CETAC M-7600 Mercury Analyzer Operator's Manual

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Operator’s Manual Chapter 4: Using the Analyzer NOTE The CETAC QuickTrace M-7600 mercury analyzer measures inorganic mercury (free Hg 2+ or HgCl 2 , 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 Hg 2+ or HgCl 2, 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”. WARNING 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!) 80
CETAC QuickTrace M-7600 Mercury Analyzer Chapter 4: Using the Analyzer 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 Gas Pressure Gas Flow Rate N 2 UHP, high purity grade cylinder (dry, research grade) or Argon, high purity grade (supplied, for example, from a liquid Dewar boil-off or cylinder). 120 psig (825 kPa) 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 KMnO 4 trap is filled as described on page 42. 81
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CETAC M-7600 Mercury Analyzer Opera
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Contents 1 Introduction ...........
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M-7600 Mercury Analyzer Operator's
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1 Introduction Overview The CETAC Q
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CETAC QuickTrace M-7600 Mercury Ana
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2 Preparing for Installation Instal
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3 Installing the Analyzer Installat
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6 Troubleshooting the Mercury Analy
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8 Glossary A Amperes, electrical cu
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ng Nanogram (10 -9 gram), mass or w
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Index autosampler data cables, 44,
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Manual Part Number 480195 Rev 2 Pri
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