Agilent 7697A Troubleshoting

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Agilent 7697A

Headspace Sampler

Troubleshooting

Agilent Technologies
Notices
© Agilent Technologies, Inc. 2012 Warranty Safety Notices
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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

4 Leaks
Leak Check General Procedure 34
Flow Paths 36

Agilent 7697A Troubleshooting 3


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

4 Agilent 7697A Troubleshooting


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

Agilent 7697A Troubleshooting 5


6 Agilent 7697A Troubleshooting
Agilent 7697A Headspace Sampler
Troubleshooting

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.

Agilent Technologies 7
1 Concepts 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:
1 Observe the symptoms of the problem.
2 Check 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.
3 Consider what may have changed recently. See “What
Changed?”.
4 Consider whether the symptom can be caused by the GC.
5 Look up the symptoms in this manual using the table of
contents or the search tool. Review the list of possible
causes of the symptom.
6 Check 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.

8 Agilent 7697A Troubleshooting


Concepts and General Tasks 1

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 9


1 Concepts 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).

10 Agilent 7697A Troubleshooting


Concepts and General Tasks 1

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:
1 Press [Config].
2 Scroll to Loop Volume (mL).

Gas configuration

WA R N I N G 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.

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:
1 Press [Config].
2 Scroll 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.

Agilent 7697A Troubleshooting 11


1 Concepts 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.

12 Agilent 7697A Troubleshooting


Concepts and General Tasks 1

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).

Agilent 7697A Troubleshooting 13


1 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.

14 Agilent 7697A Troubleshooting


Agilent 7697A Headspace Sampler
Troubleshooting

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.

Agilent Technologies 15
2 Chromatographic 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.

16 Agilent 7697A Troubleshooting


Chromatographic Symptoms 2

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).

Agilent 7697A Troubleshooting 17


2 Chromatographic 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.

18 Agilent 7697A Troubleshooting


Chromatographic Symptoms 2

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.

Agilent 7697A Troubleshooting 19


2 Chromatographic 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.

20 Agilent 7697A Troubleshooting


Chromatographic Symptoms 2

Low Peak Area or Height (Low Sensitivity)


• Check gas supply purity.
• Check all trap indicators and dates.
• 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
sensitivity. 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 configured sample loop size. If incorrect, the
peak areas may be reduced due to insufficient headspace
pressure for filling a bigger sample loop than configured.
• 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 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 21


2 Chromatographic Symptoms

Contamination or Carryover
Carryover results when sample condenses on the flow path
or is trapped in any unswept areas of the flow path.
Normally, the HS reduces the possibility of carryover by
purging the sampling system between injections using with a
high flow rate of vial pressurization gas.
If your output has contamination or unexpected peaks:
1 Check for contamination in the lab air or on the sample
vials.
• Use new, clean vials, caps, and septa.
• Purge a vial with pure nitrogen or argon, then run a
standard.
• Consider the sample preparation process.
2 Check gas supplies. Check gas traps.
3 Check the GC.
• Check GC split vent trap (as applicable).
• Check the GC inlet flows. Verify there is enough
septum purge flow to sweep the inlet weldment.
• Check GC consumables. For example, When were the
inlet liner and septum last changed?
• If possible, mount an automatic liquid sampler (ALS)
over the inlet and inject a sequence of air blanks or
solvent blanks. (Use fresh solvent from a clean source.)
If the carryover disappears, check the headspace
sampler and original solvent source.
• If the problem is in the GC, perform GC maintenance
as needed (bakeout, inlet or detector maintenance,
column maintenance, and so forth). Refer to the GC’s
documentation.
4 Check the HS.
5 Is the HS due for routine maintenance?
• Run a series of solvent blanks. Use fresh solvent from
a clean source. 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).

22 Agilent 7697A Troubleshooting


Chromatographic Symptoms 2

• For systems that have been exposed to long periods of


use with aggressive samples, consider whether the flow
path has been compromised. Replace flow path parts
as needed.
6 Check the transfer line connection to the GC inlet. Verify
the interface is hot. If using a split/splitless (or
multimode) inlet on an Agilent 7890A GC, try installing a
side inlet weldment accessory, G4556- 67070. This
accessory reduces unswept volume, allows easy ALS use
on the GC inlet, and reduces the chance for sample
condensation with at the transfer line to GC interface.
7 Check the reducer union where the transfer line connects
to the six port valve.
8 Check the HS sequence log, event log, and status displays
for messages. Especially check the sequence log for
method deviations related to vial pressure and purge flow.
9 Check HS method parameters.
• Check the purge flow and the standby flow. Try
increasing the purge flow (between sample vials) to
further eliminate residual sample in the sample loop,
probe, and related flow path. Try increasing the purge
hold time. Make sure that standby flow is enabled to
prevent contaminants from condensing in the sampling
system during periods of inactivity.
• Check the oven, loop/valve, and transfer line
temperature setpoints. The setpoints must be high
enough to keep the analytes volatile.
• Check the vial pressurization pressure and time.
10 After running the HS solvent blanks, if the carryover
decreases by a factor of 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 23


