaces throughout the system. The software will give a report on the status of the interface if there is a failure.

To Power On the System for the First Time (Customer-Supplied PC)

If you are supplying your own PC, you will need to set up drivers to communicate with the M-7600 and the autosampler.

When you turn off the QuickTrace™ M-7600, wait at least 15 seconds before turning it back on. Rapidly cycling power can cause the optical monitoring feedback system electronics to temporarily malfunction, potentially resulting in an optical performance error.

1 Power on the PC, QuickTrace™ M-7600 mercury analyzer, and the autosampler.

2 Check to ensure that the communication cables are properly connected.

3 Run the USB device driver installation program. Navigate to

C:\Program Files\QuickTrace\USB Drivers

then double-click CDM2.02.04.

CAUTION

CAUTION



65

4 Select All Programs | CETAC QuickTrace | Specify Installed Hardware.

Figure 3-64 Starting the Specify Installed Hardware Program.

5 Select the M-7600 analyzer.

Figure 3-65 Selecting the Analyzer.

Once the M-7600 is chosen the software will search the network for analyzers.

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Figure 3-66 Searching for the Analyzers.

6 When the search is complete, select the analyzer. The IP address and other communication parameters will be filled in automatically.

Figure 3-67 Selecting the Analyzer.

7 Select the model of the autosampler you are using.



67

Figure 3-68 Selecting the Autosampler Model.

8 Select the autosampler COM port.

The autosampler is connected via USB, but the USB driver emulates a serial (COM) port. The driver automatically assigns a COM port number of COM3 or greater.

Figure 3-69 Selecting the Autosampler COM port.


10 When the software is initializing, it will test the connections to the QuickTrace™ M-7600 mercury analyzer and the autosampler.

The QuickTrace™ M-7600 software runs a test routine at startup to test the various interfaces throughout the system. The software will give a report on the status of the interface if there is a failure.

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To Test the Autosampler

1 In the QuickTrace™ software, click the Instrument Control button.

Figure 3-70 Instrument Control Button.

2 Click the Autosampler button.

Figure 3-71 Autosampler Button.

3 Click the buttons to turn the autosampler's peristaltic rinse pump on and off, move the probe (“sipper”) up and down, and move the probe to a sample vial and back.

Refer to the QuickTrace™ software online help for more information on how to control the autosampler.

Step 12: Fill the Rinse Solution Bottle

1 Fill the rinse bottle with trace metal grade 1% HCl / 2% HNO3 v/v.

NOTE:

When analyzing samples and standards of high concentration such as 20 ppb or greater use a stronger concentration of acid; such as 5% HCl / 2% HNO3 or a similar mix but do not exceed 10% HNO3.

2 Insert the rinse solution drain tube (from the autosampler rinse station drain port, via the peristaltic pump) about ¼ of the height of the rinse bottle.

3 Insert the rinse solution supply tube (to the autosampler rinse station intake port, via the peristaltic pump) so that it is just above the bottom of the rinse bottle.

The end of the drain tube must remain above the end of the supply tube.

For help identifying the rinse solution drain and supply tubes, see Figure 3-10 on page 30.



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Step 13: Fill the Reagent Bottle The reducing agent will be used with the QuickTrace™ M-7600 system during operation of the system.

The reducing agent is 10% SnCl2 w/v (in 7% HCl v/v). To mix the reducing agent, perform the following steps under a hood:

1 Add 100 g of SnCl2 to the reagent bottle.

2 Add 70 mL of trace metal HCl.

3 Swirl and wait ~ 2 min or until SnCl2 begins to dissolve.

4 Add ~ 100 mL of DI water, swirl and wait ~ 2 min.

5 Add ~ 100 mL of DI water, swirl and wait ~ 2 min.

6 Fill with DI water to the shoulder of the rinse bottle.

7 Cap until ready for use.

Preserving the SnCl2

Cap the Luer fitting when not in use.

Refrigerate unused portions.

NOTE

All solutions must be room temperature prior to use.

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Step 14: Adjust the Peristaltic Pump Tubing Clamp Tension (Optional) The tension of the tubing in the mercury analyzer's built-in peristaltic pump affects how smoothly liquid will flow through the system.

NOTE

The clamps are preset at the factory to optimal tension. Perform the following steps only if you believe the clamps may need adjustment.

1 Verify that the “11HG VAPOR12” tube is disconnected from the GLS vapor outlet.

Figure 3-72 Disconnecting the Hg Vapor Tube.

2 Open the QuickTrace software.

3 Open the QuickTrace hardware Controls (see the QuickTrace software manual) by clicking the Instrument button, or select Window|Instrument.


4 With zero clamp tension on the tubing (screws nearly unscrewed), snap all four clamps into place and start the peristaltic pump.

5 Set the gas pressure to 120 psi (825 kPa).



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6 Set the analyzer gas flow to 100 mL/min.

Figure 3-74 Gas Flow Controls (Shown Before Setting to 100 mL/min.).

Read through steps 7-11 before proceeding. It is extremely important to set the peristaltic pump drain clamps in a timely fashion after the GLS begins to fill with liquid. Failing to do so can cause an overflow and spillage.

CHEMICAL SPILL HAZARD Do not start liquid flow without the carrier gas being on and set to 100 mL/min with and pressure set to 120 psi. Otherwise, fluid backfill can occur.

Refer to the QuickTrace help or software manual for more information on instrument control.

7 Place the autosampler sample probe into rinse station. Click the Up button, then the Park button. Visually verify the probe's movement.

Figure 3-75 Autosampler Button.

8 Place a Kimwipes wiper at the GLS gas exit port to prevent any liquid from spilling onto the GLS mount.

9 Manually increase the clamp tension on the Santoprene® sample tubing (Channel three) until liquid uptake begins to flow with a jerky motion in the sample tube from the autosampler. Now rotate the tension screw ¼ turn past this point and verify that the flow is steady.

CAUTION

WARNING

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10 Watch the liquid flow as it makes its way from the autosampler rinse station, to the pump, through the mixing tee, and to the Gas-Liquid Separator.

The GLS will begin to fill with rinse solution.

11 Increase the clamp tension on both of the drain tubing clamps (Channels one & two) until flow begins from the drain port of the GLS and the liquid level begins to drop.

Do this quickly before the GLS fills to the point where fluid overflows the GLS. The GLS should slowly drain to empty, even though sample continues to be delivered to the top of the frosted center post. The GLS is intended to operate “empty” with only a thin film of liquid continuously wetting the frosted center post and exiting the drain.

NOTE

If GLS overflow occurs, the pump will stop. To restart the pump, simply click the Pump On button.

12 Tighten both drain tube clamps equally to ensure even flow to each.

Check this by observing the segmented flow at both drain tees. The rate of flow in and out should be balanced through both Santoprene drain tubes. Adjust the clamp tension to keep the GLS empty and to achieve a smooth, balanced, segmented flow. Unstable drain flow can cause baseline noise in the system. The drain tube tension should exactly match the sample flow tension.

13 Start the SnCl2 flow.

Place the SnCl2 uptake tube in the reagent bottle

Close the Channel 4 clamp.

Increase the reagent clamp tension until reagent uptake begins in the tube.

Adjust the clamp so that the flow from the SnCl2 bottle is smooth, with no jerks in the flow.

14 Once liquid is running through the QuickTrace M-7600, note that the drain tubing clamp tension is properly adjusted by watching the flow through the Gas-Liquid Separator.

The GLS should remain empty and liquid exiting the GLS should appear nearly motionless, with no flutter or instability.



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15 The flow into the GLS should be as smooth and pulse free as possible.

View this closely at the top of the GLS frosted center post. The liquid should stream continuously from the capillary tip to the top of the post, and the liquid column spanning the gap between the capillary tip and post should be nearly “motionless,” with minimal fluctuation and no jerkiness or discontinuity. If this is not the case check that the “gap” between the bottom of the GLS capillary insert tube and the top of the GLS frosted center post is ~0.5 mm (range of 0.3-0.6 mm). If not, very carefully slide this insert up or down, as needed. Refine the clamp tension of the sample and reagent channels as needed to stabilize the liquid flow to the GLS.

A flow check with a 10 mL graduated cylinder (less than 100 mm tall) and stopwatch should yield a sample uptake rate of ~15 mL/min, and a reagent uptake rate of ~5.7 mL/min. Check liquid flow stability at the drain exit of the GLS after final adjustments of clamp tension to sample and reagent pump tubing. The pump tension will not need further adjustments; do not adjust pump tension to compensate for worn pump tubing.

NOTE:

When properly adjusted the tension on the bottom three peristaltic pump tubes (channels 1-3) should be the same and the tension screw for the top pump tube (reagent tube, channel 1) should be screwed in 1 to 2 mm farther than the other channels.

Step 15: Check the Reagent Flow

1 Fill the 10 mL graduated cylinder with 10 mL DI water.

2 Simultaneously place the reagent uptake tube in the graduated cylinder and start the stopwatch.

3 After 30 seconds, remove the uptake tube from the cylinder.

4 Measure the water remaining in the cylinder, and calculate the reagent flow rate.

Step 16: Check the Sample Probe Flow

1 Fill the 10 mL graduated cylinder with 10 mL DI water.

2 Move the sample probe to the middle of the sample rack. (1:35 if set for a 60 position rack).

3 Position the graduated cylinder beneath the sample probe.

4 Simultaneously click the Down button and start the stopwatch.

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5 After 30 seconds press the Up button.

6 Measure the water remaining in the cylinder, and calculate the flow rate.

7 Park the sample probe.

NOTE:

When properly adjusted the tension on the bottom three peristaltic pump tubes (channels 1-3) should be the same and the tension screw for the top pump tube (reagent tube, channel 1) should be screwed in 1 to 2 mm farther than the other channels.

Once the clamp tension on the pump tubing is established, relieve their stretch:

8 Unclamp reagent and sample clamps.

9 Park the sample probe.

10 Press the Up button to remove the sample probe from the rinse station.

11 Remove the reagent uptake tube from the SnCl2.

12 Allow the waste tube to empty.

13 Unclamp waste tube clamps.

14 Turn the pump off using the software controls.

Do not leave tubes clamped in place when the system is not being used. The next time the system is used, hook the tubes and close the quick-release mechanisms. No screw adjustments will be needed. Previous clamp tension is “remembered” as the quick release is engaged and disengaged.

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4 Using the Analyzer

Operation of the M-7600 is mostly through the QuickTrace™ software interface.

For a detailed description of the software see the QuickTrace™ help file and the QuickTrace™ mercury analyzer software manual.

Theory of Operation

Autosampler

The autosampler is prepared for operation by loading sample vials of digested samples, into selected positions of the sample racks. Vials of calibration standards are placed in user-selected positions of the standards rack. Rinse solution, for sample-to-sample probe decontamination, fills the rinse station and re-circulates to the rinse bottle.

After a method worksheet is prepared/loaded, the system is ready for unattended operation to begin. The autosampler operates under computer control to move the sample uptake probe to any sample position; the rinse station, reference standard, blank, etc., in a user-programmed sequence. The sample probe supplies the multi-channel peristaltic pump's sample inlet.

For further information, see the Autosampler Operator's Manual.

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QuickTrace™ M-7600 Automated Mercury Analyzer

Figure 4-1 QuickTrace™ M-7600 Block Diagram.

Sample Introduction & Stannous Chloride Reactor

Refer to Figure 4-1 to trace the path of liquids through the M-7600 System. An acidified digested aqueous sample from the autosampler is introduced, via peristaltic pump as Hg2+ dissolved in solution. A reducing agent (10% stannous chloride in 7% HCl), is introduced via a parallel pump channel. The sample and reagent (SnCl2) streams join at the mixing tee (1), and immediately enter the QuickTrace™ M-7600 tubing reactor (“Liquid Mix”). Sn2+ reduces Hg2+ in solution to Hg0 while the mixture is en route to the Gas-Liquid separator (GLS). At this stage and prior to the GLS, the analyte is present as a finely dispersed emulsion of liquid (metallic) Hg0 micro-droplets, in excess SnCl2 solution.



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NOTE

The CETAC QuickTrace™ M-7600 mercury analyzer measures inorganic mercury (free Hg2+ or HgCl2, which is subject to efficient stannous chloride reduction in the QuickTrace™ M-7600 tubing reactor); using inorganic mercury standard solutions for instrument calibration. If insoluble mercury, bound mercury, or organomercurials are present in samples, an appropriate sample dissolution/digestion procedure will have to be employed to convert these other forms to free inorganic Hg2+ or HgCl2, prior to analysis with the QuickTrace™ M-7600.

Gas-Liquid Separation

The finely dispersed Hg0/SnCl2 emulsion is introduced into the top of the GLS (Gas-Liquid Separator (2)). The Hg0/SnCl2 emulsion flows over the frosted GLS center post in a relatively thin film, covering the entire post from top to bottom. A carrier gas simultaneously enters the bottom of the GLS tangentially (10). The carrier gas (Ar or N2) swirls around the wetted center post and upwards toward the GLS gas exhaust port (11).

Hg0 droplets in the thin emulsion film quickly evaporate into the gas vortex surrounding the post. The carrier gas stream efficiently sweeps this Hg0 vapor (along with some evaporated water) upward and out of the GLS gas exhaust (11), and on to the drying (12, 13) and optical section (14, 15) of the QuickTrace™ M-7600 for an absorbency measurement.

The liquid water, containing excess reducing agent, acid, any non-participating “spectator ions,” and reaction by-products, finally drains out the bottom of the GLS (3) and is pumped to waste (4), (channels one & two).

NOTE

The GLS operates “empty” with no liquid level. The liquid spreads out as a film that wets the center post. At the bottom of the post, the film collects at a single point and is then continuously pumped to waste, so the “liquid level” should not rise in the GLS.

Carrier Gas

Refer again to Figure 4-1 on page 76 to trace the path of the carrier gas. A clean, dry carrier gas, such as UHP N2 or Argon, must be supplied to the back of the instrument. The gas passes through fixed restrictors to produce primary flow rates in the range of 30-1000 mL/min at 825 kPa (120 psig). The carrier gas first enters the reference cell (6) to facilitate measurement of the incident radiant power (P0) at 253.7nm. It exits (7) and passes through the GLS (10) to pick up Hg0 vapor from the reduced sample. The carrier gas and Hg0 vapor exit the GLS (11) and enter (12) a Perma Pure® drying cartridge where water vapor is removed by a Nafion® membrane (13). For the Perma Pure® dryer, an auxiliary sweep gas from a restrictor (5A) enters an auxiliary port (17) and selectively removes water vapor from the dryer cartridge at 18.

