Agilent Technologies 7697A Troubleshooting Manual
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Agilent Technologies 7697A Troubleshooting Manual

Headspace sampler
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Headspace Sampler
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  • Page 1 Agilent 7697A Headspace Sampler Troubleshooting Agilent Technologies...
  • Page 2 A CAUTION notice denotes a hazard. It prior agreement and written consent from permitted by applicable law, Agilent calls attention to an operating Agilent Technologies, Inc. as governed by disclaims all warranties, either express procedure, practice, or the like that, if United States and international copyright...

  • Page 3: Table Of Contents

    Peak Areas Not Repeatable Low Peak Area or Height (Low Sensitivity) Contamination or Carryover Log Entries and Errors Sequence Log Entries Event Log Entries (Errors) Maintenance Log Entries Tray Error Messages Leaks Leak Check General Procedure Flow Paths Agilent 7697A Troubleshooting...
  • Page 4 Carrier Gas Deviation or Shutdown HS provides all carrier flow HS provides additional flow during the injection To resolve a carrier flow deviation or shutdown Communications Troubleshooting Headspace Sampler Communications General information Using DHCP To Troubleshoot LAN Connectivity Issues Agilent 7697A Troubleshooting...
  • Page 5 If the ping failed with “Request timed out” errors If ping succeeds, but you still cannot connect The GC Does Not Start After the HS Injects Electronics To Check the Headspace Sampler Power Configuration To Perform the Instrument Self Test Thermal Shutdowns Agilent 7697A Troubleshooting...
  • Page 6 Agilent 7697A Troubleshooting...
  • Page 7 Agilent 7697A Headspace Sampler Troubleshooting Concepts and General Tasks Concepts Keeping Configuration Settings Current To View the Event Log, Sequence Log, or Maintenance Log Information Customers Should Provide When Calling Agilent for Service What Changed? This section provides general information applicable for troubleshooting problems found in the headspace sampler system.

  • Page 8: Concepts And General Tasks

    The [Status] key Be sure to also use the [Status] and [Info] keys on the HS keypad while using this troubleshooting information. These keys will display additional useful information related to the status of the HS and its components. Agilent 7697A Troubleshooting...

  • Page 9: Error Conditions

    Concepts and General Tasks Error conditions If a problem occurs, a status message appears. If the message indicates broken hardware, more information may be available. Press [Status] to cycle through the status views. Look for more detailed error messages. Agilent 7697A Troubleshooting...

  • Page 10: What Changed

    These problems tend to be related to the sample, sample preparation, the method, and the consumables (such as the analytical column). Agilent 7697A Troubleshooting...

  • Page 11: Keeping Configuration Settings Current

    The HS relies on this information to calculate flows. Not updating the HS after altering a GC column causes incorrect flows, changed or incorrect split ratios, retention time changes, and peak shifts. Agilent 7697A Troubleshooting...

  • Page 12: Headspace Sampler Logs

    To View the Event Log, Sequence Log, or Maintenance Log To access the logs, press [Logs] until the desired log displays. The display will indicate the number of entries the log contains. Scroll through the list. Agilent 7697A Troubleshooting...

  • Page 13: Information Customers Should Provide When Calling Agilent For Service

    • HS firmware revision (press [Status], then [Clear]). • HS power configuration (located on a label on the back panel of the HS to the left of the HS power cable). Agilent 7697A Troubleshooting...
  • Page 14 Concepts and General Tasks • Press the [Status] key to display previous Error, Not Ready, and other messages. To obtain service/support contact numbers, see the Agilent Web site at www.agilent.com/chem. Agilent 7697A Troubleshooting...

  • Page 15: Chromatographic Symptoms

    Agilent 7697A Headspace Sampler Troubleshooting Chromatographic Symptoms General Information Peaks Not Displayed/No Peaks Retention Times Not Repeatable Peak Areas Not Repeatable Low Peak Area or Height (Low Sensitivity) Contamination or Carryover This section provides troubleshooting information for resolving chromatographic issues in a headspace sampler system.

