Agilent Technologies VGA 77 User Manual
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Agilent Technologies VGA 77 User Manual

Vapor generation accessory
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Agilent Vapor
Generation
Accessory VGA 77
and VGA 77P
User's Guide

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Summary of Contents for Agilent Technologies VGA 77

  • Page 1 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 2 1995), or as a “commercial item” as defined in FAR 2.101(a) or as “Restricted computer software” as defined in FAR 52.227-19 (June 1987) or any equivalent agency regulation or Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 3: Table Of Contents

    Color Coding Electromagnetic Compatibility EN55011/CISPR11 ICES/NMB-001 2. Introduction About the VGA 77 and VGA 77P About this Manual Specifications Environmental Power Gas Supplies Weights and Dimensions 3. Getting Started Unpacking Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 4 Connecting a Mercury Trap (for AA only) Connection to the Autosampler 4. Operation Setup General Setup Pump Adjustment AA Setup ICP Setup Operation Automatic Operation Shutting Down Changing Modules 5. Analytical Notes Background Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 5 Reductant—Sodium Borohydride Pump Tubing Sources (AA only) Basic Methods Antimony Arsenic Bismuth Mercury Selenium Tellurium Additional Notes References Additional References 6. Maintenance and Spare Parts Cleaning Procedures General Absorption Cell Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 6 Contents Gas/Liquid Separator Tubing Replacement Procedures Pump Tubes Reaction Coil Uptake Capillary Tubes Fuses Spare Parts 7. Appendix – AA Performance Log Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 7: Safety Practices And Hazards

    Do not position the equipment so that it is difficult to operate the disconnecting device. Verifying Safe State The following general safety precautions must be observed during all phases of operation, maintenance and service of this instrument. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 8: Hazard Warnings

    Contact with these circuits, devices and components can cause death, serious injury or painful electric shock. Covers that are retained by screws on the VGA 77 may be opened only by Agilent field service engineers. Use of the wrong supply voltage, connection of the accessory to an...

  • Page 9: Chemical Hazards

    Warning Messages The following symbol may be used on warning labels attached to the Agilent VGA 77. When you see this symbol, refer to the relevant operation or service manual for the correct procedure referred to by that warning label.

  • Page 10: Information Symbols

    Information Symbols A ‘Note’ is used to give advice or information. Mains power on Mains power off Fuse Single phase alternating current Caution, disconnect all supplies, risk of electric shock Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 11: Color Coding

    This device complies with the requirements of CISPR11, Group 1, Class A as radiation professional equipment. Therefore, there may be potential difficulties in ensuring electromagnetic compatibility in other environments, due to conducted as well as radiated disturbances. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 12: Ices/Nmb-001

    Technologies could void the user’s authority to operate the equipment. ICES/NMB-001 This ISM device complies with Canadian ICES-001. Cet appareil ISM est conforme à la norme NMB-001 du Canada. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 13: Introduction

    Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES) applications. Unless otherwise specified, both the VGA 77 and VGA 77P will be refered to as VGA 77 throughout the rest of this User’s Guide. Vapor generation is an extremely sensitive procedure used for determining the level of mercury, arsenic, selenium and a range of other hydride-forming elements in samples.

  • Page 14: About This Manual

    As you use this manual, there are some procedures that will apply to specific applications only. For example, the section referring to ‘Installing the Cell’ does not apply if you are using your VGA 77 with an Agilent ICP-OES system. The instructions will inform you when this occurs.

  • Page 15: Power

    Complies with CEE7 sheet vii or NFC61.303VA Gas Supplies Argon or nitrogen, 99.99% pure (minimum) Only argon gas can be used when the VGA 77 is coupled with an ICP NOTE spectrometer. The inert gas must be dry and dust-free, otherwise you must insert a suitable filter in the supply line.

  • Page 16: Weights And Dimensions

    195 mm 6 kg 13 in. 14 in. 8 in. 13 lb Shipping dimensions 590 mm 490 mm 320 mm 10 kg 23 in. 19 in. 13 in. 22 lb Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 17: Getting Started

    Carefully open the shipping case and the enclosed packages. Inspect all parts for damage in transit. Any damage should be reported immediately. You should have received the following: VGA 77 pump unit (with mounting bracket if ordered for the  700 Series ICP-OES instruments) Cover for the pump unit ...

  • Page 18: Installation

    During installation, refer to the following diagram to help you identify the different parts of your VGA and pump module. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 19: Installation Checklist

    See Page 22. Check the environmental requirements. See Page 15.  Install the pump unit. See Page 24.  Install the reagent module. See Page 24.  Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 20: Gas Supply Requirements

    (AA only). See Page 41. Gas Supply Requirements A regulated supply of argon must be provided for your VGA 77 through the captive hose located in the right side panel. You may also use nitrogen with the AA reagent module only.
  • Page 21 2 Attach a regulator to control the flow of argon to the VGA 77. 3 Place a tap in the argon supply to the VGA 77. The tap is required to shut off the argon supply to the vapor generator, as gas can flow through the VGA 77 even when it is switched off.