Finally, the dry Hg0/carrier gas mixture exits the dryer (13) and enters the sample cell (14B) for measurement of transmitted radiant power (P) at 253.7 nm.

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Ultimately, the gas stream (carrier gas and Hg0) exits the sample cell (15) and is exhausted to a solid KMnO4 trap (16) where Hg0 is absorbed, and clean carrier gas passes to the lab atmosphere.

Dryer Cartridge

The mercury analyzer uses a Perma Pure® DuPont Nafion®-based dryer cartridge. Dryer cartridges typically last three to six months.

The dryer cartridge contains Perma Pure® dryer tubing which is made with a tubular DuPont Nafion® membrane. The Nafion® tubing is housed within an outer tube and coiled inside the cartridge. The argon or nitrogen carrier gas containing mercury and water vapor is swept along the inner Nafion® membrane, allowing water vapor to permeate the membrane selectively, whereas the membrane is not permeable to mercury vapor. On the “waste” side of the membrane, a counter gas flow, split from the carrier gas supply, selectively sweeps the water vapor out of the system, whereas non-permeating mercury vapor proceeds to the sample cell.

The Perma Pure® dryer cartridge and associated plumbing is already pre-installed in your new QuickTrace™ M-7600 factory shipment. No further installation is required.

Optics and Cold Vapor AAS

Refer again to Figure 4-1 on page 76 to trace the optical path of the QuickTrace™ M-7600. The Cold Vapor AAS (Atomic Absorption Spectrometry) process within the sample cell begins with a low pressure, high frequency, thermally stabilized, electro-optically regulated Hg vapor lamp, which produces the Hg emission spectrum. Emitted light is collimated (L1) and projected in two parallel, isolated beams one each through the reference and sample cells. Absorbance of 253.7nm radiation by Hg0 vapor (derived from the chemically reduced sample and GLS) occurs only in the sample cell. P is thereby decreased, relative to P0.

Light from the cells enter the binocular camera, where both collimated beams are independently focused (L2) and filtered (F) before reaching the Charged Coupled Device (CCD) detector. Narrow band 254 +/- 2nm interference filters (F) remove all radiation but the strong 253.7 nm Hg0 “resonance line” from both the sample (P) and reference (P0) beams. By a photovoltaic effect, the CCD converts the light beams into electrical signals, proportional to radiant power (P and P0). These outputs are processed to yield an electrical signal proportional to optical absorbance (Abs = -log (P/P0)).

Software In the host computer, the sample absorbance value is drift corrected, blank subtracted, if through blank is desired. The absorbance value is then measured against a calibration curve derived from previously obtained absorbance values of calibration standards.

The QuickTrace™ software operates under a Windows environment. The QuickTrace™ software provides complete instrument, autosampler control. The QuickTrace™ software also provides a variety of EPA compliant quality control functions, display features, report generation and diagnostic routines.



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The user interface is sufficiently powerful that it will satisfy the requirements of experienced technically advanced analysts and scientists.

The reader is referred to the separate QuickTrace™ Help file and QuickTrace™ Mercury Analyzer Software Manual for a detailed description of the software features, functions, and operation instructions.

Preparing Reagents and Calibration Standards Always use high purity gas, chemicals, acids, water, standards, and clean glassware for analysis. It may be necessary to acid wash and rinse all glassware more than once to eliminate contamination for the most sensitive mode of operation (<20 ppt).

Recommended Chemical Concentrations:

Reagent 10%(w/v) SnCl2 in 7%(v/v) HCl. See “Step 13: Fill the Reagent Bottle” on page 69.

Standards for Instrument Calibration

All intermediate standards used to prepare the calibration standards (Hg2+) are prepared in 7%(v/v) HCl then aliquots of those standards are added to an acidified matrix and treated to the same procedure as a sample prior to instrument calibration.

NOTE: It is recommended that the calibration standards are prepared from the same intermediate standard.

Rinse Solution 1% v/v HCl / 2% v/v HNO3 trace metal grade in the autosampler rinse reservoir bottle.

NOTE

HCl media must be used for stock standard preparation! Hg standards in nitric acid (only) are unstable at ppb levels and below. With 7% HCl media (in glass at room temperature), the standards are stabilized for weeks at the ppb level, and for several days at the ppt level.

NOTE

Acidified rinse prevents carryover contamination from high samples and standards to subsequent low samples. Rinsing with deionized water alone is not sufficient to prevent carryover.

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NOTE

The CETAC QuickTrace™ M-7600 mercury analyzer measures inorganic mercury (free Hg2+ or HgCl2, which is subject to efficient stannous chloride reduction in the QuickTrace™ M-7600 tubing reactor). Inorganic mercury standard solutions are used for instrument calibration. If insoluble mercury, bound mercury, or organomercurials are present in samples, an appropriate sample dissolution/digestion procedure will have to be employed to convert these forms to free inorganic Hg2+ or HgCl2, prior to analysis with the QuickTrace™ M-7600. If it is desired to confirm the oxidative digestion procedure accuracy (recovery) regarding organomercurials, then organomercurial standards or appropriate standard reference materials would have to be carried through the digestion as “process standards”.

ORGANOMERCURIAL EXPOSURE HAZARD The handling of organomercurial concentrates, which may be used in the preparation of process standards, presents a substantial (potentially lethal) safety hazard. Only an experienced, professionally trained organo-metallic chemist, knowledgeable and skilled specifically in the safe handling of organomercurials (using approved apparatus and approved protection measures in an approved facility) should attempt to prepare diluted organomercurial process standards from concentrates. Always be sure to obtain and carefully read the MSDS (Material Safety Data Sheets) before handling organomercurials! Always wear appropriate personal protective equipment when operating the mercury analyzer or handling organomercurials. At a minimum, you should wear eye protection, acid-resistant gloves, and a lab coat.

NOTE:

CETAC Technologies assumes no liability for the handling of organomercurial concentrates or the preparation, handling, or use of diluted organomercurial process standards.

In most cases, CETAC Technologies recommends that samples be oxidized following standard, safe, well known, approved sample dissolution or digestion procedures, and that the QuickTrace™ M-7600 instrument calibration standards be prepared only from inorganic mercury concentrates or diluted from commercially available inorganic mercury standard solution concentrates. Where possible, the recommended means of overall process (dissolution/digestion + QuickTrace™ M-7600 analysis) validation should be through use of commercially available standard reference materials (SRM’s) of composition matching (or similar to) the samples and containing certified, known mercury levels in a concentration range similar to the samples. (Being by far the safest alternative, this SRM approach to overall process validation should be used whenever possible, and is nearly always preferred to preparing diluted process standards from hazardous organomercurial concentrates!)

WARNING



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Gas Parameters The QuickTrace™ M-7600 has controls gas flow based on settings in the QuickTrace™ software. The user needs to adjust the method flow rate to achieve increased or decreased signal responses which are in part derived from gas flow rate.

Carrier Gas N2 UHP, high purity grade cylinder (dry, research grade) or Argon, high purity grade (supplied, for example, from a liquid Dewar boil-off or cylinder).

Gas Pressure 120 psig (825 kPa)

Gas Flow Rate 30-1000 mL/min

For exact response versus gas flow parameters for your instrument, please consult the final test documentation, which accompanied the instrument.

See Table 4-1 and Table 4-2 for a more complete listing of optimal instrument setups.

Starting the System

1 Power on the QuickTrace™ M-7600.

2 Power on the autosampler.

3 Open the QuickTrace™ software.

The mercury vapor lamp automatically turns on when the QuickTrace™ software starts.

4 Once the QuickTrace™ M-7600 has powered up, and while the lamp is warming up, perform the following checks:

If this is the first time the instrument is started, check that the pump tubing is installed and tension is adjusted as described beginning on page 70.

Check that supply gas is connected and 120 psig (825 kPa) pressure is applied to the unit.

If this is the first time the instrument is started, check that the KMnO4 trap is filled as described on page 42.

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NOTE:

The mercury vapor trap will exhibit a noticeable brown color migrating toward the vapor exit port as the KMnO4 is consumed. It may take a considerable amount of time to consume the entire amount of KMnO4. The reaction is the oxidation of Hg0 to mercuric oxide with the KMnO4 being reduced to manganese dioxide.

Mercury Vapor Lamp Warmup

The mercury vapor lamp automatically turns on when the QuickTrace™ software starts.

The lamp will require 30-60 minutes to stabilize, as described in the following sections. Other instrument preparation may be performed during this time.

Turning Off the Mercury Vapor Lamp for System Warm-Up

If your intent is to only warm up the system and you are not going to analyze samples within the next hour it is recommended to navigate to instrument controls and turn off the mercury lamp.

1 In the QuickTrace™ software, click the Instrument Control button.


2 Click the Hg Analyzer button then click Lamp Off.

Figure 4-3 Turning Off the Lamp.

System Warm-Up for Trace or Ultra-Trace Analysis

For analysis in the trace to ultra-trace range (ppt), it is recommended to allow extra stabilization time as follows:

1 Turn on the instrument and open the QuickTrace™ software.

2 Navigate to instrument controls and turn off the mercury lamp.



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3 Allow 2 hours for the instrument to stabilize.

5 Turn on the lamp.

4 Disengage the pressure shoe of the mercury analyzer's peristaltic pump.

Disengaging the pressure shoe reduces wear on the peristaltic pump tubing while the pump stabilizes. Do not adjust the clamp tension.

5 Run the peristaltic pump at the desired method rate.

6 Allow 1 hour for the lamp and pump to stabilize.

7 Proceed with liquid introduction to the system.

System Warm-Up for ppb or Non-Ultra-Trace Analysis

If the desired range is ppb or non-ultra-trace analysis the warm-up time from a warm start is just the lamp stabilization time. For a cold start in a non-trace range the system would need 30-60 minutes with the lamp and pump on at the desired rate to stabilize all parts of the system. For a warm start, allow 15-30 minutes to stabilize the lamp.

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Wetting the GLS At the beginning of each day or after any period of pump inactivity and prior to analysis ensure that the GLS center post is fully wetted.

Refer to Figure 4-8 while reading the procedure below.

1 Disconnect “11HG Vapor12” tube from the GLS vapor outlet.

NOTE

Always disconnect the Hg Vapor tube from the GLS when the system is not in use.


2 Set the gas to maximum flow. There are two ways to do this:

Click the Instrument Control button and set the flow rate to 1000 mL/min, or

Figure 4-5 Gas Flow Setting.



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Click the “Wet The Gas Liquid Separator Post” button. This will result in a gas flow of about 1000 mL/min with a pump rate of 100%.

Figure 4-6 Wet GLS Button.

3 Check that the bottle supplying the autosampler rinse station is filled with clean trace metal grade acidified rinse solution.

4 Place the reagent uptake tube in a beaker of DI water.

5 If the peristaltic pump is not already on, turn it on.

Figure 4-7 Turning On the Pump.

6 Engage the pressure shoe (quick release mechanism) on the peristaltic pump.

7 Pinch the drain tube as shown in Figure 4-8. The drain tube runs from the GLS to the inlet side of the peristaltic pump.

Figure 4-8 Pinching the Drain Tube.

Pinch the Drain tube here

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8 With the drain tube pinched, the GLS should begin to fill with liquid. Once the liquid level rises, gas will bubble through it.

9 Allow the GLS to fill until a gas bubble propels a “meniscus” upward to wet the post all along its length, including its top. (THE POST IS NOW WETTED.)

10 When this happens, release (un-pinch) the drain tube. With the drain tube tension properly set and the drain tube un-pinched, the liquid will begin draining.

11 Once the GLS has “emptied,” leave the pump running (keep liquid flowing) and reconnect “11HG Vapor12” tube to the GLS vapor outlet.

12 Place reagent uptake tube in the SnCl2.

13 The post is now wetted and the QuickTrace™ M-7600 is ready to run samples.

The analyst may now operate the QuickTrace™ M-7600 to perform analysis of samples. The help system built into the QuickTrace™ software has been developed specifically to assist the analyst in this task. Refer to the software manual, the online help, or the QuickTrace™ interactive demo to perform the desired analytical tasks.

14 Once the analysis is finished, place the QuickTrace™ M-7600 instrument in either Standby or Cold Shutdown condition (page 101).

NOTE

Concentration ranges greater than 20 ppb may require a higher percent acid in the rinse solution. A 5% HCl / 2% HNO3 v/v should be sufficient for the highest concentration mode.

NOTE

If you don't want to consume stannous chloride reagent during a “standby” condition, you may alternatively keep the GLS center post wetted by immersing the reagent uptake tube in a beaker of deionized water (with the autosampler's sample probe also immersed in the autosampler rinse station).



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Running the Interactive Demo The QuickTrace™ software comes with an interactive demonstration which will help you quickly understand the basic operation of the software.

1 From the Start menu, select All Programs | CETAC QuickTrace | Interactive Demo.

Figure 4-9 Starting the Interactive Demo.

Figure 4-10 Interactive Demo Interface.

Overview of the CETAC QuickTrace™ Software The QuickTrace™ software lets you create a method tailored to your analytical needs. You can specify a calibration, quality control limits with error actions and specific end-of-run routines such as automated standby, print or export routines.

There are three basic parameters that affect the M-7600’s method ranges:

Gas flow rate

Sample peristaltic pump rate

Sample uptake rate

By changing these basic parameters, you can set the QuickTrace™ M-7600 mercury analyzer to function in method ranges of ultra-trace to high µg/L

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methods such as a high calibration standard of ~ 500 µg/L. These method ranges are guaranteed to exhibit at a minimum three orders of magnitude.

The M-7600 QuickTrace™ software comes with two basic templates or starter methods as described in “QuickTrace™ M-7600 Startup Summary” on page 89. Follow these basic steps to create a new method based on one of the supplied templates:

1 Open one of the supplied templates.

The M-7600 QuickTrace™ software comes with two basic templates or starter methods as described in “Summary of Gas and Liquid Flows for Analytical Ranges of the QuickTrace™ M-7600” on page 98.

Click the File icon or the File menu and select New From… You will be asked to supply a name for the new method.

Figure 4-11 Creating a New Method Using the File Icon.