  • Page 16: General Information

    • The data system (acquisition setpoints, integration parameters, peak identification settings, quantitation settings, and reporting). • The GC (method or hardware). • The headspace sampler (method or hardware). To troubleshoot chromatographic symptoms, begin troubleshooting with the sample and sample preparation. Agilent 7697A Troubleshooting...

  • Page 17: Peaks Not Displayed/No Peaks

    Check for a broken transfer line. Verify there is a flow of carrier gas from the HS to the GC inlet. • Check for leaks in the other parts of the sampling system (probe, six port valve, and lines and fittings between). Agilent 7697A Troubleshooting...
  • Page 18 • Check for restrictions that block the vial pressurization flow path for filling the sample loop. Run the vial leak test. • If using HS carrier gas control, confirm that the current HS column configuration matches the column actually installed in the GC. Agilent 7697A Troubleshooting...

  • Page 19: Retention Times Not Repeatable

    If not enabled, check the sample vial for cracks or other leaks. See the Operation Guide. • If using dynamic leak checking, make sure the entered leak rate is appropriate for the sample and its preparation technique. Agilent 7697A Troubleshooting...

  • Page 20: Peak Areas Not Repeatable

    • Try shaking the sample to improve equilibration time. • Check sample loop size. If the installed sample loop is actually bigger than the configured sample loop size, precision may suffer. The vial headspace pressure may not be sufficient to repeatably fill the loop. Agilent 7697A Troubleshooting...

  • Page 21: Low Peak Area Or Height (Low Sensitivity)

    • Check that the transfer line is correctly installed at both ends. • Check for leaks at the six port valve and within the rest of the sampling system (sample probe, its connections to the six port valve). Agilent 7697A Troubleshooting...

  • Page 22: Contamination Or Carryover

    If the carryover in a series of solvent blanks does not decay for each run, the carryover is probably due to adsorbed or condensed sample in the flow path. Replace flow path parts as needed (sample loop, sample probe, transfer line, and so forth). Agilent 7697A Troubleshooting...
  • Page 23 5 to 10 for each run, the carryover is probably due to an unswept area in the flow path. If contamination exists in the six port valve, increase the purge flow or purge time to sweep residual sample from the system. Agilent 7697A Troubleshooting...
  • Page 24 Chromatographic Symptoms Agilent 7697A Troubleshooting...

  • Page 25: Log Entries And Errors

    Agilent 7697A Headspace Sampler Troubleshooting Log Entries and Errors Sequence Log Entries Event Log Entries (Errors) Maintenance Log Entries Tray Error Messages This section describes the headspace sampler (HS) logs most useful during troubleshooting. The headspace sampler logs any deviations to the Sequence log or Event log. While the...

  • Page 26: Sequence Log Entries

    When vial # was ready for injection, an external device was not ready. Vial # external timed out Vial # exceeded the method’s time limit while waiting for an external device to become ready. Start of vial equib time Agilent 7697A Troubleshooting...
  • Page 27 Spacer missing from carousel for vial #. For 12 vial model instrument only. Leak rate x.xxx mL/min Dynamic leak test failed with indicated leak rate. Check the sample vial. Vial # abort sequence The sequence was aborted due to an error condition on vial # indicated. Agilent 7697A Troubleshooting...

  • Page 28: Event Log Entries (Errors)

    Needle lifter error # # Tray Error Messages. Tray lifter error # # Tray Error Messages. Carousel error # Tray Error Messages. Shutter error # # Tray Error Messages. Six port valve error # # Tray Error Messages. Agilent 7697A Troubleshooting...
  • Page 29 BCR read error # #, t = # The barcode reader failed to decode the barcode in time, t, seconds. Check the barcode label, See the Operation Guide Barcode Reader Errors. Agilent 7697A Troubleshooting...

  • Page 30: Maintenance Log Entries

    Indicates that a tray calibration was successfully performed. Tray calibration failed Indicates that a tray calibration failed. Leak Test Passed Leak Test (Part 2) Passed Leak Test failed Indicates a leak test step failed, where ## is the part of the test which failed. Agilent 7697A Troubleshooting...