  • Page 22: Power Supply Requirements

    Getting Started The indicator light is the single blue light on the top panel of the accessory. If the indicator light turns on, switch the VGA 77 off immediately, rectify the gas supply problem, then switch the VGA 77 back on. If the indicator light again turns on, you should call your Agilent field service engineer.
  • Page 23 230 +14% -6% Down 230 +6% -14% Down Down 220 ± 10% Down Down 120 ± 10% 100 ± 10% Down Selector switches Figure 2. Side of the VGA Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 24: Installing The Pump Unit

    ICP-OES, you should place the VGA 77 flat on a bench, close to the sample compartment of the instrument. When the VGA 77 is in position, fit the drip tray to the front of the pump unit by positioning the large holes over the studs on the front of the VGA 77 and sliding the tray downwards.

  • Page 25: Installing The Drain Tubing

    WARNING Corrosive Liquid Waste solutions from the VGA 77 may contain concentrated acids which can cause severe burns. Your waste vessel must be of durable, acid-resistant material. Do not use a glass container. Locate the vessel where it cannot be knocked over.
  • Page 26 The end of the tube must be above the surface of the liquid in the waste vessel. NOTE If the end of the drain tube is submerged, possible back-pressure may lead to unreliable results. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 27: Installing The Vga 77 Pump Tubing

    Ensure that the tubing is free of kinks or sharp bends so that the waste liquid will drain freely into the waste vessel. Use only the purple-black tubing for draining the ICP/VGA 77 system. Other NOTE smaller diameter pump tubing, for example the black-black tubing, may not give a large enough drain flow rate.
  • Page 28 Adjust the speed of the peristaltic pump on the ICP spectrometer to ensure that liquid is being pumped out of the gas/liquid separator faster than it is being pumped in by the VGA 77. For best results, try not to overfill the gas liquid separator and try not to completely empty it.

  • Page 29: Installing The Burner Clamp

    Mark 7 Burner The VGA 77 is supplied with a cell holder for the Mark 7 burner. The Mark 7 does not require mounting brackets as the cell holder simply sits on top of the burner.
  • Page 30 Figure 7. Cell holder pulled forward with cut-outs hooked around burner edge Lower the holder into position. Figure 8. Lowering the cell holder into position on the Mark 7 burner Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 31 Use the screws provided to fix the burner clamps in position. The clamps can be left permanently installed since they will not interfere with NOTE normal flame analyses. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 32 Fit the clamp over the burner so that the two positioning lugs at each end of the clamp rest on top of the burner, on either side of the burner slot. Tighten the clamping screws. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 33: Installation Of Zeeman Adapter For 240Z/280Z Aa

    VGA 77 for Zeeman Adapter. When assembled, the adapter is hooked over the sample compartment. The VGA 77 for Zeeman Adapter is shipped with the Standard Cell Holder and a bracket for the ETC 60 Workhead Mk 2.
  • Page 34 Heavy Weight The workhead weighs approximately 16 kg (35 lbs). To avoid injury or damage always handle carefully The VGA 77 can be fitted to the front of the instrument as described in the NOTE instrument operation manual. Make sure that the sample compartment is empty.
  • Page 35 Figure 14. Adapter, standard cell holder and cell inside sample compartment Cell Holder and Adapter Removal The standard cell holder must be removed to allow installation of the ETC 60 Workhead Mk 2. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 36: Installing The Cell

    In these locations you should use the flow-through mercury cell together with a suitable trap (see Page 41). Sharp Objects WARNING Absorption cells are fragile. Handle with care. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 37 Place the cell in its holder on top of the burner. Installing a Standard Absorption Cell on Older Burners To install a standard absorption cell on older burners (e.g., Mark VI, Mark VI-A, Mark V): Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 38: Connecting The Gas/Liquid Separator Outlet

    NOTE Connecting the Gas/liquid Separator Outlet The VGA 77 is supplied with a length of black fluoro-elastomer tubing (AA only). This tubing is used to connect the vapor outlet of the gas/liquid separator to the inlet stem of the quartz absorption cell.
  • Page 39 When the VGA 77 is not being used, disconnect the tubing from the separator NOTE and store the cell in its holder at the front of the module.
  • Page 40 Use a sharp scalpel to neatly cut an appropriate length of the black fluoro-elastomer tubing supplied. Fit the large black fluoro-elastomer tubing over the vapor outlet of the plasma gas/liquid separator. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 41: Connecting A Mercury Trap (For Aa Only)

    Connect the free ends to a ‘T’-piece and then to a suitable mercury trap in accordance with local regulations governing the discharge of mercury vapor. Fitting is easier if the ends of the tubing are first softened in hot water. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 42: Connection To The Autosampler

    Getting Started Bubble type collectors must not be used, because the VGA 77 is not designed to CAUTION accommodate the excessive back pressure generated by such collectors. Using bubble type collectors may lead to vapor being forced through the drain of the gas/liquid separator and results in an unreliable signal.