Figure 4-12 Creating a New Method Using the File Menu.

2 Adjust the template to create a laboratory-specific method

3 Perform the peak profile described in “Setting Baseline Correction” on page 91.

4 After a successful peak profile, start the analytical sequence by selecting the green GO button, navigating to Analyze | Start Run, or typing Shift+Ctrl+F8.

Learning More

It is strongly recommended to navigate through the interactive demo, then view the help file or read the QuickTrace™ software manual to find out about more software features. In most cases, there are multiple ways to accomplish a given task.



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QuickTrace™ M-7600 Startup Summary


If the software was left open and in standby, open the instrument controls and start the autosampler rinse pump by clicking Pump On or Move Sipper to Park (either method will start the autosampler rinse pump).

Figure 4-13 Turning On the Pump.

2 Turn on the lamp and initiate the carrier gas flow. A minimum of a 15-minute warm-up time is required.

NOTE

The lamp will automatically turn on when you start the QuickTrace™ software.

Figure 4-14 Turning On the Lamp and Carrier Gas.

3 Clean and rinse the 2 L rinse bottle with DI water and refill with the desired trace metal grade HCl / HNO3 solution.

4 Place the autosampler rinse tubing into the rinse bottle.

5 Prepare a fresh 10% SnCl2.H2O w/v 7% HCl v/v solution if old solution is yellow (oxidized) or precipitated. Prepare only what you need to complete the calibration and sample run including all QC checks and spikes. The reagent flow is ≈ 3.8 mL/min at 50% pump rate.

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6 Verify that the sample capillary (inlet insert) is 0.5mm above the Gas-Liquid Separator (GLS) center post.

7 Open the vents on the waste container.

8 Inspect the peristaltic pump tubing for wear and flat spots (replace if necessary). If you remove any of the peristaltic pump tubes, do so one channel at a time, and be careful to return the tube to the appropriate pump channel. Do not lock the pressure shoes at this time.

9 Place the reagent capillary in a beaker of DI water.

10 Lock down the peristaltic pump pressure shoes.

11 Inspect liquid flows. The GLS drain should be flowing smoothly with no build up or pulsing of liquid. The waste tube from the peristaltic pump to the waste container should be liquid/gas etc… with no vibration. If this is not the case upon inspection, stop immediately and change GLS drain tube and or waste tube.

12 Wet the GLS center post as described on page 84.

13 Inspect the rinse station for a convex liquid bubble adhering to the sample probe. If this is not the case, change the rinse pump peristaltic tubing.

14 Open the appropriate worksheet (see the online help in the QuickTrace™ software) and set the gas pressure to match the method.

You can also set the gas pressure by clicking on the Set Gas & Pump Speed icon.

Figure 4-15 Setting the Gas Pressure.

15 Zero the QuickTrace™ M-7600 using the auto zero.

Figure 4-16 Auto-Zero.



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16 Peak profile the high standard and verify the baseline and sample integration times. Record µAbs and concentration of the peak profile standard in a daily instrument logbook. This operation should be performed on the highest standard.

Figure 4-17 Profiling the Highest Standard.

17 Calibrate instrument and analyze samples.

Setting Baseline Correction To guarantee a high quality result it is essential to always use the correct baseline correction.

For trace to ultra-trace levels (ng/L), use a two-point base line correction.

For µg/L levels, use a single point base line correction.

Keeping an Instrument Log Book

At a minimum, it is recommended that you record the following information in an instrument log book every day:

Date

Lamp current

Method

Response of highest calibration standard

This will assist in troubleshooting any change in peak response.

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Viewing the Graphs

To scroll an absorbance/time graph, place the mouse pointer over the graph and hold the right mouse button.

To zoom in on a graph, hold the left mouse button to draw a box from the upper-left to the lower-right corner of the region you wish to view.

Setting a One-Point Baseline

1 Examine the absorbance curve.

The absorbance curve is displayed in the Method Editor after the peak profile has been performed.

NOTE

If you leave the method editor, the peak graph will not be retained. Make all your inspections and adjustments then save prior to exiting method editor. To save the adjustments, select File | Save, which will save the entire worksheet.

2 Check “Baseline drift correction” to enable setting Baseline Point #1.

Figure 4-18 Typical Results from µg/L Settings.

3 To set Baseline Point #1, place the end of the read about 4 seconds before the inflection point on the left side of the peak.



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Figure 4-19 Setting Baseline Correction Point #1 (µg/L).

4 Zoom in on the graph to see the top of the peak, and record the peak height in the instrument log book.

Figure 4-20 10.0 µg/L Peak Profile Response With Baseline Correction.

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Setting a Two-Point Baseline

1 Examine the absorbance curve.

The absorbance curve is displayed in the Method Editor after the peak profile has been performed.

NOTE

If you leave the method editor, the peak graph will not be retained. Make all your inspections and adjustments then save prior to exiting method editor. To save the adjustments, select File | Save, which will save the entire worksheet.

2 Check “Baseline drift correction” to enable setting Baseline Point #1.

3 Check “Two-point baseline correction” to enable setting Baseline Point #2.

Figure 4-21 Typical Results from ng/L Settings.



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4 To set Baseline Point #1, place the end of the read about 4 seconds before the inflection point on the left side of the peak.

Figure 4-22 Setting Baseline Correction Point #1 (ng/L).

5 Set Baseline Point #2 just after the signal returns to its baseline level on the right side of the peak.

Figure 4-23 Setting Baseline Correction Point #2 (ng/L).

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Figure 4-24 View of ng/L Baseline Correction Points.

The software will average the baseline points and subtract that value from the peak height. The response will remain the same for each standard or duplicate sample and the drift correction will compensate for baseline drift, effectively zeroing out any instrument drift.

For example, if the 100 ng/L response is 5000 units at time 0 and the baseline is at 0 the software will report 5000 units. If the baseline should drift over time, such as a baseline drift of 1000 units, and you analyze the 100 ng/L the response will be 6000 units. With baseline correction, the software will subtract the 1000-units drift from 6000 units and report a value of 5000 units or 100 ng/L. The same is true for a negative baseline drift.



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Figure 4-25 100 ng/L Peak Profile Response With Baseline Correction.

6 Zoom in on the graph to see the top of the peak, and record the peak height in the instrument log book.

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Summary of Gas and Liquid Flows for Analytical Ranges of the QuickTrace™ M-7600

RANGE #1: M-7600 ng/L <5.0 – 100 ng/L Hg

Gas Flow 40 mL/min

Peristaltic Pump Speed 100%

Sample Flow Rate ~ 15 mL/min

ASX Rinse Pump Speed 100%

Sample Time (for Liquid Uptake or autosampler “Sip”) 65 s

Rinse Time 100 s

Read Delay 68 s

Replicate Read Time 2.5 s

Replicates 4

Baseline Correction Method 2 point (15-15 s & 150-160 s)

Expected Results: 100 ng/L | 7% HCl ~5000 µAbs

Detection Limit (nominal): < 0.5 ng/L

Sample Throughput Rate (minutes/sample) 2.75 min/sample

Table 4-1 ng/L Parameters to Optimize.

Figure 4-26 Typical Results from ng/L Settings.



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RANGE #2: M-7600 µg/L 0.1 – 20 µg/L Hg

Gas Flow 100 mL/min

Peristaltic Pump Speed 50%

Sample Flow Rate ~5 mL/min

ASX Rinse Pump Speed 50%

Sample Time (for Liquid Uptake or autosampler “Sip”) 40 s

Rinse Time 95 s

Read Delay 52 s

Replicate Read Time 1.5 s

Replicates 4

Baseline Correction Method 1 point (20-25 s)

Expected Results: 10 ppb | 7% HCl ~150,000 µAbs

Detection Limit (nominal): < 0.01 ppb

Sample Throughput Rate (minutes/sample) ~ 2.25 min/sample

Table 4-2 µg/L Parameters to Optimize

Figure 4-27 Typical Results from µg/L Settings.

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Placing the QuickTrace™ M-7600 in Standby Mode To prolong instrument life, do not leave the system fully on (with lamp on) overnight, or when not in use. However, to speed the next day’s startup, the QuickTrace™ M-7600 can be left on with the lamp off overnight without significantly shortening its life.

1 Turn the lamp off.

Figure 4-28 Turning Off the Lamp.

NOTE

The lamp will automatically turn off when you exit the QuickTrace™ software.

2 When analysis is done for the day, rinse with 10% HNO3 for several minutes through the reagent uptake tube.

3 Rinse with deionized water through the reagent uptake tube for several minutes.

NOTE

Failure to perform this “shutdown rinse” may result in a system clog.

4 Withdraw the reagent uptake tube.

Secure the reagent uptake tube in a container that will keep it clean. A plastic re-sealable zipper storage bag, a plastic bottle, or a graduated cylinder with a plastic bag sealed over the top all work sufficiently.

5 Remove the autosampler rinse supply tube from the bottle of rinse solution and allow the rinse station to run completely dry.

Use the QuickTrace™ software controls to withdraw the autosampler probe from the rinse station when the rinse station becomes empty. Allow the drain and waste tubes to run completely dry.

Make sure the rinse return tube stays inside the bottle of rinse solution. Rinse solution may drain from the tubing while you are removing and wiping off the rinse supply tube.

CAUTION



101

6 Turn off both the M-7600 peristaltic pump the autosampler peristaltic rinse pump.

7 Release the M-7600 peristaltic pump pressure shoes, and then lift the stops on the tubes out of the slots.

8 Turn off the gas (main supply).

9 Disconnect the Hg vapor tube from the GLS.

Leave the system mains power on. The Hg lamp sent with the system has an operation life of ~5000 hours, but internal optical filter life may be substantially extended by turning off just the lamp whenever analyses are not being performed. Leaving the main power on leaves the lamp block heaters on, and consequently the lamp block remains thermally stable.

To return the instrument to “run” status, simply turn the lamp on again, re-establish appropriate gas and liquid flows and operate the instrument normally. The system will be stable and ready to run within 5-10 minutes.

If desired, exit the QuickTrace™ software, but leave the mains power on. This will also effectively keep the system in a warm start state.

Cold Shutdown For a total system shutdown (to cold condition), prepare the pump tubing as you would for standby mode. Exit the QuickTrace™ software, shut down Windows and turn off the computer. Turn off the gas, autosampler, pump, and QuickTrace™ M-7600 main power.

Summary of QuickTrace™ M-7600 Shut Down

1 Place the reagent capillary in a beaker of 10% HNO3 and cap the reagent bottle. Rinse the system for a minimum of ten minutes.

2 Place the reagent capillary in a beaker of DI water and rinse the system for one minute.

3 Remove reagent capillary from DI water.

4 Remove the autosampler rinse supply tube from the bottle of rinse solution and allow the rinse station to run completely dry.

Use the QuickTrace™ software controls to withdraw the autosampler probe from the rinse station. Allow the drain and waste tubes to run completely dry.

Make sure the rinse return tube stays inside the bottle of rinse solution. Rinse solution may drain from the tubing while you are removing and wiping off the rinse supply tube.

5 Turn off both the M-7600 peristaltic pump the autosampler peristaltic rinse pump.

CAUTION

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6 Release the M-7600 peristaltic pump pressure shoes, then lift the stops on the tubes out of the slots.

7 Close the vents on the waste container.

8 Disconnect the GLS exhaust tube from GLS.

9 Turn off gas and lamp.

10 If you are going to use the instrument the next day or in the near future, leave the instrument in this condition. It will then be ready for a warm start.

11 If you are not going to be using the instrument in the near future then exit the QuickTrace™ software and turn off the autosampler and QuickTrace™ M-7600.

NOTE

Before shutting down the instrument to either Standby or Cold condition, remember to run 10% HNO3 and deionized water through the SnCl2 reagent tubes. This will clean out any chemicals from the peristaltic pump and sample tubing and prevent residue encrustation in the Gas-Liquid Separator and its drain. Remember to pump all tubes completely dry after rinsing.

Always remember to release all clamps and unhook the pump tubing from the peristaltic pump. Failure to release clamps and unhook the tubing when the pump is off, will cause tube fatigue and lead to poor results (bad RSD) when used for analysis the next time.

CAUTION

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5 Maintaining the Mercury Analyzer

Routine maintenance of the analyzer consists of daily and weekly cleaning of specific analyzer components. Routine maintenance also includes checking for leaks or other damage. Additional periodic maintenance tasks may be required, including replacement of the following analyzer components: peristaltic pump tubing, sample probe, rinse station tubing, GLS capillaries, GLS drain tubing and Perma Pure® dryer cartridge.

Discharge static buildup and ground to the analyzer base or cabinet before performing any maintenance. Avoid touching the contacts on the communication ports.

Maintenance Schedule

Daily Maintenance (Always Check Before Analysis)

Ensure the autosampler rinse bottle is rinsed between analytical batches with small amounts 10% HNO3 follow by DI water and refilled with acidified rinse solution. For concentration of standards and samples greater than 20 µg/L, a 5% HCl / 2% HNO3 v/v should be sufficient. For trace to ultra-trace calibrations (such as 0 to 500 ng/L) a rinse solution of 1% HCl / 1% HNO3 v/v should be sufficient.

Ensure the rinse bottle tubes are completely submerged in rinse solution. The rinse station supply tubing should be at the bottom of the rinse bottle and the rinse station return tubing should be at the top of the rinse bottle. This will ensure that the rinse is a true recirculating rinse. Inspect the rinse station flow and ensure that the rinse is not removed via the sample probe faster than it is supplied. If the rinse station is being drained faster than the supply rate, you may need to adjust the autosampler pump rate in the method or change rinse pump tubing. Replace the autosampler rinse pump tubing periodically for best performance (See the Autosampler Operator’s Manual).

CAUTION

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Chapter 5: Maintaining the Mercury Analyzer

104

Inspect the sample peristaltic pump tubing for fatigue and wear. Replace if too worn or fatigued.

If the pump tubing was left clamped overnight, install new tubing.

Pre-wet the GLS center post and be sure it remains completely wet during operation.

Check that the liquid flows, to and from the GLS, are smooth. Verify by close inspection the inlet to the GLS center post and drain exit points.

Be sure the waste bottle will not overflow during the run.

Check that the reagent bottle is sufficiently full for the number of samples to analyze.

Check that the SnCl2 is fresh and not precipitated, crystallized, yellowed, or oxidized or that the small cap on reagent bottle was left open overnight. Replace if necessary.