2 Chromatographic Symptoms

24 Agilent 7697A Troubleshooting


Agilent 7697A Headspace Sampler
Troubleshooting

3
Log Entries and Errors
Sequence Log Entries 26
Event Log Entries (Errors) 28
Maintenance Log Entries 30
Tray Error Messages 31

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
sequence log resets at the start of each new sequence, it
contains information very useful for troubleshooting
chromatographic issues.
The Maintenance log contains records of user- performed
maintenance tasks.

Agilent Technologies 25
3 Log Entries and Errors

Sequence Log Entries


The sequence log contains entries related to the running or
completed sequence. The log contains up to 256 records. If
at capacity, any new entries overwrite the oldest ones.
Many entries simply log routine sequence events, such as
starting and stopping. Others indicate potential problems.
See Table 1.
See also “Vial Handling” and “Pressures and Flows”.

Table 1 Sequence Log entries and descriptions

Message Description
Start Sequence
Stop Sequence
Pause Sequence
Resume Sequence
Active Method Change The active method in the HS changed. This happens frequently during a sequence.
(It does not indicate changes to saved methods.)
Instrument ready
Instrument not ready
Setpoint changed A method setpoint was changed during the sequence.
Chiller temp out of range, 0C The chiller temperature went out of the expected temperature range.
Vial # skipped The indicated vial was skipped. Look for other messages.
Vial # continue The indicated vial was processed with some issue, in accordance with the method’s
sequence actions. Look for other messages.
Vial # not found The indicated vial was missing.
Vial # wrong vial size The method specified a different vial size than the one detected.
Vial # barcode read error The barcode for vial # was not decoded.
Vial # barcode mismatch The barcode for vial # was decoded but the decoded string did not match the
expected string.
Vial # barcode chksum error The barcode for vial # was decoded but the checksum character did not match the
checksum calculated for the decoded string.
Vial # external not ready 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

26 Agilent 7697A Troubleshooting


Log Entries and Errors 3

Table 1 Sequence Log entries and descriptions (continued)

Message Description
Vial injection
Vial pressurization, x.xxx psi
Vial extraction, x.xxx psi
Vial temperature, x.xxx
Vial # missing spacer 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 27


3 Log Entries and Errors

Event Log Entries (Errors)


The event log records HS events that are not specifically
related to sequence processing. These events include errors
and instrument faults that are also shown on the HS display.
The log contains up to 250 records. If at capacity, any new
entries overwrite the oldest ones. The log remains until
specifically cleared.
The table below lists selected event log entries and errors.
For errors not listed, try power cycling the HS.

Table 2 Event log entries and descriptions

Message Description
7697 power on successful Normal.
7697 power on with exceptions See any exception message descriptions.
7697 power on with warnings See any warning message descriptions.
Vial pressure shut down See Pressures and Flows.
Vial flow shut down See Pressures and Flows.
Carrier pressure shut down See Pressures and Flows.
Carrier flow shut down See Pressures and Flows.
Firmware updated: XX.XX The firmware was updated to the given version.
Tray Error # See Table 5.
Tray Rail move failed.
Tray Error # See Table 5.
Tray Gantry move failed.
Tray Error # See Table 5.
Tray z-axis move failed.
Tray Error # See Table 5.
Tray gripper move failed.
Reset to factory defaults The active method and configuration have been reset to factory defaults.
Needle lifter error # # See Tray Error Messages.
Tray lifter error # # See Tray Error Messages.
Carousel error # See Tray Error Messages.
Shutter error # # See Tray Error Messages.
Six port valve error # # See Tray Error Messages.

28 Agilent 7697A Troubleshooting


Log Entries and Errors 3

Table 2 Event log entries and descriptions (continued)

Message Description
Spacer missing from carousel 12 Vial model only. Check for a missing vial spacer in the carousel. Check for
contamination that can cause a spacer to stick to a vial.
BCR read error # #, t = # The barcode reader failed to decode the barcode in time, t, seconds. Check the
barcode label, See the Operation Guide and Barcode Reader Errors.

