Agilent Technologies 7697A Operating instructions

Agilent Technologies
Agilent 7697A
Headspace Sampler
Troubleshooting

Notices
© Agilent Technologies, Inc. 2012
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laws.
Manual Part Number
G4556-90018
Edition
Third edition, January 2012
Second edition, November 2011
First edition, January 2011
Printed in USA
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Wilmington, DE 19808-1610 USA
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CAUTION
A CAUTION notice denotes a hazard. It
calls attention to an operating
procedure, practice, or the like that, if
not correctly performed or adhered to,
could result in damage to the product
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proceed beyond a CAUTION notice
until the indicated conditions are fully
understood and met.
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A WARNING notice denotes a hazard.
It calls attention to an operating
procedure, practice, or the like that, if
not correctly performed or adhered to,
could result in personal injury or
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WARNING notice until the indicated
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met.

Agilent 7697A Troubleshooting 3
Contents
1 Concepts and General Tasks
Concepts 8
How to troubleshoot using this manual 8
The [Status] key 8
Error conditions 9
What Changed? 10
Keeping Configuration Settings Current 11
Sample loop size 11
Gas configuration 11
Column configuration 11
Headspace Sampler Logs 12
The Sequence log 12
The Event log 12
The Maintenance log 12
To View the Event Log, Sequence Log, or Maintenance Log 12
Information Customers Should Provide When Calling Agilent for
Service 13
2 Chromatographic Symptoms
General Information 16
Peaks Not Displayed/No Peaks 17
Retention Times Not Repeatable 19
Peak Areas Not Repeatable 20
Low Peak Area or Height (Low Sensitivity) 21
Contamination or Carryover 22
3 Log Entries and Errors
Sequence Log Entries 26
Event Log Entries (Errors) 28
Maintenance Log Entries 30
Tray Error Messages 31
4Leaks
Leak Check General Procedure 34
Flow Paths 36

4Agilent 7697A Troubleshooting
Checking for External Leaks 38
To Run the Restriction and Pressure Decay Test 40
If the test passes 41
If the test fails 42
To Run the Cross Port Leak Test 53
If the test passes 54
If the test fails 54
To Check for Leaks in the Transfer Line 58
5 Vial Handling
How the Headspace Sampler Handles Vials 60
No Vial Found in Gripper/Vial In Gripper 61
Vial Size Errors 62
Carousel Errors 63
Sample Probe Lifter Errors 64
Six Port Valve Errors 65
Shutter Errors (111 Vial Model) 66
Tray Lifter Errors (111 Vial Model) 67
Barcode Reader Errors 68
Tray Errors (111 Vial Model) 69
Gripper Errors (111 Vial Model) 70
Vial Breaks During Thermal Equilibration 71
6 Pressures and Flows
Flow and Pressure Shutdowns 74
Purge Flow Deviations 75
Vial Pressurization Setpoint Deviations 76
Carrier Gas Deviation or Shutdown 77
HS provides all carrier flow 77
HS provides additional flow during the injection 77
To resolve a carrier flow deviation or shutdown 78
7 Communications
Troubleshooting Headspace Sampler Communications 80
General information 80
Using DHCP 80
To Troubleshoot LAN Connectivity Issues 81

Agilent 7697A Troubleshooting 5
If the ping failed with “Request timed out” errors 83
If ping succeeds, but you still cannot connect 83
The GC Does Not Start After the HS Injects 85
8 Electronics
To Check the Headspace Sampler Power Configuration 88
To Perform the Instrument Self Test 89
Thermal Shutdowns 90

6Agilent 7697A Troubleshooting

7
Agilent 7697A Headspace Sampler
Troubleshooting
Agilent Technologies
1
Concepts and General Tasks
Concepts 8
Keeping Configuration Settings Current 11
To View the Event Log, Sequence Log, or Maintenance Log 12
Information Customers Should Provide When Calling Agilent for
Service 13
What Changed? 10
This section provides general information applicable for
troubleshooting problems found in the headspace sampler
system.