  • Page 31: Tray Error Messages

    The vial sensor senses that there is no vial in the gripper when a vial is expected. See No Vial Found in Gripper/Vial In Gripper. Received abort The stop key was pressed on the instrument while the tray was executing a command. The command was aborted. Agilent 7697A Troubleshooting...
  • Page 32 Check for any obstructions to tray movement. Gripper home failed Check for any obstructions to gripper movement. Gripper open failed Check for any obstructions to gripper movement. Gripper close failed Check for any obstructions to gripper movement. Agilent 7697A Troubleshooting...

  • Page 33: Leaks

    Agilent 7697A Headspace Sampler Troubleshooting Leaks Leak Check General Procedure Flow Paths Checking for External Leaks To Run the Restriction and Pressure Decay Test To Run the Cross Port Leak Test To Check for Leaks in the Transfer Line This section discusses leak testing in the headspace sampler (HS).

  • Page 34: Leak Check General Procedure

    1/16- in. stainless steel ZDV plug (six port valve cap). Check any potential leak points associated with any recent maintenance. Check for external leaks. See “Checking for External Leaks”. Check the GC for leaks. See the GC user documentation. Agilent 7697A Troubleshooting...
  • Page 35 Run the HS Restriction & pressure decay test. See To Run the Restriction and Pressure Decay Test. Run the HS Cross port leak test. See To Run the Cross Port Leak Test. Agilent 7697A Troubleshooting...

  • Page 36: Flow Paths

    PS - Pressure sensor Vial pressurization gas FS - Flow sensor SV - Switching valve Vent Carrier gas PV - Proportional valve Flow control module Six port valve Sample loop Transfer line Figure 1 HS flow paths (standard installation) Agilent 7697A Troubleshooting...
  • Page 37 Six port valve PS - Pressure sensor Sample loop FS - Flow sensor Transfer SV - Switching valve line PV - Proportional valve Figure 2 HS flow paths with optional G4562A 7697A Carrier Gas EPC Module Accessory installed Agilent 7697A Troubleshooting...

  • Page 38: Checking For External Leaks

    A pressure decay test cuts off carrier flow through the HS and GC. C A U T I O N To prevent damage to the flow path components (column, inlet liner, and so forth), cool the HS and GC before beginning. Agilent 7697A Troubleshooting...
  • Page 39 Fully turn the regulator pressure adjustment knob counterclockwise to shut the valve. Wait 5 min. If there is a measurable drop in pressure, there is a leak in the external connections. No drop in pressure indicates that the external connections are not leaking. Agilent 7697A Troubleshooting...

  • Page 40: To Run The Restriction And Pressure Decay Test

    [Enter]. Install a new septum into the blue leak test vial. Place the blue leak test vial into priority position 1 (111 vial model) or into tray position 1 (12 vial model). Agilent 7697A Troubleshooting...

  • Page 41: If The Test Passes

    After the test passes, restore the instrument to operating condition. If the test passes If the test passes all stages, the sampling system is leak free. If still experiencing leak- like symptoms: • Check the transfer line. • Check the interface to the GC. Agilent 7697A Troubleshooting...