Agilent 7697A Troubleshooting 29


3 Log Entries and Errors

Maintenance Log Entries


The maintenance log records maintenance operations
performed and logged by the user. The log contains up to
128 records. If at capacity, any new entries overwrite the
oldest ones. The log remains until specifically cleared.
The HS always logs messages such as leak test results and
firmware updates. However, “serviced” and “service due”
messages are logged only when using the Early Maintenance
Feedback (EMF) features of the instrument. (See the
Advanced Operation guide.) When the user resets a resource
counter, the HS assumes that maintenance has been
performed.

Table 3 Event log entries and descriptions

Message Description
<Component> serviced Indicates that the counter was reset for the indicated component.
Firmware updated: x.xx.xx Indicates an the instrument firmware update to the revision shown.
<Component> due, or The EMF counter for the indicated component has been reached.
<Component> service due
Tray calibrated 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.

30 Agilent 7697A Troubleshooting


Log Entries and Errors 3

Tray Error Messages


Table 4 summarizes the error messages related to the 111
vial tray hardware. These types of errors can occur when the
carousel or lifters cannot move as desired, for example,
when debris from a broken vial obstructs carousel or lifter
movement.

Table 4 Tray error messages

Event Log Error Comments


Carousel error # 1 Check for obstructions in the carousel and
oven.
2 Power cycle the HS.
3 Contact Agilent for service.
Needle lifter error # 1 Check for obstructions in the carousel and
oven.
2 Power cycle the HS.
3 Contact Agilent for service.
Shutter error # 1 Check for obstructions near the shutter.
2 Power cycle the HS.
3 Contact Agilent for service.
Six port valve error # See Six Port Valve Errors.
Tray lifter error # 1 Check for obstructions in the carousel and
oven.
2 Check for obstructions near the shutter.
3 Power cycle the HS.
4 Contact Agilent for service.

Table 5 lists selected tray and barcode reader errors that


can occur during method execution.

Table 5 Tray error codes and messages

Error Number Event Log Number Description


103 Vial in gripper The vial sensor senses a vial in the gripper when no vial is expected. See
No Vial Found in Gripper/Vial In Gripper.
104 No vial in gripper 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.
105 Received abort The stop key was pressed on the instrument while the tray was
executing a command. The command was aborted.

Agilent 7697A Troubleshooting 31


3 Log Entries and Errors

Table 5 Tray error codes and messages (continued)

Error Number Event Log Number Description


180 Bad barcode label The barcode label does not have enough white space before the first
line. See the Operating guide and Barcode Reader Errors.
181 Bad barcode label The method calls for a checksum on the barcode label and there is none
checksum or the label was not decoded correctly. See the Operating guide and
Barcode Reader Errors.
182 Failed to decode The barcode label could not be read. See the Operating guide and
barcode Barcode Reader Errors.
183 Barcode code label not No barcode label was detected. See the Operating guide and Barcode
found Reader Errors.
301 Tray parked The tray is in the park position and cannot execute a move command.
302 Tray rack not found The rack sensor for a given rack location indicates there is no rack
present. Check rack installation. Check sequence vial locations.
304 Vial not found No vial was detected at the source location during a move operation.
Check sequence vials locations. Were vials loaded correctly? Check
sequence locations against vial placement in the tray.
305 Vial left in gripper After a move operation completed the vial sensor still reports a vial in
the gripper.
312 Z-axis stalled Check for any obstructions to tray movement.
313 Gripper stalled Check for any obstructions to tray movement.
314 Rail axis move timed Check for any obstructions to tray movement.
out
315 Gantry axis move timed Check for any obstructions to tray movement.
out
316 Z-axis move timed out Check for any obstructions to tray movement.
317 Gripper move timed out Check for any obstructions to tray movement.
330 Rail home failed Check for any obstructions to tray movement. The rail axis homing
routine failed.
331 Gantry home failed Check for any obstructions to tray movement.
332 Z-axis home failed Check for any obstructions to tray movement.
333 Gripper home failed Check for any obstructions to gripper movement.
334 Gripper open failed Check for any obstructions to gripper movement.
335 Gripper close failed Check for any obstructions to gripper movement.

32 Agilent 7697A Troubleshooting


Agilent 7697A Headspace Sampler
Troubleshooting

4
Leaks
Leak Check General Procedure 34
Flow Paths 36
Checking for External Leaks 38
To Run the Restriction and Pressure Decay Test 40
To Run the Cross Port Leak Test 53
To Check for Leaks in the Transfer Line 58

This section discusses leak testing in the headspace sampler


(HS). Chromatographic symptoms such as loss of sensitivity
can result from leaks and restrictions. Use the following set
of tests for verifying leaks and restrictions within the HS.
Verify that the GC is leak free before checking for leaks
within the HS.