  • Page 43: Operation

    These safety practices should include the wearing of appropriate safety clothing. In the VGA 77 system, highly concentrated acids are being pumped under pressure. If a leak occurs, acid could be sprayed from the system and cause serious personal injury.

  • Page 44: Setup

    Set the regulator to the recommended pressure and turn on the inert gas supply. Ensure that the inert gas supply is turned on before switching on the VGA 77 NOTE power. If you start to pump solutions through the system before the inert gas is turned on, the signal will be unreliable.
  • Page 45 Repeat Step 5 with the rear pressure adjusting screw. Measure the uptake rate through the sample pump tubes. The uptake rate should be within the range 6–8 mL/min. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 46 NOTE Appendix A at the end of this manual. If you are using the VGA 77 with an ICP system, you must now adjust the speed CAUTION of the instrument peristaltic pump until liquid is being pumped out of the gas/liquid separator faster than it is being pumped in by the VGA 77.

  • Page 47: Aa Setup

    Follow all instructions and observe all warnings. Set the acetylene flow rather higher than normal in order to obtain a fuel-rich air-acetylene flame. This is required for igniting the flame. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 48 WARNING Explosion Hazard With the VGA 77 cell installed, the burner will be lower than usual, and a standard mixture or a fuel-lean mixture may not ignite readily. To avoid an explosive accumulation of fuel and oxidant in the sample compartment, ALWAYS ensure that the gas mixture is fuel-rich before operating the Ignite button.

  • Page 49: Icp Setup

    The following procedure conditions the ICP system for the vapor generation analysis. This procedure should be carried out: When the system is first installed  After the system has been completely flushed and cleaned  Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 50 View the signal as you alternate between the blank and top calibration standard. Use the cursor to determine the suitable delay time required. Due to the high sensitivity of the VGA 77/ICP-OES system, the upper NOTE concentration of standards used for calibration is limited (by memory effects etc.).

  • Page 51: Operation

    You can use the VGA 77 with non-Agilent instruments and autosamplers. The general procedure for using automatic samplers is given in the next section. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 52: Automatic Operation

    Operation Automatic Operation Operation of the VGA 77 is not interlocked to the system. In the event of gas CAUTION supply failure, pumping faults, or if the reagent containers are emptied, the program will not be automatically stopped and results from the program will not be analytically valid.

  • Page 53: Shutting Down

    Switch the VGA 77 off, but leave the inert gas supply on at the regulator. Open the pressure bar and swing the pump tube beds clear of the pump rollers. Remove the pump tubes from the pump rollers and release them from the retaining bracket.

  • Page 54: Changing Modules

    Disconnect the inert gas connections from the pump unit to the module (refer to Page 24, Steps 4 and 5). Undo the locking screw on the bottom left of the VGA 77 frame. Ensure the drain tube is completely empty, and remove it from the module.

  • Page 55: Analytical Notes

    Memory Effects Background Absorption (AA only) Laboratory Procedures General Standards Reductant—Sodium Borohydride Pump Tubing Sources (AA only) Basic Methods Antimony Arsenic Bismuth Mercury Selenium Tellurium Additional Notes References Additional References Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 56: Background

    Nitrogen gas can be used with the AA reagent module. NOTE The following figure shows a schematic diagram of the VGA 77. To spectrometer Peristaltic Gas/liquid Reaction coil...

  • Page 57: Factors Affecting The Formation Of Hydrides

    The gas containing the element of interest then passes out of the separator into the spectrometer where it is analyzed. As the VGA 77 produces a continuous signal, you should use the integration mode with Agilent AA or ICP-OES systems. (Agilent AA users can also use PROMT mode.)

  • Page 58: Interferences

    Al, B, Ba, Be, Ca, Cr, Cs, Ga, Hf, Hg, K, La, Ge, In, Ni, Pb, Pd, Pt, Li, Mg, Mn, Na, Rb, Sr, Ti, V, Y, Zn, Zr Re, Rh, Ru, Se, Sn Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 59: Contamination

    NOTE bismuth, mercury, selenium and tellurium. You must always ensure that the VGA 77 system is completely free of residual iodide ions (e.g., KI) before attempting to determine these elements. The most practical way of minimizing contamination problems is to provide a separate module (including the reagent containers and pump tubes) for these elements.