For autosampler maintenance, see the appropriate autosampler Operator’s Manual.

Weekly Maintenance

Remove the GLS and clean if residue is building up. See page 112 for instructions.

Clean the SnCl2 reagent bottle weekly or before refilling.

Change the pump tubing if it is too worn, appreciably “flattened,” or left in place overnight.

Empty the waste bottle. Cap all Luer fittings to carry this bottle.

Check the cells and cell windows for cleanliness.

Monthly Maintenance

Clean the GLS. See page 112 for instructions.

Clean the cells and cell windows. See page105 and following.

Replace the GLS inlet tubing and capillary insert. See page 115.

Replace the GLS drain tube. See page 116.

Check that the Perma Pure® dryer cartridge is still good. A failing dryer cartridge may be indicated by loss of mercury absorbance sensitivity and an increase in the baseline of more than 3000 µabs during a short run of 30 minutes or less. If the mercury absorbance for a given standard solution drops to 50% or more of its original value, change the cartridge. See page 117.

Yearly Maintenance

Replace the Perma Pure® dryer cartridge bi-yearly, or as needed. (See page 117.) A failing dryer cartridge may be indicated by loss of mercury absorbance sensitivity and an increase in the baseline of more than 3000 µabs during a short run of 30 minutes or less. If the mercury



105

absorbance for a given standard solution drops to 50% or more of its original value, change the cartridge.

Replace the 2-micron filter (See “Step 5: Connect the Carrier Gas Tubing” on page 40).

Autosampler Yearly Maintenance

Replace the sample probe.

Replace the autosampler rinse peristaltic pump tubing.

See the autosampler Operator’s Manual.

Removal or Inspection of the Sample Cell

Opening the Optics Access Panel

1 Turn off power to the mercury analyzer and wait five minutes.

2 Remove the four Philips screws which hold the access panel in place.

Figure 5-1 Screws for Optics Access Pane.

For continued protection against hazards indicated on the warning labels, always retighten the screws securely after servicing.

WARNING

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3 Lift the access panel and set it aside.

Figure 5-2 Optical Access Panel of QuickTrace™ M-7600 Mercury Analyzer.

4 Remove the thumbscrews on the optical cell clamps.

Figure 5-3 Optical cabinet of QuickTrace™ M-7600 Mercury Analyzer. (Note that Viton® tubing is always used for the carrier gas tubing; the color of the tubing in this figure has been modified to make it visible.)

Thumbscrews

Cells



107

Removing the Sample Cell

Refer to Figure 5-3 and Figure 5-4. The cells are designed for simple removal and cleaning. When removing the cells, be careful to not touch the cell windows at the ends of the optical cells. If the cells and cell windows are dirty, use a clean foam swab and isopropyl alcohol (spectrophotometric grade only) to clean the surfaces (see page 107). If needed, the windows can be taken out by removing the end caps and the O-rings.

Once the cell clamps have been removed, disconnect the carrier gas tubes from the cell end caps. Remove the cell end caps by holding the glass cell, pull, and rotate the end cap until it slides off the glass cell. Repeat this procedure for the reference cell. Inspect and/or clean the cell and its windows per the instructions beginning on page 107, or perform tubing maintenance as described in on page 113.

Cleaning the Cell Windows Refer to Figure 5-4.

There are two ways to clean cell windows:

Quick exposed surface cleaning (without dismantling).

Dismantling for total cleaning.

The need for cleaning (or re-cleaning) is determined by close inspection of the window (D in Figure 5-4), visible through the hole in the window cap (A), while maintaining a low-angle total surface reflection of room light on the window. Any film, fingerprint, dust, or dirt will show up dramatically against the “white” background of a low-angle surface reflection of room light from the window.

Quick Exposed Surface Cleaning

Cleaning the exposed surface of the window requires the following: a clean foam swab, Kimwipes wipers, and a bottle of isopropyl alcohol (use only spectrophotometric grade).

NOTE

Do NOT use cotton swabs. They will leave small bits of lint, which can offset the absorbance baseline and add a great deal of noise, if the lint moves or flutters in the optical beam. Use only clean foam swabs. To pre-clean the foam swab, rinse in alcohol and dry with a KIMTECH SCIENCE™ KIMWIPES® delicate task wiper. Do not dip the swab in the alcohol supply (when new, the swabs may be dirty and contaminate the alcohol supply). Instead, squirt alcohol onto the swab with a wash-bottle that is for alcohol only and dry with the Kimwipes®

wiper. Rinse and only lightly blot the swab with Kimwipes® wipers when cleaning; this will leave the swab moist with alcohol, which will be enough to clean the cell windows.

Using the pre-cleaned, alcohol-moistened swab, gently swab the outside of the cell window. Wipe with a Kimwipes wiper and blow-dry with UHP Argon or Nitrogen. The blow-drying will also remove any lint or dust that may have

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settled after cleaning. Re-check the surface reflection to see if the window is completely clean. If residue, fingerprints, or particles remain, repeat the process with another pre-cleaned alcohol-moistened foam swab until the windows are clean. If this quick procedure fails, it may be necessary to dismantle the assembly for more rigorous “total” cleaning, as described below.

Figure 5-4 Cell assembly diagram. A - Window cap C - Phillips screws E - Cell end cap

B - Window O-ring D - Sapphire windows F - Glass cell



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Dismantling for Total Cleaning

Refer again to Figure 5-4. Total cleaning requires a small Phillips screwdriver, clean Kimwipes wipers, isopropyl alcohol, and a clean plastic forceps. Carefully pull the cell end caps (E) off the cell (F), using a twisting motion, next remove the Phillips screws (C) and the window caps (A). This will allow the sapphire windows to be removed. Grip the window (D) with the forceps or wear powder free gloves when cleaning. Squirt the window with alcohol or use an alcohol wetted foam swab, then rub the surface of the window clean with a Kimwipes wiper. Rotate the forceps to a different position on the window and repeat the cleaning. Blow-dry with clean UHP Nitrogen or Argon.

Clean the non-O-ring portion and gas ports of the end cap (E) with alcohol. Do not use alcohol to clean the O-ring (B). Do not handle the cleaned parts with your fingers; use clean forceps or powder free gloves. It will be necessary to blow dry the end cap; gas orifice and fitting with clean gas before assembly. Be sure not to touch the windows after cleaning.

NOTE

It is strongly recommended to clean both reference cell and sample cell at the same time. Be careful to keep the part orientation as originally supplied.

Cell Assembly Reassemble the sapphire window (D), O-ring (B), and a window retainer (A) onto the cell end cap (E) with three flat-head Phillips screws (C), as shown in Figure 5-4. Be sure not to touch the clean O-ring (B). Handle it instead with clean forceps.

Grip the cell (F) near one end and insert the cell into the open end of the cell-end cap (E) with a pushing twisting motion. From Figure 5-5, which shows the “open” end, note that each cell end cap has two imbedded O-rings (A, B). Firmly push (with twisting motion) the cell into the open end of the cell end cap and continue pushing until both O-rings (A, B) are fully engaged.

Figure 5-5 Open End of Cell End Cap. A - O-ring B - O-ring

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Inspect the assembled cell to determine that both O-rings (A, B) are fully engaged as shown in Figure 5-6. In Figure 5-6, shown without the window and cell cap, area “C” reveals no O-ring gap. This indicates that both O-rings A and B of Figure 5-5 are fully engaged. Figure 5-7, shown with window and cell cap, also reveals no O-ring gap at point C, (the boundary between the cell end (E) and the cell end cap.

Figure 5-6 Engaged O-Ring. Shown without the window and cell cap. C - No gap visible

Figure 5-7 Engaged O-Ring. Shown with the window and the cell cap. C - No O-ring visible D - Window O-ring E - Cell

NOTE

The O-ring “D” visible in Figure 5-7 seals against the cell window.

If an O-ring is NOT engaged, as in Figure 5-6, the O-ring “B” Figure 5-8 is visible in the gap immediately at the end of the glass cell “E” Figure 5-8. This should look, instead like region “C” in Figures 5-5 and Figure 5-7. If the O-rings are not engaged correctly (as in Figure 5-8), then the system may drift and perform poorly. Assemble and attach the remaining cell end cap to the other end of the glass cell.



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Figure 5-8 O-Ring NOT Engaged. B - O-ring is visible E - Cell end

An alternate means of checking complete engagement of all O-rings in both cells is to measure the overall length of the fully assembled cell with a ruler. If the overall assembled cell length is: 8 29/32 inches (226.5mm), then both O-rings are engaged; 8 31/32 inches (228mm) indicates one O-ring is not engaged; 9 1/32 inches (229.5mm) indicates that two O-rings are not engaged (one in each end).

The glass tubing is sufficiently thick-walled that there is almost no danger of breakage (provided you have gripped near the end being inserted). However, for maximum safety, grip the glass tube with a sufficient thickness of cloth or paper towel to protect your hands in the unlikely event of glass breakage. Never insert or try to use a cracked or chipped glass tube.

Once the cell has been completely assembled, with both O-rings fully engaged, place the cell on a flat surface with both cell end cap “flats” facing downward. Rotationally adjust the cells until both “flats” are flat against the surface and parallel with each other. Recheck O-ring engagement (as above) and re-inspect both windows under low-angle reflection illumination to verify that no residual dust, lint, fingerprints, or other smudges exist on the windows. If both windows are “clean”, attach the appropriate Viton® interconnect tubing and reinstall the cells.

To reinstall the clean (and/or re-tubed) sample cell, first check that the two cell holder “flats” are parallel to each other. A simple check will reveal both cell end cap flats to be completely “tight down” against a flat surface with no gap visible between the end cap and the flat surface, when parallel.

Finally, reconnect the tubing and the optical cabinet cover.

CAUTION

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Cleaning the Gas-Liquid Separator Periodically it will be necessary to clean the Gas-Liquid Separator. Try pumping 10% HNO3 through the system for 30 minutes continuously, followed by a deionized water rinse. For more aggressive cleaning, disconnect all tubing from the GLS. Be careful not to pull hard on the tubing; this can break the glass side arms off. Instead, use a fingernail to gently work the tubing off the glass arms.

Figure 5-9 Removing the GLS.

Refer to Figure 5-9. After removing the drip tray, loosen the white, plastic retainer screw, and carefully remove the GLS by rotating the vapor outlet to the front and slide the GLS down through the clamp and exiting at the clamp bottom.

Once the GLS is removed, place it in a beaker containing 50% HNO3 v/v in DI water. If an ultrasonic bath is available, place the beaker in the bath, sonicate for 30 minutes, rinse both inside and outside with DI water, then repeat the cleaning with fresh acid. If an ultrasonic bath is not available, let the GLS soak for two hours in the 50% HNO3. If excessively dirty immerse the GLS in a mixture of 20% nitric and 20% sulfuric acid and heat on a hot plate for several hours or until clean.

Finally, rinse with DI water and dry. Reassemble GLS as shown on page 115. Tighten the plastic screw finger tight only.

INHALATION HAZARD Hot concentrated acids may cause severe burns, severe fume inhalation trauma and/or death. They should be handled only by professionally trained chemists, who employ proper safety precautions and equipment (hoods, goggles, gloves, tongs, etc.).

WARNING

GLS Retainer Thumbscrew



113

Changing the Cell Gas Tubing Begin by opening the optical access panel as shown on page 106.

Next, replace the tubing. The replacement tubes, which are in the cell gas tubing kit, are labeled and precut to length. See Figure 5-10 for label designations. Match these numbers and letters with the existing tubing to see where each labeled tube should go. It is best to replace one tube at a time.

Figure 5-10 Tubing Diagram and Connection Table.

To remove an old tube from a plastic connector, grip it near its connector and pull firmly. For glassware, it is better to slit the old tube with a razor blade or sharp knife, before removing. Alternatively, you may use the edge of a fingernail to ease the tube off its glass arm.

A simple way to avoid making wrong connections is to remove only one tube at a time, and replace this tube with the appropriate, labeled new one, before proceeding to the next tube.

Drying cartridges are replaced as assemblies (replacements with tubing already attached).

When finished, be sure no tubing is pinched when the covers are replaced.

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Replace the Tygon® drain waste as described on page 59.

Sample in and drain tubes need to be replaced monthly. If needed, a cell gas tubing kit is available from CETAC with the correct labeled tubing included, pre-cut to the correct length.

NOTE:

Do not use waste tubing other than that provided by CETAC. The interior diameter and length (3 feet) of the drain tube are optimized for maximum system stability, and should not be altered. Other tubes are similarly optimized and substitutions/alterations should not be made.



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Retubing the Gas-Liquid Separator This procedure should be followed once a month, unless the samples are excessively “dirty,” in which case the procedure should be followed more often, as needed. Improper installation can damage the GLS, so it is recommended to read the entire procedure before beginning.

This procedure shows the drain tubing being installed after the GLS is mounted on the instrument. Alternatively, the capillary, liquid mix tube, and drain tube can be installed prior to the GLS being installed in its mount.

GLS Inlet

Refer to Figure 5-11. Note tubing routing and then remove all tubing, drain sleeve (J), inlet capillary (C) and silicone sleeve (D) from the GLS using the same procedure as for Viton® tubing above.

A – Liquid mix tube

B – Capillary heat-shrink

C – Teflon capillary

D – Silicon inlet sleeve

E – Sample inlet guide

F – Hg vapor outlet

G – Frosted center post

H – Carrier gas inlet

I – Teflon drain tubing

J – Silicon drain sleeve

Figure 5-11 Assembled Gas-Liquid Separator.

1 Select a new translucent white silicone inlet sleeve (D), and push it down over the glass sample inlet guide (E) until ≈ 6mm (1/4 inch) of silicone tubing protrudes above the top of the glass inlet guide (E).

2 Select a replacement GLS Teflon inlet capillary assembly, (C). Carefully direct the capillary end of the insert into the top protruding end of the silicone tube (D), and GENTLY push straight down.

The capillary insert (C) should go down inside the inlet guide (E). Continue pushing gently downward until the exposed capillary end (C) protrudes below

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the glass guide (E). Stop pushing when the bottom edge of the capillary is about 0.5 mm (range of 0.3 - 0.6 mm) above the top of the GLS frosted center post (G).

The capillary insert should not touch the GLS center post. Pushing the capillary too far can damage the GLS.