Agilent Technologies 33
4 Leaks

Leak Check General Procedure


When checking for leaks, consider the system in three parts:
external leak points, GC leak points, and HS leak points.
• External leak points include the gas cylinder (or gas
purifier), the regulator and its fittings, the supply shutoff
valves, and the connections to the HS and GC supply
fittings.
• For GC leak points, refer to the GC user documentation.
• HS leak points include the connections at the six port
valve (sample loop and transfer line), the transfer line
connection to the GC inlet, and the connections for the
sampling probe.

WA R N I N G Hydrogen (H2) is flammable and is an explosion hazard when


mixed with air in an enclosed space (for example, a flow meter).
Purge flow meters with inert gas as needed. Always measure
gases individually.

WA R N I N G Hazardous sample may be present.

1 Gather the following:


• Electronic leak detector capable of detecting the gas
type (Agilent part number G3388A).
• 7/16- inch, 9/16- inch, and 1/4- inch wrenches for
tightening Swagelok and column fittings.
• Leak test kit, Agilent part number G4556- 67010.
Includes: no hole ferrule, 11 mm low bleed septa,
headspace (blue) leak test vial, 1/8- in. nylon tube
fitting plug, 1/16- in. stainless steel ZDV plug (six port
valve cap).
2 Check any potential leak points associated with any
recent maintenance.
3 Check for external leaks. See “Checking for External
Leaks”.
4 Check the GC for leaks. See the GC user documentation.

34 Agilent 7697A Troubleshooting


Leaks 4

5 Check HS fittings and connections that undergo thermal


cycling, since thermal cycling tends to loosen some fitting
types. Use the electronic leak detector to determine if a
fitting is leaking.
• Start by checking any newly made connections first.
• Remember to check connections in the gas supply lines
after changing traps or supply cylinders.
6 Run the HS Restriction & pressure decay test. See To Run the
Restriction and Pressure Decay Test.
7 Run the HS Cross port leak test. See To Run the Cross Port
Leak Test.

Agilent 7697A Troubleshooting 35


4 Leaks

Flow Paths
Figure 1 and Figure 2 below show the flow paths within the
headspace sampler (HS).

PS - Pressure sensor
Vial pressurization gas FS - Flow sensor
SV - Switching valve
Vent Carrier gas PV - Proportional valve

Flow control module

SV2 PS

PV1
FS

PS
SV1

PV2

Six port valve

4
3

Sample loop 5
Transfer line 2

1 6

Figure 1 HS flow paths (standard installation)

36 Agilent 7697A Troubleshooting


Leaks 4

Vial pressurization
gas HS carrier control module
Vent Carrier gas

PV1
FS
Flow control module
PS

PV1
FS

PS

SV1

PV2

Six port valve

4
3
PS - Pressure sensor
Sample loop 5
Transfer 2 FS - Flow sensor
line SV - Switching valve
1 6 PV - Proportional valve

Figure 2 HS flow paths with optional G4562A 7697A Carrier Gas EPC
Module Accessory installed

Agilent 7697A Troubleshooting 37


4 Leaks

Checking for External Leaks


Figure 3 below shows typical external leak points to check.
Check all fittings and correct as needed.

Figure 3 External leak points (HC configured with GC carrier gas


control, with optional valves and fittings shown)

• Gas supply bulkhead fittings


• Gas cylinder fittings
• Regulator fittings
• Traps
• Shut- off valves (if installed, not included in ship kit)
• Unions and tee fittings (if installed, not included in ship
kit)
• Transfer line connection to the GC
Perform a pressure drop test.

CAUTION A pressure decay test cuts off carrier flow through the HS and GC.
To prevent damage to the flow path components (column, inlet liner,
and so forth), cool the HS and GC before beginning.

38 Agilent 7697A Troubleshooting


Leaks 4

1 Cool the HS sample loop, transfer line, and GC inlet and


column oven to prevent damage during the test.
2 Turn off the HS.
3 Set the regulator pressure to 415 kPa (60 psi).
4 Fully turn the regulator pressure adjustment knob
counterclockwise to shut the valve.
5 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 39