  • Page 42: If The Test Fails

    • A selection to exit the test. Exit test?: Select this line then press [On/Yes] to abort the test. • A failure code See the sections below for troubleshooting information for each stage of the test. Agilent 7697A Troubleshooting...
  • Page 43 FS - Flow sensor SV - Switching valve Vent Carrier gas PV - Proportional valve Flow control module Six port valve Sample loop Transfer line 40 mL/min Figure 4 Flow paths: Needle restriction test, stage 1: Vent CLOSED (INJECT) Agilent 7697A Troubleshooting...
  • Page 44 Leaks In this stage, the displayed pressure reading should stabilize at some value. This is your baseline value. If the test fails this stage, check: • The sample probe • A leak causing no restriction value Agilent 7697A Troubleshooting...
  • Page 45 SV - Switching valve Vent Carrier gas PV - Proportional valve Flow control module Six port valve Sample loop Transfer line 40 mL/min Figure 5 Flow paths: Needle (Sample Probe) restriction test, stage 2: Vent CLOSED (STANDBY) Agilent 7697A Troubleshooting...
  • Page 46 In this stage, the pressure should stabilize at a higher value than in stage 1, depending on your sample loop size. If the test fails this stage, check: • The sample probe • The sample loop or sample loop configuration Agilent 7697A Troubleshooting...
  • Page 47 FS - Flow sensor SV - Switching valve Vent Carrier gas PV - Proportional valve Flow control module 40 mL/min 6 port valve Transfer line Figure 6 Flow paths: Needle (Sample Probe) restriction test, stage 3: Vent OPEN Agilent 7697A Troubleshooting...
  • Page 48 Leaks In this stage, the pressure should drop to a very low value since the vent is open. If the test fails this stage, check: • The vent line • The vent valve (contact Agilent for service) Agilent 7697A Troubleshooting...
  • Page 49 Flow paths: Vial leak test, stage 1: Test up to SV1 If the test fails this stage, check: • SV1, the pressurization valve (contact Agilent for service) • The O- ring seats on the PCM module connection (contact Agilent for service) Agilent 7697A Troubleshooting...
  • Page 50 Flow paths: Vial leak test, stage 2: Test 6PORT (STANDBY) If the test fails this stage, check: • The vent valve. Cap the vent line and retest. If the test passes, contact Agilent for service. If the test fails again, the vent valve is operating properly. Agilent 7697A Troubleshooting...
  • Page 51 Leaks • The sample probe connections to the six port valve • The sample loop connections to the six port valve • Port 6 on the six port valve Agilent 7697A Troubleshooting...
  • Page 52 Figure 9 Flow paths: Vial leak test, stage 3: Test 6PORT (INJECT) If the test fails this stage, check: • The sample probe connections to the six port valve • Port 6 on the six port valve Agilent 7697A Troubleshooting...

  • Page 53: To Run The Cross Port Leak Test

    Press [Carrier], then increase the flow setpoint until the carrier pressure is 172 kPa (25 psi). • Leave the GC carrier pressure or flow unchanged. Start the test. Press [Service Mode], select Cross port leak test, then press [Enter]. The test begins. Agilent 7697A Troubleshooting...

  • Page 54: If The Test Passes

    • A selection to exit the test. Exit test?: Select this line then press [On/Yes] to abort the test. • A failure code See the sections below for troubleshooting information for each stage of the test. Agilent 7697A Troubleshooting...
  • Page 55 FS - Flow sensor SV - Switching valve Vent Carrier gas PV - Proportional valve Flow control module Six port valve Sample loop Transfer line Figure 10 Flow paths: Cross port leak test, stage 1: Test 6PORT (STANDBY) Agilent 7697A Troubleshooting...
  • Page 56 Leaks If the test fails this stage, check: • A leak across six port valve ports 3 and 4, or 1 and 2. Replace the valve rotor. Agilent 7697A Troubleshooting...
  • Page 57 Figure 11 Flow paths: Cross port leak test, stage 2: Test 6PORT (INJECT) If the test fails this stage, check: • A leak across six port valve ports 4 and 5, or 1 and 6. Replace the valve rotor. Agilent 7697A Troubleshooting...

  • Page 58: To Check For Leaks In The Transfer Line

    GC. • Check for flow out of the transfer line fused silica. No flow indicates broken fused silica. • Also consider other leaks in the GC inlet (liner, O- ring, septum and so forth). Agilent 7697A Troubleshooting...

  • Page 59: Vial Handling

    Agilent 7697A Headspace Sampler Troubleshooting Vial Handling How the Headspace Sampler Handles Vials No Vial Found in Gripper/Vial In Gripper Vial Size Errors Carousel Errors Sample Probe Lifter Errors Six Port Valve Errors Shutter Errors (111 Vial Model) Tray Lifter Errors (111 Vial Model)

  • Page 60: How The Headspace Sampler Handles Vials

    • The lifters inside the HS move vials from the tray and onto the sampling probe. • The oven stores vials in a carousel. Z-axis assembly Gripper inside Z-axis assembly Gantry Vial shown on shutter Figure 12 Moving parts in the tray Agilent 7697A Troubleshooting...

  • Page 61: No Vial Found In Gripper/Vial In Gripper

    If there were no other errors reported, you can try using the HS again. If the problem recurs: • Check the vial gripper fingers and motor. • Check the sensor on the gripper and ensure it can move up and down. Agilent 7697A Troubleshooting...