3 Select a replacement liquid mix tube (A). Carefully slide the end of the Viton® liquid inlet tube labeled "2 <-- Liq. Mix <--" onto the protruding upper end (yellow heat-shrink, B) of the GLS inlet insert assembly.

Continuously watch the lower end of the insert, to be sure that its position does not change.

Note: Alternatively, the capillary and liquid mix tube can be mated prior to the capillary being inserted into the silicone sleeve.

4 Finally, check that the lower end of the insert is still spaced 0.3 - 0.6 mm above the frosted center post (G).

5 Install the assembled GLS into its holder on the front of the analyzer and gently tighten the GLS thumbscrew clamp (Figure 5-9).

Do not over-tighten the thumbscrew, or the GLS may crack.

The above procedure may be done with the GLS in its holder, if caution is used so the fragile glass ports are not broken.

GLS Drain

1 Select a new GLS drain tube. Prior to installation, the Teflon® drain tube should be pushed all the way into the silicone drain tube-sleeve. Do not kink the Teflon® drain tube.

2 To install, line up the end of the assembly against the glass drain and push. Refer again to Figure 5-11. The silicone tube-sleeve (J) should automatically slide over the outside of the glass tube, and the Teflon® drain tube (I) should slide inside Figure 5-11 the glass drain tube as seen in .

Keep pushing until the Teflon® tube is approximately flush with the interior wall curvature of the GLS, or about 2 mm withdrawn from this point.

3 Inspect the drain area closely. If the liquid pulsates or segments immediately prior to

CAUTION

the Teflon® drain tube end, then try a different position for this tube end. Try it further inserted (about 1 mm into the chamber), or try it with less insertion (several mm withdrawn from the chamber). Select the position that eliminates or minimizes segmentation and/or pulsation of the flow at the entry point of the Teflon® insert. A steady, high-speed stream of tiny bubbles should form within the Teflon® drain tube, and larger bubble segments should emerge from the remote end, where a longer silicone tube is attached.

CAUTION



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Replacing the Perma Pure® Dryer Cartridge Replace this cartridge if mercury absorbance diminishes to less than 50% of original value.

Figure 5-12 Perma Pure® Cartridge. (The numbers in this figure refer to the labels which are attached to each tube.)

1 Open the instrument front door for access to the dryer cartridge.

2 Disconnect the Hg vapor tube (labeled “11>Hg Vapor>12”) from the GLS arm (11).


Hg Vapor

Sample Gas

Dryer Supply

Dryer Exhaust

14 11

17 18

12

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3 Disconnect the sample gas tube (labeled “>Sample Gas>14”) from the bulkhead (14).

Figure 5-14 Disconnecting the Sample Gas Tube.

4 Disconnect the dryer gas supply tube (labeled “<Dryer Supply<17”) from the bulkhead.

Figure 5-15 Disconnecting the Dryer Gas Supply Tube.

5 Carefully unhook the remaining dryer tube (labeled “18<-Dryer Exhaust”) from the clips on the side of the instrument.

Figure 5-16 Unhooking the Dryer Exhaust Tube.



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6 Pull the Perma Pure® dryer forward to detach it from the two black clamps and set aside.

7 Install a new Perma Pure® dryer cartridge and reattach tubes described above. (When reconnecting Luer lock fittings, be careful not to kink the tubing, which could cause gas flow constriction.) Remember to route the dryer tube (“18<-Dryer Exhaust") through the cabinet cover cut out.

Figure 5-17 Suggested Arrangement of Tubing.

GLS Overflow Recovery Observation of a full or overflowing GLS, absorbance over-range, and loss of gas flow or liquid in the sample cell may indicate a GLS overflow accident. During normal operation, an overflow should not occur because the system has safeguards built in. The system has an overflow sensor built into the GLS mounting block and in the event of a drain failure the peristaltic pump will automatically stop its rotation. A GLS overflow could occur if the GLS drain outlet-tubing clogs from non-filtered digested samples during unattended operation and the analyst then starts the peristaltic pump without investigation of the stoppage. In addition, an overflow may occur if the waste pump tubes fail, or the clamp tension is too loose and or not clamped. When any of the above symptoms occur, liquid may have overflowed the Perma Pure® dryer cartridge into the optical sample cell, and possibly beyond.

If the overflow is discovered quickly, it is possible that the Perma Pure® dryer can be cleaned and dried (See Step 11) before the membrane pores become saturated and enlarged, which render the dryer useless.

Follow the steps below to correct the problem and bring the instrument performance back to normal. Also, refer to page 109.

CHEMICAL BURN HAZARD Be sure to wear protective eyewear and safety gloves when handling chemicals.

1 Shut off the instrument main power and unplug the QuickTrace™ M-7600.

2 Open the optical access panel. Inspect the sample cell (in place) and judge whether any liquid is likely to have passed through the sample cell to the “gas

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exhaust.” If liquid has passed through the system, then proceed with the below corrective action steps.

3 Remove the sample cell, GLS, and Perma Pure® cartridge (with all tubing still attached). Place all parts on a clean lab cloth (or equiv.) on the lab bench.

4 Dismantle the sample cell completely. See page 109.

Do NOT remove the cell window blocks over the optical rail if the cell is wet or full of water. Do this instead outside the instrument to avoid spillage onto the optical components.

5 Dump out all water and brine from the sample cell glass tube.

6 Rinse the sample cell glass tube with deionized water and oven dry. Alternatively, dry by rinsing with alcohol (recommended spectophotometric isopropyl alcohol (isopropanol)) and blowing dry with clean air, nitrogen, or argon.

You can supply drying gas from the argon carrier gas source by simply disconnecting the instrument gas supply and turning down the gas pressure to create a low flow.

The flow used for drying of the optical components must be less than 100 mL/min or extremely low psig such as < 5 psi. If a flow greater than this is used, the gas could blow the optical parts from your grip and cause personal injury.

7 Rinse and all remaining cell holder parts, fittings and transfer tubing with deionized water. Dry these parts by rinsing with alcohol (recommended spectophotometric isopropyl alcohol (isopropanol)) and blowing dry with clean air, argon, or nitrogen. Inspect closely to be sure all water, and/or all residual alcohol is completely eliminated from all fittings, tubes, parts, and gas ports.

When you re-assemble the cell components and install the cleaned cells, use new or clean, dry reference and sample cell tubing.

Do not oven dry any of the parts except for the sample cell glass tube. Instead, use the alcohol rinse/blow-dry procedure. Excessive heat could damage these parts.

8 Clean the sapphire window first with water and then as described on page 109.

9 Reassemble the window and cell end caps. Handle the window with clean forceps or hold by the edge with fingertips while wearing gloves (verify cleanliness by inspection with low-angle room light reflection).

10 Install the glass tube into the cell end caps, and seat firmly to fully engage both O-rings.

CAUTION

WARNING

CAUTION



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11 For Perma Pure® dryer cartridges that have gotten wet, if not already disconnected, disconnect the cartridge “sample gas” from sample cell. Attach a 10 mL Luer lock syringe filled with DI water to tube 14 and gently push the water through the dryer cartridge. The water will exit through the cartridge at tube 11 (Figure 5-12, tube numbered 11). Hold tube 11 so it is positioned over an empty beaker (do not pull on tube 11 because it may disconnect from the cartridge and render it useless). Repeat the flushing procedure again followed by a syringe filled with air, which will flush the water out of the dryer cartridge. Next, adjust carrier gas flow to 40 mL/min. Reconnect tube 11 to the GLS. Turn on the gas and allow GLS and cartridge to blow dry for one hour with flowing gas. Be sure to engage all peristaltic pump tube clamps before initiating gas flow (otherwise the gases will leak out the pump tubing and bypass the dryer cartridge).

12 Turn off gas!

13 Reattach the cartridge sample outlet tube to the QuickTrace™ M-7600 SAMPLE IN gas port, verify that the gas path tubing is correctly installed, and close the front door.

See Figure 5-10 on page 113 for the gas path tubing. At this point, all of the tubing should be attached except for the final tube end labeled “18GAS EXHAUST”.

NOTE:

More than likely, water saturation of the Perma Pure® dryer will destroy it, making replacement necessary. However, if the overflow accident is quickly caught, cleaning and drying the Nafion® membrane in the dryer immediately (per above procedures) may save it.

14 Determine whether any rinse solution (acidic stannous chloride dissolved in water) got past

Determine this by dismantling all fittings “en route” and inspecting for the presence of any liquid or salt encrustation in any of the fittings or tube ends. Make sure to check the dark purple potassium permanganate powder to see if it is wet or no longer “free flowing” in any part of the trap tube.

the sample cell (during the original accident), and into any portion of the remaining gas exhaust tubes and KMnO4 trap.

15 If no undesirable conditions are found in the above plumbing inspection, reconnect all the system plumbing and check the gas flow. The gas flow that exits the GLS should exit the exhaust fitting on the rear of the system at rate equal to the GLS exhaust rate less 1 to 2 mL/min due to internal Perma Pure® dryer restrictions. As an example, if the flow out of GLS is 100 mL/min the flow out of the exhaust port should be ~ 98 mL/min. Be sure all peristaltic pump tubes are engaged by their clamps before checking gas flow (otherwise the gases will leak out the pump tubing and bypass the flow meter).

16 If any undesirable condition was found during the above plumbing inspection proceed to the next step. Otherwise, skip to step 25.

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17 Remove the potassium permanganate mercury trap from the rear of the instrument.

POISON HAZARD The mercury vapor trap contains potassium permanganate (KMnO4) and may contain mercury. Handle and dispose of the used KMnO4 according to your laboratory’s procedures and your country’s hazardous waste regulations.

If it is completely dry, simply set it aside.

If the vapor trap is wet:

1. Empty the KMnO4 and dismantle the trap.

2. Remove the glass wool plugs.

3. Rinse all parts, fittings and tubes with deionized water and then Hydroxylamine Hydrochloride. The Hydroxylamine Hydrochloride will clean any remaining purple color from the vapor trap.

4. Dry by means of rinsing with alcohol and blowing dry with clean air, argon, or nitrogen.

5. Reinstall loose glass wool plugs into the endcaps.

6. Install one cap, and refill tube body with potassium permanganate powder (crystals). Gently tap the tube as you fill it to settle the KMnO4.

7. Install the remaining end cap and set the trap aside.

Do not reinstall the mercury vapor trap on the QuickTrace™ M-7600 instrument at this time.

18 It is still necessary to rinse residual acidic stannous chloride brine out of remaining internal and external gas exhaust tubing. Refer to Figure 5-10. Locate the sample cell exit. Disconnect the exhaust tube at the sample cell.

19 Connect the sample cell exhaust tube to a 10 mL syringe filled with water to perform a water flush of the internal and external exhaust tubes and port.

20 Place the disconnected tubing from the KMnO4 vapor trap into a waste receptacle (>100 mL) immediately under the “gas exhaust” fitting on the rear of the instrument. Alternatively, use the appropriate Luer fittings and hook another transfer tube from the rear gas exhaust fitting to the drain bottle on the floor.

21 Using the syringe, push 50 to 100 mL of deionized water through the exhaust tube, until it all passes through to the waste collection receptacle. This will wash all residual perchlorate salt encrustation and/or acidic stannous chloride brine out of the internal gas exhaust tubes and fittings.

22 Dry all of the tubing. To do this, engage the peristaltic pump tubing with all connections to the GLS and gas ports connected and allow gas to flush through the system until the exhaust tubing is dry.

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23 Reinstall all covers and close all doors.

24 Initiate a reasonable gas flow, then pump rinse solution through the GLS continuously, and let the system “purge,” “dry” and thermally stabilize for a period of 90 minutes.

25 Reinstall the permanganate trap onto the back of the instrument.

26 Operate instrument normally.

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Replacing the Hg Lamp Bulb The effect of lamp current on data quality (absorbance and noise) is minimal over the range 2 – 15 mA. When a lamp is new, the normal operating lamp current is 2 – 5 mA. As the lamp ages, the lamp current will automatically adjust to maintain constant emission intensity reaching the EOFM filter/detector.

ULTRAVIOLET RADIATION HAZARD Before opening the cover, turn off the power switch and disconnect the power cord. Sustained exposure of eyes to UV rays emitted from the lamp may result in permanent eye injury.

When to Replace or Service the Lamp

If the OVER RANGE indicator on the front of the mercury analyzer remains illuminated for more than 15 minutes when the mercury analyzer is turned on, it is time to consider replacing the lamp. The OVER RANGE indicator is illuminated whenever the current through the lamp exceeds a certain threshold.

Cleaning the EOFM

The electro-optical feedback monitor (EOFM) monitors the output of the lamp and adjusts the lamp current to ensure constant light intensity as the lamp ages. A filter ensures that the lamp output is measured only at the correct wavelength.

Use a dentist mirror and flashlight to check that the EOFM filter is not “smudged.” Refer to Figure 5-18. If it's clean, order a replacement lamp.

If the EOFM filter is dirty, clean in place using the cell cleaning procedure. If the OVER RANGE indicator continues to stay on, or if you need greater absorbance sensitivity than the old “high current” lamp can provide, replace the lamp.

Figure 5-18 M-7600 Optical Rail.

WARNING

Cells Lamp

Assembly Detector Assembly



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Figure 5-19 Lamp Assembly with Cover Removed (Side View).

Figure 5-20 Lamp Assembly with Cover Removed (Side View).

Getting a Replacement Lamp

Lamps may be ordered from CETAC Technologies by visiting www.cetac.com.

Lamp Block (Lamp is inserted from the other side of the bulkhead)

EOFM Block

EOFM Filter (Faces the lamp)

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Caring for the Lamp

Do not touch the glass part of the lamp. Fingerprints may damage the lamp.

If it becomes necessary to clean the bulb, follow the same procedure as for cleaning the cell windows on page 107.

Replacing the Lamp

BURN HAZARD Turn off power and allow the mercury analyzer to cool for at least five minutes before touching the lamp.

1 Turn off the mercury analyzer and disconnect the power cord.

2 Allow the instrument to cool five minutes.

3 Remove the cabinet screws from the electrical cabinet cover of the QuickTrace™ M-7600 and remove the cover.

Figure 5-21 Location of Screws for Access to Lamp.

4 Lift the right side of the gasket away from the sheet-metal divider to free the yellow lamp cord. It is not necessary to completely remove the gasket.

Figure 5-22 Lifting the Gasket.