4 Leaks

To Run the Restriction and Pressure Decay Test


The built- in restriction and pressure decay test sequentially
checks for restrictions and leaks in the sampling system. The
test checks for:
• Restrictions in the sample probe
• Restrictions in the vent line
• Leaks around the sample probe
• Leaks around the sample loop
• Leaks in valves and in the six port valve
The test consists of several parts. If one part fails, the test
reports the failure and stops before attempting any
subsequent parts. Correct the problem, then re- run the test.
Continue correcting problems and retesting until the test
completes successfully.
Before running the built- in restriction and pressure decay
test, check the GC for leaks. See “Leak Check General
Procedure” and the GC user documentation.
1 Gather the following:
• Leak test kit (G4556- 67010). Includes: six port valve
cap (G6600- 80039), no hole ferrule (5181- 7458), blue
leak test vial (G4556- 20600), 1/8- inch Nylon Swagelok
plug (0100- 2414)
• GC liner, O- ring, and septum as needed
• 3/16- inch wrench
• 7/16- inch wrench
• 1/4- inch wrench
• 5/16- inch wrench
2 If unsure of the quality of the GC inlet septum, liner, and
liner O- ring, change them now. Refer to the GC user
documentation for details.
3 Set the active method vial size to 20 mL. Press [Vial],
scroll to Vial size, press [Mode/Type] to select the vial size
from a list, then press [Enter].
4 Install a new septum into the blue leak test vial.
5 Place the blue leak test vial into priority position 1 (111
vial model) or into tray position 1 (12 vial model).

40 Agilent 7697A Troubleshooting


Leaks 4

5
1

4
3
1
2

G4556A G4557A

6 Set the carrier pressure to a low value.

If using HS Control or GC Control:


a Cool the GC inlet and column oven.
b When cool, press [Carrier].
c Set the carrier pressure setpoint to 14 kPa (2 psi). (If
in a flow mode, reduce the flow setpoint until the
carrier pressure is below 14 kPa (2 psi).)
If using GC + HS Control:
• Press [Carrier], then reduce the flow setpoint until the
carrier pressure is below 14 kPa (2 psi).
• Leave the GC carrier pressure or flow unchanged.
7 Start the test. Press [Service Mode], select Restriction &
pressure decay, then press [Enter].
The test begins.
8 The test displays information for the current action (for
example, “Purging,” “Zeroing Pressure Sensor,” or “Moving
Test Vial,” and the pressure and flow readings).
See “If the test passes” or “If the test fails”.
9 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 41


4 Leaks

• If not already done, check the GC. The HS leak test


cannot test for leaks in the GC.

If the test fails


If the test fails, the display provides:
• The reading for the stage that failed (for example, leak
rate or flow rate).
• Command lines to toggle related valves (for example, a
switching valve or the six port valve).
SV1 or SV2 or PV1 or PV2: Scroll to this line and press
[On/Yes] to turn on (energize) the valve, or [Off/No] to
turn it off.
Six-port valve: Scroll to this line and press [On/Yes] to
switch the valve to the load position, or [Off/No] to switch
it to the inject position.
• 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.

42 Agilent 7697A Troubleshooting


Leaks 4

Needle (Sample Probe) restriction test, stage 1: Vent CLOSED


(INJECT)
During this stage, the HS flow paths are as shown in
Figure 4:

Vial pressurization PS - Pressure sensor


gas
FS - Flow sensor
Vent Carrier gas SV - Switching valve
PV - Proportional valve

Flow control module

SV2 PS

PV1
FS

PS

SV1

PV2

Six port valve

4
3
5
Transfer Sample loop 2
line
1 6
40 mL/min

Figure 4 Flow paths: Needle restriction test, stage 1: Vent CLOSED


(INJECT)

Agilent 7697A Troubleshooting 43


4 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

44 Agilent 7697A Troubleshooting


Leaks 4

Needle (Sample Probe) restriction test, stage 2: Vent CLOSED


(STANDBY)
During this stage, the HS flow paths are as shown in
Figure 5:

Vial pressurization PS - Pressure sensor


gas
FS - Flow sensor
Vent Carrier gas SV - Switching valve
PV - Proportional valve

Flow control module

SV2 PS

PV1
FS

PS

SV1

PV2

Six port valve

4
3
5
Transfer Sample loop 2
line
1 6

40 mL/min

Figure 5 Flow paths: Needle (Sample Probe) restriction test, stage 2:


Vent CLOSED (STANDBY)

Agilent 7697A Troubleshooting 45


4 Leaks

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

46 Agilent 7697A Troubleshooting


Leaks 4

Needle (Sample Probe) restriction test, stage 3: Vent OPEN


During this stage, the HS flow paths are as shown in
Figure 6:

Vial pressurization PS - Pressure sensor


gas
FS - Flow sensor
Vent Carrier gas SV - Switching valve
PV - Proportional valve

Flow control module

SV2 PS

40 mL/min
PV1
FS

PS

SV1

PV2

6 port valve

4
3
5
Transfer 2
line
1 6

Figure 6 Flow paths: Needle (Sample Probe) restriction test, stage 3:


Vent OPEN

Agilent 7697A Troubleshooting 47


4 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)

48 Agilent 7697A Troubleshooting


Leaks 4

Vial leak test, stage 1: Test up to SV1


During this stage, the HS flow paths are as shown in
Figure 7:

Vial pressurization PS - Pressure sensor


gas
FS - Flow sensor
Vent Carrier gas SV - Switching valve
PV - Proportional valve

Flow control module

SV2 PS

PV1
FS

PS

SV1

PV2

Six port valve

4
3

Sample loop 5
Transfer 2
line
1 6

Figure 7 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 49


4 Leaks

Vial leak test, stage 2: Test 6PORT (STANDBY)


During this stage, the HS flow paths are as shown in
Figure 8:

Vial pressurization PS - Pressure sensor


gas FS - Flow sensor
Vent Carrier gas SV - Switching valve
PV - Proportional valve

Flow control module

SV2 PS

PV1
FS

PS

SV1

PV2

Six port valve

4
3
5
Transfer Sample loop 2
line
1 6

Figure 8 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.

50 Agilent 7697A Troubleshooting


Leaks 4

• 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 51


4 Leaks

Vial leak test, stage 3: Test 6PORT (INJECT)


During this stage, the HS flow paths are as shown in
Figure 9:

Vial pressurization PS - Pressure sensor


gas
FS - Flow sensor
Vent Carrier gas SV - Switching valve
PV - Proportional valve

Flow control module

SV2 PS

PV1
FS

PS

SV1

PV2

Six port valve

4
3
5
Transfer Sample loop 2
line
1 6

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

52 Agilent 7697A Troubleshooting


Leaks 4

To Run the Cross Port Leak Test


Run cross port leak test immediately after the HS passes the
restriction and pressure decay test. See “To Run the
Restriction and Pressure Decay Test”. These instructions
assume that the HS is already prepared and that the GC is
leak- free.
The built- in cross port leak test sequentially checks for leaks
across the six port valve, from the carrier side to the vial
pressurization side.
The test consists of two parts. If one part fails, the test
reports the failure and stops before attempting any
subsequent parts. Correct the problem, then re- run the test.
Continue correcting problems and retesting until the test
completes successfully.
1 Install a new septum into the blue leak test vial.
2 Place the blue leak test vial into priority position 1 (111
vial model) or into tray position 1 (12 vial model).

2
7

1
4

3
1
2

G4556A G4557A

3 Set the carrier pressure to 172 kPa (25 psi).

If using GC + HS Control:
• Press [Carrier], then increase the flow setpoint until the
carrier pressure is 172 kPa (25 psi).
• Leave the GC carrier pressure or flow unchanged.
4 Start the test. Press [Service Mode], select Cross port leak
test, then press [Enter].
The test begins.

Agilent 7697A Troubleshooting 53


4 Leaks

The test displays information for the current stage, for


example, the flow path being tested and the setpoint and
actual pressure or flow readings.
To stop the test, press [Clear] during a purge step
(monitor the HS display). Otherwise, the test continues
until it passes or fails.
See “If the test passes” or “If the test fails”.
5 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.
• If not already done, check the GC. The HS leak test
cannot test for leaks in the GC.

If the test fails


If the test fails, the display provides:
• The reading for the stage that failed (for example, leak
rate or flow rate).
• Command lines to toggle related valves (for example, a
switching valve or the six port valve).
SV1 or SV2 or PV1 or PV2: Scroll to this line and press
[On/Yes] to turn on (energize) the valve, or [Off/No] to
turn it off.
Six-port valve: Scroll to this line and press [On/Yes] to
switch the valve to the load position, or [Off/No] to switch
it to the inject position.
• 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.

54 Agilent 7697A Troubleshooting


Leaks 4

Cross port leak test, stage 1: Test 6PORT (STANDBY)


During this stage, the HS flow paths are as shown in
Figure 10:

Vial pressurization PS - Pressure sensor


gas FS - Flow sensor
SV - Switching valve
Vent Carrier gas PV - Proportional valve

Flow control module

SV2 PS

PV1
FS

PS

SV1

PV2

Six port valve

4
3
5
Transfer Sample loop 2
line
1 6

Figure 10 Flow paths: Cross port leak test, stage 1: Test 6PORT
(STANDBY)

Agilent 7697A Troubleshooting 55


4 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.