8Agilent 7697A Troubleshooting
1Concepts and General Tasks
Concepts
This manual provides symptoms associated with headspace
sampler (HS) hardware or associated chromatographic
output, Not Ready messages, and other common issues. It
also provides the corresponding tasks to perform should you
experience these symptoms.
Each section describes a problem and provides a bulleted list
of possible causes for you to troubleshoot. These lists are not
intended for use in the development of new methods. (For
help when developing methods, see the Advanced Operation
Guide.) Proceed with troubleshooting under the assumption
that method(s) are working properly.
This manual also includes common troubleshooting tasks as
well as a list of information needed prior to calling Agilent
for service.
How to troubleshoot using this manual
Use the following steps as a general approach to
troubleshooting:
1Observe the symptoms of the problem.
2Check the HS status displays and logs, especially the
sequence log and event log. Check the GC logs, events,
and display. If using a data system, check its logs also.
These logs may contain valuable information that directly
indicates the root cause of problem.
3Consider what may have changed recently. See “What
Changed?”.
4Consider whether the symptom can be caused by the GC.
5Look up the symptoms in this manual using the table of
contents or the search tool. Review the list of possible
causes of the symptom.
6Check each possible cause or perform a test that narrows
the list of possible causes until the symptom is resolved.
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.

Concepts and General Tasks 1
Agilent 7697A Troubleshooting 9
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.

10 Agilent 7697A Troubleshooting
1Concepts and General Tasks
What Changed?
When troubleshooting, keep the following points in mind:
•If the problem occurred suddenly, look for what changed.
Often sudden issues occur due to discrete events, such as
maintenance, changes in gas supplies, changing to a
different method or analysis, a defective part, and so
forth. Resolving a sudden change often involves changing
a consumable item, loading the correct method, or
replacing a defective part.
•If the problem happens gradually, for example, a steadily
rising baseline or gradual increase in ghost peak areas,
look for routine maintenance or changes in the method to
resolve the problem. These problems tend to be related to
the sample, sample preparation, the method, and the
consumables (such as the analytical column).

Concepts and General Tasks 1
Agilent 7697A Troubleshooting 11
Keeping Configuration Settings Current
Certain configurable items in the HS must always be kept
current. Failure to do so will lead to reduced sensitivity,
chromatographic errors, and possible safety concerns.
Sample loop size
Reconfigure the sample loop size whenever you change the
sample loop.
To confirm the sample loop size:
1Press [Config].
2Scroll to Loop Volume (mL).
Gas configuration
Reconfigure the HS every time the gas type is changed. If
the HS is configured to a gas other than what is actually
being plumbed, incorrect flow rates will result.
To confirm the gas configuration:
1Press [Config].
2Scroll through the display entries to see the configured
gas types.
Column configuration
If using HS carrier gas control, reconfigure the HS every
time the GC column is trimmed or changed. Also verify that
the data system reflects the correct column type, length, id,
and film thickness. 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.
WARNING
Always configure the HS appropriately when working with
hydrogen. Hydrogen leaks quickly and poses a safety concern if
too much of it is released into the air or into the GC oven.

12 Agilent 7697A Troubleshooting
1Concepts and General Tasks
Headspace Sampler Logs
The HS maintains internal event logs. Use these logs to
troubleshoot problems, especially when a message no longer
appears on the display. The most useful logs for
troubleshooting are the Sequence log and the Event log.
The Sequence log
The Sequence log contains an entry for up to 256 significant
events that occurred during the sequence. These entries
include vial start and stop times, as well as deviations from
the method. The HS also logs parameter changes, method
changes, and sequence changes (if these occur during
sequence execution). If the log becomes full, the HS
overwrites the oldest entries. The log clears every time the
HS starts a new sequence.
The Event log
The Event log contains up to 250 entries for general events
(events not related to a sequence) that occur to the HS. For
example, this log records power on/off events, faults, and
firmware updates. If the log becomes full, the HS overwrites
the oldest entries.
The Maintenance log
The Maintenance log contains up to 128 entries that record
whenever a maintenance counter crosses a limit or when the
counter is reset. If the log becomes full, the HS overwrites
the oldest entries.
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.

Concepts and General Tasks 1
Agilent 7697A Troubleshooting 13
Information Customers Should Provide When Calling Agilent for Service
Gather the following information before contacting Agilent
for service:
•Symptoms.
•Problem description. Record details from the instrument
logs and status screen.
•Hardware installed and parameters/configuration when
the error occurred: sample, supply gas types, gas flow
rates, GC detectors/inlets installed, and carrier gas
configuration.
•Data system information: data system name, version, and
also driver version. (Obtain the driver version from the
live Status display, or from the instrument configuration
utility.)
•Any messages that appear on the GC display.
•Results of any troubleshooting tests you have run.
•Instrument details. Obtain the following information:
•HS serial number, which can be found on a sticker
located beneath the keypad on the bottom right corner
of the instrument.
•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).