  • Page 60: Laboratory Procedures

    It is, of course, standard practice to check the analytical signal from the blank solution before calibrating the instrument and carrying out the analytical program. Dispose of waste in accordance with relevant safety practices. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 61: Standards

    When concentrated acid is first pumped through the acid tube, the inside of the NOTE tubing may turn white, but this does not impair the efficiency of the tube. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 62: Sources (Aa Only)

    Sources (AA only) Hollow cathode lamps or UltrAA lamps can be used for all VGA 77 methods for AA analysis. Basic Methods The hydride-forming elements may exist in more than one oxidation state in samples and standards.

  • Page 63: Arsenic

    As , reduction by potassium iodide is not required. Reductant container: NaBH 0.6% w/v (see also above) NaOH 0.5% w/v Acid container: 5 to 10 M HCl Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 64: Bismuth

    ), will be necessary. If digestion is necessary, use acid digestion, or ashing with an appropriate ashing aid. Simple dry ashing is not recommended as the mercury will be lost. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 65 Refer to Page 41. Mercury can be determined using stannous chloride as the reductant. Reductant container: SnCl (25% w/v) in HCl (20% v/v) Acid container: Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 66: Selenium

    If digestion is necessary, use acid digestion, or ashing with an appropriate ashing aid. Simple dry ashing is not recommended because selenium is highly volatile and recovery will be poor. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 67: Tellurium

    70-90 °C for at least 10 minutes and cool to room temperature before analysis. Reductant container: NaBH 0.6% w/b NaOH 0.5% w/v Acid container: 5 M HCl (Higher acid concentrations will reduce the analytical signal.) Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 68: Tin

    Some improvement in calibration linearity has also been noted. The concentration of acid pumped into the VGA 77 is also critical in tin determinations, and the analytical signal will be severely depressed at concentrations higher than 0.5 M. (See Page 57 ‘Acid Concentration’.)

  • Page 69: Additional Notes

    Appl. Spectrosc., 1985, Vol 39 (1), 48  Jiri Dedina and Dimiter L. Tsalev, Hydride Generation Atomic  Absorption Spectrometry. Published by John Wiley and Sons, Edited by J.D. Winefordner. ISDN 0 471 953644 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 70 Analytical Notes This page is intentionally left blank. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 71: Maintenance And Spare Parts

    Spare Parts Cleaning Procedures General The VGA 77 uses high concentrations of HCl. Continual exposure to HCl fumes may damage the instrumentation. Maintain an efficient exhaust system during VGA determinations and remove HCl solutions from the VGA 77 and the spectrometer when you finish your analyses.

  • Page 72: Absorption Cell

    Do not leave the cell in the sodium hydroxide for too long because this solution CAUTION may accelerate cell devitrification. Avoid handling the central part of the quartz cell with bare hands after it has been cleaned or while it is in use. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 73: Gas/Liquid Separator

    Do not allow hydrochloric acid solutions to remain in the separator. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 74 Refit the separator into its mounting bracket, secure it with the retaining strap and reconnect all tubing. If the system is not to be used for some time, the separator should be filled with distilled water. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 75: Tubing

    KI (i.e., As or Sb). If there is no KI contamination, you can clean the tubing by flushing it well with distilled water. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 76: Replacement Procedures

    You will find it easier if you remove all of the ‘T’ pieces and pump connectors. Hold the upper ‘T’ piece and sleeve firmly with one hand and pull the reaction coil out of the sleeve. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 77: Uptake Capillary Tubes

    Fuse information on the rear of the instrument is the most up to date. For safety reasons, any other internal fuse or circuit breaker is not operator- NOTE accessible, and should only be replaced by Agilent authorized representatives. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 78 Reconnect the unit to the mains power supply. If a fuse blows repeatedly, it may indicate other problems with the accessory. NOTE You should contact your local Agilent sales office and arrange a service call. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 79: Spare Parts

    Spare Parts Use only Agilent supplied parts unless otherwise indicated. NOTE The following spare parts are available from Agilent for your VGA 77: Module for AA includes reagent module, tubing and connectors 9910062100 Module for ICP includes module, tubing and connectors 9910062200 Absorption cell for AA.
  • Page 80 Maintenance and Spare Parts This page is intentionally left blank. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...

  • Page 81: Appendix - Aa Performance Log

    Appendix – AA Performance Log 7. Appendix – AA Performance Log Date Operator Uptake rate Element Concentration Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 82 Appendix – AA Performance Log This page is intentionally left blank. Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide...
  • Page 84 Analytical Notes  Laboratory Procedures  Maintenance Procedures  Instrument Cleaning  Spare Parts  Performance Log  © Agilent Technologies 1993, 1994, 1996, 1997, 1999, 2000, 2003, 2004, 2010, 2012, 2014 and 2016 12/16 *8510104700* *8510104700* 8510104700 Issue 13...

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