CAUTION

WARNING

Yellow Lamp Cord

Gasket



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5 Locate the “heavy” yellow/orange colored lamp cord, on the right-hand side of the cabinet interior. Trace the cord backward and unplug it from the lamp controller board. Squeeze the lever on the bottom of the connector to release it.

Figure 5-23 Unplugging the Lamp Cord.

6 On the top surface of the lamp block, push back the edge of the gray foam. Under the edge of this foam is a small Allen set screw. Insert the lamp replacement tool (a 0.050 inch Allen wrench, supplied with the M-7600 completion kit) into the setscrew head and loosen the screw.

Figure 5-24 Loosening the Set Screw.

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7 Grab the old bulb where it attaches to its yellow cord and pull it straight out. The bulb will slide out easily.

Figure 5-25 Removing or Inserting the Lamp.

8 Clean the new bulb by wiping clean with a Kimwipes® wiper or optical tissue moistened with high purity (spectrophotometric grade) isopropanol, and blow dry with argon gas. Don't touch the bulb face, once it is clean.

9 Holding it by the base, carefully insert the bulb into the lamp block until it stops.

10 Rotate the bulb base until the mark on the lamp body faces straight up.

Light output from the lamp is asymmetric—it is stronger toward the positive side of the lamp.

11 Hold this position carefully while tightening the Allen set screw.

12 Plug the yellow lamp cord into the lamp controller board.

13 Replace the gasket. Start on the left end and work it onto the edge of the sheet metal.

14 Replace the cover.

15 Check the lamp current as described in the next section.

Alignment Mark

Lamp Bulb – DO NOT TOUCH



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Adjusting the Lamp Current

The lamp current can be adjusted using a potentiometer on the back of the instrument.

Note that the effect of lamp current on data quality (absorbance and noise) is typically minimal when a lamp is new. As the lamp ages, the lamp current will automatically adjust to maintain constant emission intensity reaching the EOFM filter/detector.

A new lamp needs a minimum of a 30 minute warm up time before final adjustment. After installation of the new lamp, the lamp current will automatically return to a value similar to the initial set up value.

1 Make sure the mercury analyzer is turned on and that it is connected to the PC.

2 Move the PC's display so that you can see it while you are behind the mercury analyzer.

3 Exit the QuickTrace software, if it is running.

4 Run the M-7600 Lamp Current Configuration Tool. On the taskbar navigate to Start | All Programs | CETAC QuickTrace | M-7600 Lamp Current Configuration Tool.

5 Click Search for Analyzers.

Figure 5-26 Searching for the Analyzer.

6 Select the analyzer (if more than one is found) and click Connect.

If you see an “analyzer in use” error, double-check to make sure that the QuickTrace software is not running.

7 Allow 30 minutes for the lamp to warm up.

8 While the lamp is warming up, remove the LAMP ADJUST access panel on the back of the instrument.

9 Click Check Lamp Current.

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10 Locate the mA ADJ potentiometer and use a small flat-blade screwdriver (jewelers screwdriver) to adjust the lamp current.

Figure 5-27 Adjusting the Lamp Current.

Begin by rotating the potentiometer fully clockwise until the OVER RANGE LED lights, then counterclockwise until the lamp current reads < 0.5 mA. At this point, the lamp is ready for adjustment.

Adjust the lamp current potentiometer until the marker is in the center (the green region) of the scale.

Clockwise will increase the current and counter-clockwise will decrease the current.

After each adjustment, click Check Lamp Current. Let the voltage stabilize and make fine adjustments until the system

stabilizes.

11 Reinstall the cover and begin using the mercury analyzer.



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Replacing the Fuse

FIRE AND SHOCK HAZARD Replace only with the specified fuse. Using an incorrect fuse may cause fire or personal injury.

Two fuses are located in the power supply, just above the power cord connector. Use a 5 A, 250 V, SLOBLO, 5x20 mm cylindrical fuse.

1 Disconnect the power cord.

2 Inspect all of the equipment which is plugged into the power supply for moisture or other conditions which might pose a hazard and cause the new fuse to blow.

3 Using your fingernails or a small, flat-blade screwdriver, squeeze the ends of the fuse holder.

4 Pull the fuse holder out.

Figure 5-28 Removing the Fuse Holder.

WARNING

M-7600 Power Switch

Fuses

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5 Replace the blown fuse with a new one of the same size, type, and rating.

Figure 5-29 Fuse.

6 Press the fuse holder back in until it clicks into place.

7 Plug the power cord back in.

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6 Troubleshooting the Mercury Analyzer

This chapter explains how to troubleshoot mercury analyzer problems. If you cannot solve a problem using the steps given in this chapter, you should contact CETAC Technologies Customer Service and Support.

Troubleshooting Communication Issues If the QuickTrace™ cannot connect to the analyzer:

Step 1: Check the Cable

Check that the PC is connected directly to the M-7600 with a standard Ethernet cable. To eliminate the possibility of an IP address conflict with another device on the company network, disconnect the PC from the company network while troubleshooting.

Step 2: Use the IPSetup Tool to Check the Configuration

Figure 6-1 IPSetup Tool.

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IPSetup a product of Netburner, Inc. IPSetup.exe is installed in the following folder:

C:\Program Files\QuickTrace\IPSetup

On the right hand side of the window will be a list of all Netburner-based devices (like the M-7600) that the program could find on the network. If you select one such device, its current IP configuration will appear on the left hand side of the window. These settings can be changed, and the changes applied simply by clicking on the “Set ” button in the middle. (The gateway and DNS settings are not necessary if the M-7600 is connected directly to the PC, and can be left at 0.0.0.0 or any other legal value.) After making a change this way, turn the M-7600 off, wait 15 seconds, then turn it back on.

If no device is detected by the IPSetup tool then it is likely that either the device is not powered, or it is not connected to the network that the computer running IPSetup is connected to. It should be noted that IPSetup uses UDP, so if the M-7600 is not directly connected to the PC, a router or bridge could be blocking UDP broadcasts.

Step 3: Check the Subnet Configuration Using the Define QuickTrace Hardware Tool

Once we know the device is connected to the network, and powered on we have to make sure the device is on a logical subnet that our PC can communicate with.

1 To start CETAC's Define QuickTrace Hardware tool, click Start | All Programs | CETAC Technologies | QuickTrace | Define QuickTrace Hardware.

If the instrument is seen and connected to, then subnet compatibility is assured. Skip to “Step 4: Check for an IP address conflict” on page 137.

If the instrument is not detected, then we’ll have to look at the IP address of the device.

2 Open the Windows network connections dialog.

For Windows 7, open the Windows Control Panel and select Network and Internet | Network and Sharing Center | View network status and tasks.

Figure 6-2 Network and Internet Settings (Windows 7, View by Category).



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For Windows XP, open the Windows Control Panel and select Network Connections. Note that the remainder of the instructions below assume Windows 7.

3 Click on the connection name (shown in blue).

Figure 6-3 Network Connections in the Windows Control Panel.

The network status will pop up.

4 Click Properties.

Figure 6-4 Network Connection Properties Button.

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5 Select ‘Internet Protocol Version 4’ and click ‘Properties’.

Figure 6-5 IPv4 Properties Button.

6 Click Internet Protocol Version 4 (under XP there is no 4/6) and then click Properties.

You will see a dialog that shows the TCP/IP setup for the connection.

Figure 6-6 IP Address and Subnet Mask.

Subnet masks are often 255.255.255.0 and if this is the case, then you have to make sure that the first 3 sets of numbers for each device match (192.168.1 in this example; note that this is not the default value) and that the last numbers are different. The network administrator is in charge of allocating IP



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addresses, and should be consulted if there’s any doubt about what number(s) to use. Once this configuration has been achieved, Define QuickTrace Hardware should be able to connect to the M-7600 – this will result in the device IP configuration appearing as seen below.

Figure 6-7 Example of Network Settings for the Mercury Analyzer.

Step 4: Check for an IP address conflict

Checking for an IP address conflict is an important diagnostic step. A symptom of an IP address conflict might be that the M-7600 works fine when the computer is not connected to the company network, but fails to connect, or fails intermittently when connected to the network.

1 Determine the IP address of the M-7600 using the IPSetup tool, then power off the M-7600.

2 Open a command prompt (found under the “Accessories” folder on the Start menu.)

Figure 6-8 Opening a Command Prompt Window.

3 Type the following command to change to the Windows system folder:

CD \Windows\System32

4 Type

ping <IP address of analyzer>

In our working example that would be ping 192.168.1.148. If a device with that address exists on the network (and is therefore in conflict with our M-7600) it will respond as seen at the top of the screen capture below with “Reply from <IP Address>: bytes= 32 time …” If there is no device with that IP address you’ll get a response that indicates “Destination host unreachable” as seen below for the ping 192.168.1.149 command.

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Figure 6-9 Example “Ping” Commands.

If there’s a conflict, contact the network administrator for another IP address that can be used instead.

If the IPSetup Tool Does Not Find the M-7600

1 Reset the IP configuration on the M-7600 by holding down the recessed IP RESET button on the back of the analyzer as the analyzer is powered on. Continue to hold the button for about 5-10 seconds after you turn on the M-7600. This will reset the IP address to 192.168.0.149 with a netmask of 255.255.255.0.

2 Run IPSetup again. You should now be able to see the device and configure it.

If IPSetup still cannot see the device and configure it:

3 Switch the PC network interface to a compatible IP address (for example, 192.168.0.100). See “Step 3: Check the Subnet Configuration Using the Define QuickTrace Hardware Tool” on page 134.

4 Run Define QuickTrace Hardware to set the desired IP address.

5 Turn the M-7600 off, wait 15 seconds, then turn it back on.

6 Set the PC’s network interface to a compatible setting.



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"Subnet of this PC and the M-7600 are Not Compatible" Error

The ‘Define QuickTrace Hardware’ application may display the following message:

Figure 6-10 Error Message: Incompatible Subnet

This means that the subnet configured for the secondary network card in the PC is not compatible with the subnet of the IP address configured for the M-7600. Click Yes to see what IP addresses are currently set:

Figure 6-11 Configuration Information for an Incompatible Subnet

The address of the secondary network card should show up as "Interface 1." (The interface metrics you set earlier force this network card to be listed first.) In this example, the subnet of the M-7600 is set to 11 and the subnet of the network card is set to 0. Since the laboratory network has a subnet of 0, a possible solution is to change the IP address of the secondary card to 192.169.11.156.

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Cannot Zero Instrument Perform the following steps:

Be sure instrument is fully warmed up with the peristaltic pump running at the method rate. The warm up time is dependent on the chosen method: ultra-trace may need at least 1 hour with the lamp and pump on; a normal µg/L range may only need 15 to 30 minutes. See “Starting the System” on page 81.

Check that both cells (sample & reference) and cell end caps are clean and “dry” (no liquid or dried stannous chloride obstructing the gas flow or the optical beam). See page 107 for cleaning instructions.

Check that both cell windows are clean. See page 107 for cleaning instructions.

"Integration Adjustment Reached" Messages These messages can result if the M-7600 power is cycled too rapidly. If this happens, the lamp current can get "stuck" at 6.5 mA. Always allow at least 15 seconds before turning the M-7600 back on.

1654: Upper limit integration adjustment reached Cleaning the optics is recommended.

This message means too little light is reaching the detector, and the system cannot compensate by increasing the integration period.

Turn the M-7600 off. Wait at least 15 seconds, then turn it back on.

Clean the sample cells.

Check the lamp and replace it if needed.

1655: Lower limit integration adjustment reached Contact CETAC technical support.

This message means too much light is reaching the detector, and the system cannot compensate by decreasing the integration period.

Turn the M-7600 off. Wait at least 15 seconds, then turn it back on.

Check that the sample cells are installed.

Adjust the lamp current.

Drifting Baseline The system might not be thermally stable because of insufficient warm up time. Wait longer.

Check that gas pressures are stable and correct. Variable gas flow can cause the baseline to drift. Check that no stannous chloride encrustation exists in gas tubes/fittings after a GLS overflow accident. See “Removal or Inspection of the Sample Cell” on page 105.



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Check that the gas hoses are not pinched.

Check that the lamp block heater works. The lamp block should be hot (50°C) to touch. Turn the lamp power off. Remove lamp-housing cover and touch the lamp block momentarily to verify that it is hot.

With the Hg lamp off, check that the EOFM filter is not dirty (inspect it with a dentist’s mirror and low angle flashlight).

Check that the lamp current is not too high using the QuickTrace™ M-7600 instrument controls. High current indicates a worn-out lamp, if all the windows and optics are clean.

Replace the Perma Pure® dryer cartridge.

Low Absorbance or No Mercury Response Ensure the Hg lamp is on.

Check all liquid uptake rates and gas flow. If there is no liquid or gas flow, see page 141.

Check that the reagent tube is in the reagent bottle.

Check that SnCl2 is active, not empty, not oxidized or precipitated.

Check that standards have the correct Hg concentrations in them.

Check the liquid tubes for kinks or clogs.

Check that standards have 7% HCl in them.

Check the gas flow at the GLS outlet.

Check the gas flow at the sample cell outlet.

Check that the gas flow at the KMnO4 trap outlet; does not drop in pressure or flow, this indicates an upstream block or a leak.

Check all plumbing connections for correct location and proper seal.

Replace the Perma Pure® dryer cartridge.

Mechanically block the sample beam optical path (such as with a business card) and see if absorbance goes full scale (≥ 8,000,000 µabs). This task can be accomplished in instrument controls by starting the strip chart recorder.

Reboot the system: shut down the software, and power down the QuickTrace™ M-7600 and autosampler. Restart, and check the signal.

No Liquid or Gas Flow

No Sample or Rinse Flow

Increase the tension on the sample pump tubing to start flow.

Be sure the sample, SnCl2, and “Liq. Mix” tubes are not pinched off anywhere and restricting flow.

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Ensure the rinse station is filled with acidified rinse.

Ensure all pump tubing is centered in clamps.

Check for clogs in sample tubing.

Check for kinks in the autosampler sample probe and in the reagent uptake tube.

Check for excessive pump tubing wear. Replace if needed.

No SnCl2 Flow

Increase tension on the reagent pump tubing to start flow.

Check to see that no precipitate has formed and clogged the reagent uptake and/or pump tubing.

Check for excessive pump tubing wear. Replace if needed.