  • Page 62: Vial Size Errors

    Note that 20- mL and 22- mL vials are the same height. The HS cannot distinguish between them. (An internal capacity of 20 mL or 22 mL is within the range of exterior dimensions for either vial type.) Agilent 7697A Troubleshooting...

  • Page 63: Carousel Errors

    • Check the oven shutter. Is it open or closed? • Check the carousel/tray for broken glass or other obstructions. See the procedure for cleaning the 12 vial oven tray vial oven in the Maintenance manual. • If the problem remains, contact Agilent for service. Agilent 7697A Troubleshooting...

  • Page 64: Sample Probe Lifter Errors

    (Was this error caused by another problem?) • Check the carousel/tray for broken glass or other obstructions. See the procedure for cleaning the 12 vial oven tray vial oven in the Maintenance manual. • Check vial size configuration. • Contact Agilent for service. Agilent 7697A Troubleshooting...

  • Page 65: Six Port Valve Errors

    HS. Check for obstructions in the pneumatics area (such as whether the insulating cover interferes with the valve drive shaft). If the error persists, contact Agilent for service. Six port valve motor Six port valve shaft Agilent 7697A Troubleshooting...

  • Page 66: Shutter Errors (111 Vial Model)

    • Check the HS sequence log, event log, and status displays for messages. (Was this error caused by another problem?) • Check the shutter for obstructions, for example a vial. • Contact Agilent for service. Agilent 7697A Troubleshooting...

  • Page 67: Tray Lifter Errors (111 Vial Model)

    (Was this error caused by another problem?) • Check the shutter. • Check the carousel/tray for broken glass or other obstructions. See the procedure for cleaning the 12 vial oven tray vial oven in the Maintenance manual. • Contact Agilent for service. Agilent 7697A Troubleshooting...

  • Page 68: Barcode Reader Errors

    • If the barcode failed checksum or its value did not match the expected value, check vial locations. Check barcode type used. • If the problem persists, try test vials with new labels. Be sure each vial meets the labeling requirements. Agilent 7697A Troubleshooting...

  • Page 69: Tray Errors (111 Vial Model)

    • Check vial rack installation. Racks must be installed in their clips and must lay flat. • Check for obstructions in the tray area. • Power cycle the HS. • Calibrate the HS tray. Agilent 7697A Troubleshooting...

  • Page 70: Gripper Errors (111 Vial Model)

    • Check vial rack installation. • Check for obstructions in the tray area. • Check that the gripper fingers are not sticky (contaminated by spilled sample, for example) • Calibrate the HS tray. Agilent 7697A Troubleshooting...

  • Page 71: Vial Breaks During Thermal Equilibration

    • Reused vial. Agilent does not recommend reusing headspace vials. • Vial damaged when preparing sample. • Vial does not meet guidelines for headspace sampling. • Vial oven temperature too high, exceeds boiling point(s) in sample vial. Agilent 7697A Troubleshooting...
  • Page 72 Vial Handling Agilent 7697A Troubleshooting...
  • Page 73 Agilent 7697A Headspace Sampler Troubleshooting Pressures and Flows Flow and Pressure Shutdowns Purge Flow Deviations Vial Pressurization Setpoint Deviations Carrier Gas Deviation or Shutdown To resolve a carrier flow deviation or shutdown This section describes issues related to pressures and flows within the headspace sampler, and how to resolve them.

  • Page 74: Pressures And Flows

    After about 5 minutes, the HS will shut down components to create a safe state. In general, a flow or pressure shutdown will not stop ongoing vial equilibration processing. However, no new vials will be handled. The HS will not perform injections. Agilent 7697A Troubleshooting...

  • Page 75: Purge Flow Deviations

    • Check the gas supplies. • Check for leaks. If the problem remains, the problem may be a restriction in the vial pressurization flow path or defective flow control hardware. Contact Agilent for service. Agilent 7697A Troubleshooting...