56 Agilent 7697A Troubleshooting


Leaks 4

Cross port leak test, stage 2: Test 6PORT (INJECT)


During this stage, the HS flow paths are as shown in
Figure 11:

Vial pressurization PS - Pressure sensor


gas FS - Flow sensor
Vent Carrier gas SV - Switching valve
PV - Proportional valve

Flow control module

SV2 PS

PV1
FS

PS

SV1

PV2

Six port valve

4
3
5
Transfer Sample loop 2
line
1 6

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 57


4 Leaks

To Check for Leaks in the Transfer Line


• Check for leaks at the six port valve and interface
connection to the 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).

58 Agilent 7697A Troubleshooting


Agilent 7697A Headspace Sampler
Troubleshooting

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

This section describes vial handling issues and how to


resolve them.

Agilent Technologies 59
5 Vial Handling

How the Headspace Sampler Handles Vials


How the HS handles vials is important for understanding
error messages and entries made in the sequence log and
event logs.
In the 12 vial model, the tray (carousel) rotates for loading
samples and when moving sample vials into position. The
sample probe lifter raises and lowers the current vial into
the single- vial oven, and to and from the sampling probe.
In the 111 vial model, the tray resides on top of the unit.
To move a sample vial, the HS uses the gantry, z- axis
assembly, gripper assembly and gripper, shutter, and vial
lifters. See Figure 12.
• The gantry, z- axis assembly, gripper assembly and gripper
are used to move sample vials to and from the barcode
reader and to and from the tray lifter.
• The shutter opens and closes when the HS transfers a vial
to and from the vial oven.
• 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

60 Agilent 7697A Troubleshooting


Vial Handling 5

No Vial Found in Gripper/Vial In Gripper


The headspace sampler tray did not find a vial where it
expected to find it, or the vial did not leave the gripper as
expected. The HS logs the deviation, then follows the
method’s sequence action parameters.
To resolve the problem, do the following:
• Check the HS sequence log, event log, and status displays
for messages. (Was this error caused by another problem?)
• Check all vials. Were they loaded into the tray correctly?
• If running a priority sample, was the vial placed into the
correct location?
• Check vial rack installation.
• Check vial size configuration.
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 61


5 Vial Handling

Vial Size Errors


The HS checks vial height:
• When loading a vial onto the sampling probe (12 vial
model)
• When grasping a vial with the gripper (111 vial model)
If the vial height does not match the expected value for the
vial size defined in the method, a vial size error is logged.
The HS proceeds in accordance with the defined sequence
action for vial size.
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.)

62 Agilent 7697A Troubleshooting


Vial Handling 5

Carousel Errors
A carousel error indicates that the carousel could not
function properly. For a 12 vial model, this is the vial tray.
For the 111 vial model, the carousel resides in the vial oven.
Possible causes include:
• Broken vial in the oven
• Obstruction in the shutter. (111 vial model)
• Other obstruction in the oven
• Carousel stepper motor issue
• Belt issue
Before proceeding, cool down the vial oven (111 vial model)

WA R N I N G The oven and contents in it may be hot enough to cause burns.


Cool the oven to a safe handling temperature before proceeding,
or wear heat-resistant gloves.

WA R N I N G If there is a broken vial in the oven, the oven will contain sharp,
broken glass as well the contents of any sample material.

• Check the HS sequence log, event log, and status displays


for messages. (Was this error caused by another problem?)
• 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 or vial oven in the Maintenance manual.
• If the problem remains, contact Agilent for service.

Agilent 7697A Troubleshooting 63


5 Vial Handling

Sample Probe Lifter Errors


The sample probe lifter raises the sample vial onto the
sampling probe and lowers it back into the rotating tray. A
sample probe lifter error indicates that the lifter could not
function properly.
• Check the HS sequence log, event log, and status displays
for messages. (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 or vial oven in the Maintenance manual.
• Check vial size configuration.
• Contact Agilent for service.

64 Agilent 7697A Troubleshooting


Vial Handling 5

Six Port Valve Errors


The six port valve rotates during the sampling cycle. If the
valve cannot rotate, power cycle the 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 65


5 Vial Handling

Shutter Errors (111 Vial Model)


The shutter opens and closes when transferring a vial to and
from the vial oven.
• 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.

66 Agilent 7697A Troubleshooting


Vial Handling 5

Tray Lifter Errors (111 Vial Model)


The tray lifter transfers the sample vial between the shutter
and the carousel. A tray lifter error indicates that the lifter
could not function properly.
• Check the HS sequence log, event log, and status displays
for messages. (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 or vial oven in the Maintenance manual.
• Contact Agilent for service.