No Drain Flow

Increase tension on the drain pump tubing to start flow.

Check that there is no clogging of the drain outlet tubing of the Gas-Liquid Separator. If clogged, clean or replace the drain outlet tubing.

Be sure the drain tube is not pinched off and restricting flow. Ensure it is not pinched under the autosampler foot.

Check that the vent port on the waste bottle is open, and that the bottle is not overflowing.

No Gas Flow or Low Gas Flow

Check that the in-line gas filter is not clogged. Remove the threaded connection downstream from the filter and check for gas flow at the filter outlet.

Check that all gas supply tubes are connected correctly.

Check that no gas tube is kinked or pinched.

Be sure that the KMnO4 trap is not packed too tightly (with either the glass wool plugs or the reagent crystals) and restricting flow. Repack if too tight.

Check for leaks/clogs throughout the gas system, especially after a GLS overflow accident. Check flow after each fitting/component to isolate the bad section.

Double Peak with Low Absorbance This may indicate a problem with not enough (or none at all) reagent (stannous chloride) uptake. Check the following items:

The reagent uptake tube is in the reagent bottle (rather than sitting in a deionized water container or loose in air).

There is liquid in the reagent bottle.

The reagent uptake tube is submerged below the liquid level.



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The liquid is 10% stannous chloride solution in 7% HCl.

The reagent is not “old,” precipitated, yellowed, or otherwise oxidized (for example, by leaving the bottle open overnight).

There is no clog, kink, pinch, or other obstruction in the reagent-tubing pathway.

The reagent liquid uptake rate is at least 1.5 mL/min at ~ 30% pump rate.

The autosampler sample probe tubing is the standard i.d. optimized for the mercury system: 1.0 mm i.d. (marked with a double blue band).

The sample uptake is at least 4.5 mL/min at ~ 30% pump rate.

The autosampler probe, reagent uptake tube, QuickTrace™ M-7600 mixing tee and GLS liquid/mix capillary inlet is not under pressure from a partial clog.

Poor Reproducibility Always be sure to matrix match standards and samples as closely as

possible (excluding the 7% HCl in the standards), and rinse solution should also be acidified.

Inspect the liquid flow into and out of the Gas-Liquid Separator. If either the sample in or waste out is pulsing, adjust the clamp tension on the corresponding tubing in the peristaltic pump to smooth out flows. If unable to stop the pulsing, check to see if the pump tubing is worn out. If so, replace the pump tubing. Be sure to check all the pump tubes.

Ensure the center post is fully “wet.” If partially dry anywhere on post surface, wet the post. See page 84.

Check to see if the reagent tube is in the reagent bottle.

Ensure that the stannous chloride has not been emptied or oxidized. Old SnCl2 can lead to poor results. Replace if yellow, precipitated, or just too old.

Ensure that the autosampler rinse station and rinse bottle are filled with acidified rinse.

Inspect both cell windows for fingerprints, films, or debris. If dirty, clean the windows following the procedure on page 107.

Make sure gas pressure to the QuickTrace™ M-7600 is 120 psig (825 kPa).

Check the output gas flow after the KMnO4 gas trap with a flow meter (to check this flow, all pump tubes must be clamped or plugged). This gas flow should be the same as set in the software. Check all the seals and recalibrate if necessary. Note calibration and flow stability.

Check the gas flow at the GLS exit.

Check the gas flow at the sample cell exit.

Check that the optimal instrument settings are employed. See “Using the Analyzer” beginning on page 75, the QuickTrace™ M-7600 help file, or the QuickTrace™ M-7600 Mercury Analyzer Software Manual for more details.

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Check that the peristaltic pump rollers are not severely worn. Inspect all rollers with tubing removed. Roller facets should not be “grooved.” All rollers should spin freely when turned by sliding your thumb quickly across them. None should feel “gritty” or slow in spinning. Replace the head if any one of the 12 rollers are grooved or fail to move freely.

Ensure the baseline is not drifting severely. (See page 140).

Check that the raw analog system noise is ≤ 400 µAbs peak to peak. If not, call CETAC Support.

Noisy Baseline Check that flows into and out of the Gas-Liquid Separator are not pulsing.

Pulsation indicates improperly adjusted pump clamps.

Make sure the gas pressures are correct.

Be sure the SnCl2 is fresh and not oxidized or precipitated.

Ensure the cell windows are clean.

Check that the EOFM filter is clean. Turn the Hg lamp off and ensure that the EOFM filter is not dirty (inspect it with a dentist’s mirror and low angle flashlight).

Check that nothing has been spilled on the binocular camera lenses. Turn the Hg lamp off and ensure that the camera lenses are not dirty (inspect them with a dentist’s mirror and low angle flashlight). Call CETAC Customer Service and Support if the camera lenses are dirty.

Ensure the lamp current is not excessive. For more information see “Adjusting the Lamp Current” on page 129.

Bad DL Check Low Absorbance. See “Low Absorbance or No Mercury Response”

on page 141 and “Double Peak with Low Absorbance” on page 142.

Check noisy baseline. See page 144.

Sudden Standard Absorbance Rise During Run Ensure the rinse bottle has acidified rinse.



145

Poor Accuracy Verify good reproducibility (typically ~1% RSD on standard replicates).

If reproducibility is poor, see “Noisy Baseline” on page 144.

Be sure the standards contain 7% HCl (v/v).

Be sure the samples are properly digested.

Utilize an appropriate process standard to validate digestion and container storage.

Check process (digestion blanks, containers, and rinse solution) for mercury contamination.

Check standard solution accuracy, and all gravimetric/volumetric process steps and equipment for accuracy and calibration.

If very low samples are run immediately following high samples or standards, the rinse time may not have been long enough and the result may be reading low. (Increase rinse times when sample and/or standard concentrations are widely spread).

Be sure that the rinse solution contains at least 1% HCl / 1% HNO3. If it only contains deionized water, very low samples (acidified) may read erroneously high if they immediately follow the high standard or a high sample, regardless of allocated deionized water rinse time. The problem is avoided by a acidified rinse solution in the rinse solution bot

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Returning the Product to CETAC for Service Refer to the following information if you need to return the product to CETAC Technologies for service.

Shipping the Product

Follow these guidelines when shipping the product:

Use the original packing materials. If the original shipping materials are not available, place a generous amount of shock-absorbing material around the instrument and place it in a box that does not allow movement during shipping. Seal the box securely.

Contact CETAC Technologies before shipping the product.

Pre-pay all shipping expenses including adequate insurance.

Write the following information on a tag and attach it to the product:

Name and address of the owner Product model number and serial number Description of service required or failure indications

Mark the shipping container as FRAGILE.

In all correspondence, refer to the instrument by model name or number and full serial number.

Do not return products which are contaminated by radioactive materials, infectious agents, or other materials constituting health hazards to CETAC employees.

Product Warranty Statement

NOTE

Contact CETAC Technologies or refer to the warranty card which came with your product for the exact terms of your warranty. The following copy is provided for your convenience, but warranty terms may be different for your purchase or may have changed after this manual was published.

CETAC TECHNOLOGIES warrants that for (1) one year from the date of shipment of any CETAC unit manufactured or supplied by CETAC and found in the reasonable judgment of CETAC to be defective in material or workmanship will be repaired by CETAC without charge for parts and labor.

The unit, including any defective part, must be returned to CETAC within the warranty period. The expense of returning the unit to CETAC for warranty service will be paid for by the buyer. CETAC’s responsibility in respect to warranty claims is limited to making the required repairs or replacements, and no claim of breach of warranty shall be cause for cancellation or recession of the contract of sale of any unit.

Products may not be returned which are contaminated by radioactive materials, infectious agents or other materials constituting health hazards to CETAC employees.



147

This warranty does not cover any unit that has been subject to misuse, neglect, negligence or accident. The warranty does not apply to any damage to the unit that is the result of improper installation or maintenance, or to any unit that has been operated or maintained in any way contrary to the operating or maintenance instructions as specified in the CETAC Instruction and Operations Manual. The warranty does not cover any unit that has been altered or modified so as to change its intended use. Any attempt to repair or alter any CETAC unit by anyone other than by CETAC authorized personnel or agents will void this warranty.

In addition, the warranty does not extend to the repairs made necessary by the use of parts, accessories, or fluids which are either incompatible with the unit or adversely affect its operation, performance or durability.

CETAC reserves the right to change or improve the design of any unit without assuming any obligation to modify any unit previously manufactured.

THE FOREGOING EXPRESS WARRANTY IS IN LIEU OF ALL OTHER WARRANTIES, EXPRESSED OR IMPLIED INCLUDING WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE.

CETAC’S OBLIGATION UNDER THIS WARRANTY IS STRICTLY AND EXCLUSIVELY LIMITED TO THE REPAIR OR REPLACEMENT OF DEFECTIVE PARTS, AND CETAC DOES NOT ASSUME OR AUTHORIZE ANYONE TO ASSUME FOR THEM ANY OTHER OBLIGATION.

CETAC ASSUMES NO RESPONSIBILITY FOR INCIDENTAL CONSEQUENTIAL OR OTHER DAMAGES (EVEN IF ADVISED OF SUCH POSSIBILITY), INCLUDING BUT NOT LIMITED TO, LOSS OR DAMAGE OF PROPERTY, LOSS OF REVENUE, LOSS OF USE OF THE UNIT, LOSS OF TIME, OR INCONVENIENCE.

This warranty and all matters arising pursuant of it shall be governed by the laws of the State of Nebraska, United States.

Returned Product Procedures

Claims for shipment damage (evident or concealed) must be filed with the carrier by the buyer. CETAC must be notified within ninety (90) days of shipment of incorrect materials. No product may be returned, whether in warranty or out of warranty, without first obtaining approval from CETAC. No replacements will be provided, nor repairs made, for products returned without such approval. Any returned product must be accompanied by a return authorization number. The expense of returning the unit to CETAC for service will be paid by the buyer. The status of any product returned later than thirty (30) days after issuance of a return authorization number will be subject to review. Shipment of repaired products will generally be made forty-eight (48) hours after the receipt.

Do not return products which are contaminated by radioactive materials, infectious agents, or other materials constituting health hazards to CETAC employees.

Returned Product Warranty Determination

After CETAC’s examination, warranty or out of warranty status will be determined. If a warranted defect exists, the product will be repaired at no charge and shipped prepaid back to the buyer. If the buyer desires an air

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freight return, the product will be shipped collect. Warranty repairs do not extend the original warranty period.

If an out of warranty defect exists, the buyer shall be notified of the repair cost. At such time the buyer must issue a valid purchase order to cover the cost of repair and freight, or authorize the products to be shipped back as is, at the buyer’s expense. Failure to obtain a purchase order number approval within fifteen (15) days of notification will result in the products being returned as is, at the buyer’s expense.


Chapter 7: Safety and Regulatory Information

149

7 Safety and Regulatory Information

Review this product and related documentation to familiarize with safety markings and instructions before you operate the instrument.

Characteristics

Environmental Characteristics

Operating Temperature +5° C to +40° C (+41° F to +104° F)

Non-Operating Temperature +0° C to +55° C (+32° to +131° F)

Operating Altitude Up to 2,000 m (6,562 ft)

Relative Humidity 0% to 80% non-condensing for temperatures up to 31° C, decreasing linearly to 50% at 40° C

Non-Operating Relative Humidity 0% to 95% non-condensing

Pollution Degree Pollution Degree 2 Normally no pollution or only dry, non-conductive pollution occurs. The pollution has no influence. Occasionally, however, a temporary conductivity caused by condensation may be expected.

Table 7-1: Environmental Characteristics for Safe Operation

For indoor use only.

Avoid sudden, extreme temperature changes which could cause condensation on circuit boards in the product.

These environmental characteristics indicate the conditions for safe operation. See “Establishing Optimal Operating Conditions” on page 17 for the recommended environment for the best experimental results.

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Electrical Characteristics

Power requirements

M-7600 Mercury Analyzer

Input: AC Voltage, Frequency, and Current 100-240 V ~

50-60 Hz 3 A Installation Category: CAT II (Line voltage in appliance and to wall outlet) AUX POWER Outputs:

24 V DC, max 3.33 A each connector, max 6 A total

Table 7-2: Power Requirements

Input and output connectors

Connector Description and characteristics

AUX INPUT Trigger signal input, reserved for future use. Connect only as instructed by CETAC Technologies. (Max 28V DC)

ETHERNET Ethernet connection. (Max 5V)

Table 7-3: Electrical Input and Output Connectors on the Analyzer



151

Safety Notices

INJURY HAZARD If the equipment is used in a manner not specified by CETAC Technologies, the protection provided the equipment may be impaired.

Repair or service that this not covered in this manual should only be performed by qualified personnel.

Replacement Parts

Except as otherwise noted, all replacement parts must be obtained from CETAC Technologies. Visit www.cetac.com for a current list of available spare parts.

Chemical Hazards

POISON HAZARD Do not prepare organomercurial concentrates unless you are qualified to do so. Improper handling can result in injury or death.

The handling of organomercurial concentrates which may be used in the preparation of process standards presents a substantial (potentially lethal) safety hazard. Only an experienced, professionally trained organo-metallic chemist, knowledgeable and skilled specifically in the safe handling of organomercurials (using approved apparatus and approved protection measures in an approved facility) should attempt to prepare diluted organomercurial process standards from concentrates.

CETAC Technologies assumes no liability for the handling of organomercurial concentrates or the preparation, handling, or use of diluted organomercurial process standards. Instead, CETAC Technologies recommends use of appropriate standard reference materials to validate sample preparation (dissolution/digestion) and use of inorganic mercury standards for instrument calibration.

Power Cord Set Requirements

The power cord set supplied with your instrument meets the requirements of the country where you purchased the instrument.

If you use the instrument in another country, you must use a power cord set that meets the requirements of that country.

Power Cord Safety Maintenance

The operator should check the power/signal supply cord condition. The equipment should not be operated if the mains inlet is cracked or broken. Any obvious damage to the case (from a drop or fall) should be checked by service personnel for loose or damaged parts. See individual parts lists for approved replacement parts

WARNING

WARNING

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Grounding

This equipment is designed for connection to a grounded (-earthed) outlet. The grounding type plug is an important safety feature. To reduce the risk of electrical shock or damage to the instrument, do not disable this feature.

See “Power Requirements” on page 20 and “Electrical Characteristics” on page 150 for more information.