  • Page 76: Vial Pressurization Setpoint Deviations

    • If the vial pressure is too high, consider the method setpoint. Is the vial developing an equilibration pressure higher than the setpoint while equilibrating? If the problem remains, the problem may be defective flow control hardware. Contact Agilent for service. Agilent 7697A Troubleshooting...

  • Page 77: Carrier Gas Deviation Or Shutdown

    Processing of samples continues as described in “HS provides all carrier flow”. If the method is short, it is possible that the HS may not have time to shut down the flow. In this case, the deviations are still logged. Agilent 7697A Troubleshooting...

  • Page 78: To Resolve A Carrier Flow Deviation Or Shutdown

    • Press [Carrier], scroll to the appropriate flow parameter, and press [Off/No] to turn off the beeping. Turn on the flow after resolving the problem. • Check the gas supplies. • Check for leaks. • Check the transfer line installation. Is the transfer line broken? Agilent 7697A Troubleshooting...
  • Page 79 Agilent 7697A Headspace Sampler Troubleshooting Communications Troubleshooting Headspace Sampler Communications To Troubleshoot LAN Connectivity Issues The GC Does Not Start After the HS Injects This section provides basic communications troubleshooting for the Agilent 7697A Headspace Sampler. Agilent Technologies...

  • Page 80: Communications

    Each computer and instrument uses a Network Interface Card (NIC) to provide network communications. In the Agilent 7697A HS, the NIC is built- in. For some other instruments, the NIC is a separate accessory or “card” that is installed. In either case, the NIC provides communications programming and the physical connector (jack) for the network cable.

  • Page 81: To Troubleshoot Lan Connectivity Issues

    • If using many Agilent instruments (most MS and MSDs, the 7697A, and the 6890N, 6850N, or 7890A GCs) the IP address can be obtained from the front keypad. • For other instrument types, or for other addressing protocols, see the data system documentation or the instrument documentation.
  • Page 82 TTL=64”. If you are getting anything else, there is a problem with your NIC card. Reinstall the driver of the NIC adapter and if the problem is still there then change the NIC adapter and reconfigure Agilent 7697A Troubleshooting...

  • Page 83: If The Ping Failed With "Request Timed Out" Errors

    Monitor the collision lights on the switch or hub. Verify that the same IP address is used in the instrument and the data system. Agilent 7697A Troubleshooting...
  • Page 84 The instrument may be in use by another software application. Recheck the instrument configuration in the data system software. The HS must be configured as the correct type of instrument, for example as a 7697A headspace sampler, not as a GC. Agilent 7697A Troubleshooting...

  • Page 85: The Gc Does Not Start After The Hs Injects

    • System Not Ready sequence action setting for the HS method. If set to continue, the HS will inject regardless of GC readiness state. • GC readiness. If the GC is not ready, it will not start. Agilent 7697A Troubleshooting...
  • Page 86 Communications Agilent 7697A Troubleshooting...

  • Page 87: Electronics

    Agilent 7697A Headspace Sampler Troubleshooting Electronics To Check the Headspace Sampler Power Configuration To Perform the Instrument Self Test Thermal Shutdowns This section describes how to resolve issues in the headspace sampler electronics, including temperature control. Agilent Technologies...

  • Page 88: To Check The Headspace Sampler Power Configuration

    If the power configuration shown does not match the mains voltage available, contact Agilent. You will need to obtain the correct voltage configuration plug and power cord. See the Installation manual and Site Prep guide for more information. Agilent 7697A Troubleshooting...

  • Page 89: To Perform The Instrument Self Test

    Turn off the instrument. Wait approximately 1 minute, then turn on the instrument. If the main status appears in the display, the instrument passed self- test. Agilent 7697A Agilent 7697A A.01.01 A.01.01 Power on successful Power on successful Agilent 7697A Troubleshooting...

  • Page 90: Thermal Shutdowns

    • Missing or damaged insulation on transfer line • Missing external covers on HS • Sample valve cover installed over heater/sensor cable Power cycle the HS. If the problem does not resolve, contact Agilent for service. Agilent 7697A Troubleshooting...
  • Page 91 Electronics Agilent 7697A Troubleshooting...
  • Page 92 Agilent Technologies  © Agilent Technologies, Inc. 2012...

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