14 Agilent 7697A Troubleshooting
1Concepts 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.

15
Agilent 7697A Headspace Sampler
Troubleshooting
Agilent Technologies
2
Chromatographic Symptoms
General Information 16
Peaks Not Displayed/No Peaks 17
Retention Times Not Repeatable 19
Peak Areas Not Repeatable 20
Low Peak Area or Height (Low Sensitivity) 21
Contamination or Carryover 22
This section provides troubleshooting information for
resolving chromatographic issues in a headspace sampler
system.

16 Agilent 7697A Troubleshooting
2Chromatographic Symptoms
General Information
When troubleshooting chromatographic symptoms, always
remember that the headspace sampler is only one part of
the system. Evaluate the whole system to isolate the
problem. Often, issues that appear in the chromatography
can be caused by a problem in one or more of the following,
in order:
•The sample.
•The sample preparation (including the consumable
hardware, such as vials, septa, syringes, solvents, and so
forth).
•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.

Chromatographic Symptoms 2
Agilent 7697A Troubleshooting 17
Peaks Not Displayed/No Peaks
This topic assumes that peaks are no longer displayed when
analyzing a sample using an existing method (not during
method development).
•Check the GC.
•Check for error messages and log entries.
•If possible, mount an automatic liquid sampler (ALS)
over the inlet and inject a sequence of internal or
calibration standard directly into the inlet. If peaks
appear then the problem is not in the GC.
•If the problem is in the GC, refer to the GC’s
documentation for troubleshooting procedures.
•Check the HS sequence log, event log, and status displays
for messages. Especially check the sequence log for
method deviations and dynamic leak check failures.
•Check the vial pressurization gas pressure setting. The
vial pressurization setpoint should not be less than the
pressure developed in the vial during equilibration. (If
not, you will vent sample.)
•Check the delivery gas pressures to the HS. See the Site
Preparation Guide. The gas delivery pressure at the HS
vial gas bulkhead fitting should be 138 kPa (20 psi)
greater than the highest desired vial pressurization
setpoint.
•Enable dynamic leak checking. This feature verifies that
each sample vial is leak- free.
•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.
•Confirm the six port valve is turning.
•Check for leaks in the HS.
•Check for leaks in the transfer line to the GC inlet,
including the connection to the inlet.
•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).

18 Agilent 7697A Troubleshooting
2Chromatographic Symptoms
•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.

Chromatographic Symptoms 2
Agilent 7697A Troubleshooting 19
Retention Times Not Repeatable
•Check the GC. See the GC’s troubleshooting information.
GC problems can include:
•Leaks in the inlet, including septum
•Leaks around the inlet liner, if applicable
•Gas supply pressure
•Wrong liner type used, if applicable
•First run effects (has the GC stabilized?)
•Check the HS sequence log, event log, and status displays
for messages. Especially check the sequence log for
method deviations and dynamic leak check failures.
•If using HS carrier gas control, confirm that the current
HS column configuration matches the column actually
installed in the GC.
•Check for leaks in the transfer line to the GC inlet,
including the connection to the inlet.
•Check for leaks in the other parts of the sampling system
(probe, six port valve, and lines and fittings between).
•Enable dynamic leak checking. This feature verifies that
each sample vial is leak- free.
•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.

20 Agilent 7697A Troubleshooting
2Chromatographic Symptoms
Peak Areas Not Repeatable
Poor area count reproducibility results from changes in the
amount of sample reaching the GC detector. Check these
general areas:
•Check for inconsistent sample preparation technique,
including vial cap seals.
•Check the GC.
•If possible, mount an automatic liquid sampler (ALS)
over the inlet and inject a sequence of internal or
calibration standard directly into the inlet. Check the
area count reproducibility. If acceptable, check the HS.
If unacceptable, the problem is in the GC.
•If the problem is in the GC, refer to the GC’s
documentation for troubleshooting procedures.
•Check sample vial size. (The HS cannot distinguish
between 20- mL and 22- mL vials.)
•Check the HS sequence log, event log, and status displays
for messages. Especially check the sequence log for
method deviations and dynamic leak check failures.
•Run replicates of known standards to verify the problem.
•Enable dynamic leak checking. This feature verifies that
each sample vial is leak- free.
•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.
•Poor choice of equilibration temperature or time. For the
best reproducibility, the analytes in the sample and in the
headspace of the vial must reach static equilibrium.
Increase the equilibration time and/or increase the
equilibration temperature.
•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.