Mains Disconnect

The power switch on the rear panel is not the mains disconnect. Power mains disconnect is accomplished by unplugging the power cord at the power supply or at the wall outlet. Ensure the power cord is easily accessible and removable, in the event of an emergency which requires immediate disconnection.

SHOCK HAZARD Ensure that power cord is disconnected before removal of any covers.

Mechanical Hazards

Figure 7-1 Overview of Mechanical Hazards.

1 –PINCH HAZARD Keep fingers, hair, and loose clothing away from moving parts when the system is powered on.

Additional hazards related to the autosampler are described in the autosampler Operator's Manual.

WARNING

WARNING

1



153

Cleaning Instructions

For additional cleaning information, see “cleaning” in the index.

To clean the exterior surfaces of the instrument, complete the following steps:

1 Shut down and unplug the instrument.

2 Wipe the instrument exterior surfaces only using a towel dampened with a lab-grade cleaning agent.

3 Repeat step 2, using a towel dampened with clear water.

4 Dry the instrument exterior using a dry towel.

SHOCK HAZARD Do not allow any liquid to enter the instrument cabinet or come into contact with any electrical components. The instrument must be thoroughly dry before you reconnect power, or turn the instrument on.

Operating Environment

SHOCK HAZARD To reduce the risk of fire hazard and electrical shock, do not expose the unit to rain or humidity. To reduce the risk of electrical shock, do not open the cabinet. All maintenance is to be performed by an Authorized CETAC Service Provider. Protection provided by the equipment may be impaired if the equipment is used in a manner not specified by the manufacturer.

SHOCK HAZARD Equipment is not intended for wet locations. Miscellaneous liquids in the equipment could cause hazardous conditions.

EXPLOSION HAZARD Do not operate in an explosive atmosphere.

WARNING

WARNING

WARNING

WARNING

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Explanation of Caution and Warning Notices

Warning symbol marked on equipment. This symbol means “Attention! Refer to the manual.”

Pinch Point – Keep hands, hair, and clothing clear of moving parts.

Lifting Hazard – Single person lift could cause injury. Use assistance when moving or lifting.

The WARNING notice denotes a hazard. It calls attention to a procedure, practice, or the like, that, if not correctly performed or adhered to, could result in personal injury. Do not proceed beyond a WARNING notice until the indicated conditions are fully understood

The CAUTION notice indicates an action which must be taken to prevent equipment damage or a serious loss of data. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met.

WARNING

CAUTION



155

Avertissements en Français This section provides French translations of notices which may appear on the instrument or on other instruments used as part of the measurement system.

AVERTISSEMENT POUR UNE PROTECTION CONTINUÉ CONTRE LES RISQUES D’INCENDIE, REMPLACER UNIQUEMENT PAR DES FUSIBLES DE MÊME TYPE ET AMPÈRAGE.

AVERTISSEMENT

SURFACES CHAUDES, LAISSER LE COUVERCLE HERMÉTIQUEMENT FERMÉ.

POUR ACCÉDER, METTRE LA TEMPÉRATURE DU FOUR À ZÉRO, OUVRIR LE COUVERCLE ET LAISSER REFROIDIR 5 MINUTES AVANT DE TOUCHER LA VERRERIE OU TOUTE SURFACE MÉTALLIQUE INTÉRIEURE.

AVERTISSEMENT TOUT CONTACT AVEC LES HAUTES TENSIONS PEUT ENTRAINER LA MORT OU DES BLESSURES SÉVÈRES. CE PANNEAU NE DOIT ÊTRE ENLEVE QUE PAR UN RÉPARATEUR QUALIFIÉ.

AVERTISSEMENT

POUR LA PROTECTION PERMANENTE CONTRE UN CHOC ÉLECTRIQUE, UNE BRÛLURE DES YEUX (RADIATION UV) OU DE LA PEAU, LAISSER LE COUVERCLE HERMÉTIQUEMENT FERMÉ LORSQUE L’APPAREIL EST SOUS TENSION. LAISSER REFROIDIR 5 MINUTES (APPAREIL ÉTEINT) AVANT D’ENLEVER LE COUVERCLE.

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Electromagnetic Interference FEDERAL COMMUNICATIONS COMMISSION (FCC) NOTICE

This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to Part 15 of the FCC Rules. These limits are designed to provide reasonable protection against harmful interference in a commercial installation.

This equipment generates, uses, and can radiate radio frequency energy and, if not installed and used in accordance with the instructions, may cause harmful interference to radio communications. Operation of this equipment in a residential environment is likely to cause harmful interference, in which case the user will be required to correct the interference at his expense.

MODIFICATIONS

The FCC requires the user to be notified that any changes or modifications made to this device that are not expressly approved by CETAC Technologies may void the user's authority to operate the equipment.

CABLES

Connections to this device must be made with shielded cables with metallic RFI/EMI connector hoods to maintain compliance with FCC Rules and Regulations.

CANADIAN NOTICE

This digital apparatus does not exceed the Class A limits for radio noise emissions from digital apparatus as set out in the interference-causing equipment standard entitled "Digital Apparatus" ICES-001 of the Department of Communications.

AVIS CANADIEN

Cet appareil numerique respecte les limites de bruits radioelectriques applicables aux appareils numeriques de Classe A prescrites dans la norme sur le materiel brouilleur: "Appareils Numeriques," NMB-001 edictee par le ministre des Communications.

Explanation of Regulatory Marks

Do not dispose in domestic household waste.

The affixed label indicates that you must not discard this electrical/electronic product in domestic household waste, in compliance with the European Waste Electrical and Electronic Equipment Directive (WEEE, 2002/96/EC).

For instructions on how to return end-of-life equipment, producer-supplied electrical accessories, or auxiliary items for proper disposal please contact the supplier or importer. In the event a supplier cannot be reached, contact CETAC Technologies customer service department at 1 (800) 369 2822.

The CE mark is a registered trademark of the European Community. This CE mark shows that the product complies with all the relevant European Legal Directives.

157

8 Glossary

A Amperes, electrical current AAS Atomic Absorption Spectrometry Abs Absorbance (-log10 T or 2-LOG10 %T)

ADC or A/D Analog-to-digital converter ADX-500 Optional autodilutor accessory ASX-500 A CETAC ASX-500 series autosampler, such as the ASX-510

autosampler or ASX-520 autosampler

Bar Unit of pressure. 1 bar = 100 kPa ≈ 14.5 psi Ar Argon carrier gas, chemical formula

CH3HgCl Methyl mercuric chloride (or “methyl mercury”), chemical formula of a common organo-mercurial

CLP Contract Laboratory Protocol (analysis protocol of U.S. EPA) cm Centimeter (10-2 meter), unit of length

Cold Vapor Direct AAS or

CVAAS

Direct Atomic Absorption Spectrometric analysis (at 253.652 nm) of “head-space” gas from a stannous chloride or stannous sulfate reactor using neither flame, nor plasma, nor furnace nor any other electro-thermal atomizer. CVAAS works only for the element mercury (Hg)

Dia. Diameter DL Detection limit. Smallest statistically detectable concentration,

where the absorbance, Abs (produced by that concentration), equals 3 times the standard deviation σ of the blank Abs

DSP Digital Signal Processor ea. Each

EOFM Electro-Optic Feedback Module; used to stabilize the Hg lamp EPA U.S. Environmental Protection Agency

EPA-245.1 The standard EPA method of water quality analysis for measuring mercury (Hg)

ETFE Ethylenetetrafluoroethylene (Tefzel), a polymeric tubing material

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158

g Gram, unit of mass or “weight” GCU Gas Control Unit, sets and regulates carrier gas flow rate GLS Gas-Liquid Separator HCl Hydrochloric Acid, chemical formula Hg Mercury, chemical symbol

Hg0 Mercury, elemental (reduced) state Hg2+ Mercuric ion, mercury in +2 (oxidized) state, typically HgCl2

HgCl2 Mercuric chloride, chemical formula HNO3 Nitric acid, chemical formula

Host Computer

The computer that controls operation of the instrument .

i.d. Inside diameter IDL Instrument Detection Limit. DL in ultra-clean, high purity acid media

(for example, 7% HCl, “Ultrex II” grade). IDL is generally measured under “favorable” operating conditions and does not involve sample digestion or preparation steps. IDL indicates what the instrument is capable of doing, if not subjected to contamination, digestion loss, storage loss, or other sample collection/preparation errors or limitations

KMnO4 Potassium permanganate, chemical formula of oxidizing reagent, and mercury exhaust trap agent

L Liter, unit of volume LED Light-Emitting Diode

QuickTrace™ system

The entire mercury analyzer system including the QuickTrace™, autosampler, peristaltic pump, etc.

mA Milliamperes (10-3 amperes), electrical current MDL Method Detection Limit; DL measured under actual reagent purity,

sample preparation, and storage conditions for samples, reagents, and containers in question. Calibration standards are generally prepared in the sample media and are carried through all sample digestion/preparation, storage and transfer steps, etc., as are samples. In the presence of significant contamination, small concentration detectability gets worse and the actual MDL should be redefined as 1/3 the contamination, but not less than the statistical MDL!

mL Milliliter (cubic centimeter, cc, 10-3 L), unit of volume mm Millimeter (10-3 meter), unit of length

MSDS Material Safety Data Sheet specifying chemical hazard type and level

N2 Nitrogen carrier gas, chemical formula Nafion® DuPont's porous polymer membrane which passes water vapor, but

not Hg vapor. nm Nanometer (10-9 meter), wavelength unit.

159

ng Nanogram (10-9 gram), mass or weight unit o.d. Outside diameter

P Transmitted radiant power, photon flux at sample detector (after passing through sample)

P0 Incident radiant power, photon flux at reference detector (before

passing through sample)

PC Personal Computer PEEK Polyetheretherketone; a machined polymeric construction material

Perma Pure Brand name of the dryer tubing which uses a DuPont Nafion® membrane.

pg Picograms (10-12 g), mass or weight unit PID Proportional Integral Differential. Description of a type of precision

heater control device ppb Parts per billion (ng/mL, 10-9 g/mL, µg/L, 10-6 g/L), concentration

unit

ppm Parts per million (µg/mL, 10-6 g/mL, mg/L, 10-3 g/L), concentration unit

ppt Parts per trillion (pg/mL, 10-12 g/mL, ng/L, 10-9 g/L), concentration unit

psi Pounds per square inch. Pressure. 1 psi ≈ 0.068 bar. 1 bar = 100 kPa psig Pounds per square inch, gauge reading (above atmospheric

pressure) PTU Precision-Timed Uptake

Pump or PP Peristaltic Pump P-P Peak to Peak. A description of how signal noise is measured (One

method) RMS Root Mean Square. A description of how signal noise is measured.

RMS = 0.707 of peak amplitude (another method), approximately one standard deviation unit

RSD Relative Standard Deviation. A measure of data precision or reproducibility

SCR Stannous Chloride Reactor Sn Tin, chemical symbol. Typically as SnCl2 reagent

SnCl2 Stannous chloride, chemical formula of reducing agent SRM Standard Reference Material, containing a certified, known mercury

level T Transmittance (P/P0), often %T or percent transmittance (P/P0 x

100%)

TC “To Contain” Designation of a type of volumetric flask calibrated to accurately contain a specified volume of liquid

TD “To Deliver” Designation of a type of volumetric flask or pipet calibrated to accurately deliver a specified volume of liquid

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160

UHP Ultra High Purity UV Ultraviolet; short wavelength region of spectrum below 370 nm

(such as 253.7 nm)

VAC Volts Alternating Current VDC Volts Direct Current

XS A substantial concentration “excess” of one chemical reactant (over another)

µg Micro-gram (10-6 g), unit of mass or weight

µL Micro-liter (10-6 L), unit of volume

µAbs Micro-absorbance units. (10-6 Abs)

161

Index autosampler

data cables, 44, 46 placement, 26 power, 40 probe installation, 36 rinse solution, 79 rinse station, 26 sample tube, 61 Z-drive, 31

avertissements, 156 avis Canadien, 157 baseline correction, 91 bulb. See lamp cleaning, 154 cold shutdown, 101 condensation. See humidity dimensions, 18 disposal, 157 dryer cartridge

inspecting, 104 Nafion membrane, 78 overflow cleaning, 119 replacing, 117 water damage, 121

earthing, 21 earthquake precautions, 20 electrical characteristics, 151 EOFM, 124 Ethernet setup, 45 exhaust, 42 FCC notice, 157 footprint, 18 fuse, 131 gas pressure

maximum, 42 minimum, 70 range 1, 98 range 2, 99

GLS cleaning, 112 inspecting flow, 90 installing, 53 overflow, 71 overflow recovery, 119 parts of, 115 tubing, 115

wetting, 72, 73, 84 grounding, 21 hazards, 153

chemical burn, 42, 71, 119 electrical, 154 inhalation, 20, 112 mechanical, 153 organomercurial, 80 poison, 152

humidity, 21, 150, 154 ICES 001, 157 installation category, 151 integration limits, 140 interference, 157 IP address, 137 IP Address, 50 IP RESET button, 138 IPSetup, 133 LAMP ON indicator, 12 lamp, mercury vapor

current, 140 replacement, 124 warm-up, 82

lamps power, 12

LEDs. See lamps lifting, 22 log book, 91 mains disconnect, 153 mercury vapor trap, 82

inspecting, 43 installing, 42 refilling, 122

Nafion. See dryer cartridge network setup, 45, 63 OVER RANGE indicator, 12, 124 over voltage category, 151 PC setup, 63 Perma Pure. See dryer cartridge physical characteristics, 18 pollution degree, 150 power

requirements, 20, 151 power cord, 152 POWER indicator, 12 reagent uptake tube, 61

Index

162

reducing agent, 69 regulatory notices, 150 return procedure, 147 safety information, 150 service, 147 SnCl2, 69 standby, 100 supplies, 14 temperature

recommended, 17 safe operating, 150

tubing cell gas, 113 kinks, 21

unpacking, 21 uptake tube (reagent), 61 vibration, 20 warranty, 147 WEEE notice, 157 work surface requirements, 20

Manual Part Number 480195 Rev 2 Printed in USA

CETAC M-7600 Mercury Analyzer Operator's Manual · Ultra-trace detection limits: < 0.5 ppt at 40 mL / min. carrier gas flow 1 Wide dynamic linear working range, ≅ 4 orders of magnitude.

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