Agilent 7697A Troubleshooting 67


5 Vial Handling

Barcode Reader Errors


If using the optional barcode reader, a barcode error
indicates that the barcode reader could not read the barcode
as expected.
• Check the vial barcode label positioning, sizing, and type.
See the Operating guide.
• Barcode label not heat resistant.
• Check vial locations. Was this vial the correct vial?
• Check the barcode label. Is the label smudged or illegible?
Is the label too glossy? If possible, try reading the
barcode using another device.
• Check the HS sequence log, event log, and status displays
for messages.
• Check the method. Does the barcode type specified in the
method match the barcode applied to the vial?
• 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.

68 Agilent 7697A Troubleshooting


Vial Handling 5

Tray Errors (111 Vial Model)


A tray error indicates that the HS tray did not operate
properly, typically during a move.
• 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 69


5 Vial Handling

Gripper Errors (111 Vial Model)


A gripper error indicates that the gripper could not properly
lift or release a vial.
• 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.

70 Agilent 7697A Troubleshooting


Vial Handling 5

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 71


5 Vial Handling

72 Agilent 7697A Troubleshooting


Agilent 7697A Headspace Sampler
Troubleshooting

6
Pressures and Flows
Flow and Pressure Shutdowns 74
Purge Flow Deviations 75
Vial Pressurization Setpoint Deviations 76
Carrier Gas Deviation or Shutdown 77
To resolve a carrier flow deviation or shutdown 78

This section describes issues related to pressures and flows


within the headspace sampler, and how to resolve them.

Agilent Technologies 73
6 Pressures and Flows

Flow and Pressure Shutdowns


The HS monitors the vial pressurization gas stream. If the
optional G4562A Carrier Gas EPC module is installed and
enabled for use, the HS also monitors the carrier gas flow. If
a gas is unable to reach its flow or pressure setpoint, the HS
assumes that a leak exists. It will warn you with a beep
after 25 seconds, and it will continue to beep in intervals.
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.

74 Agilent 7697A Troubleshooting


Pressures and Flows 6

Purge Flow Deviations


If the HS cannot maintain the correct purge flow after an
injection, it logs the method deviation into the sequence log.
• 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 75


6 Pressures and Flows

Vial Pressurization Setpoint Deviations


If the HS cannot pressurize the vial to the method setpoint,
it logs the method deviation into the sequence log.
• Check the gas supplies.
• 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.
• Check the sequence log for a dynamic leak check failure
entry for this vial.
• Check the method vial pressure setpoint. If the method
setpoint is higher than the safety feature for the vial cap,
the vial cap may be releasing the excess pressure.
• Check for leaks.
• 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.

76 Agilent 7697A Troubleshooting


Pressures and Flows 6

Carrier Gas Deviation or Shutdown


The HS, if equipped with the optional G4562A Carrier Gas
EPC Module Accessory, can control carrier gas flow or
pressure in one of two modes. The HS provides either all
carrier gas flow into the GC, or an added flow during the
injection cycle (in this mode, the GC still provides its own
carrier gas control).

HS provides all carrier flow


If the HS cannot maintain carrier gas flow or pressure at
setpoint, the HS will do the following:
• Log a deviation in the sequence log.
• Display a flow or pressure shutdown message.
• Turn off the flow to avoid column damage.
• Turn off the transfer line.
The HS will continue to process sequence vials through
thermal equilibration. While in shutdown, it will not perform
injections. The HS will log deviations for any vial which
exceeds setpoint for equilibration.
However, the GC may continue to operate, depending on the
model and the type of carrier gas control used.

CAUTION If the HS is the primary source for carrier flow, and if the HS shuts
down the carrier flow, cool the GC oven to protect the column. The
HS cannot control the GC.

HS provides additional flow during the injection


If the HS cannot achieve and maintain either the added flow
during injection or the carrier saver flow after the injection,
the HS will log the deviations and may enter shutdown.
• The HS will always log a deviation in the sequence log.
• If the flow does not reach setpoint after about 5 minutes,
the HS displays a flow or pressure shutdown message.
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 77


6 Pressures and Flows

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?

78 Agilent 7697A Troubleshooting


Agilent 7697A Headspace Sampler
Troubleshooting

7
Communications
Troubleshooting Headspace Sampler Communications 80
To Troubleshoot LAN Connectivity Issues 81
The GC Does Not Start After the HS Injects 85

This section provides basic communications troubleshooting


for the Agilent 7697A Headspace Sampler.

Agilent Technologies 79
7 Communications

Troubleshooting Headspace Sampler Communications


The Agilent 7697A Headspace Sampler uses only LAN
communications. This topic provides information and tasks
designed to help resolve problems related to TCP/IP network
communications when controlling the HS using an Agilent
data system. This topic assumes a basic knowledge of
network communications, including the TCP/IP protocol, a
basic understanding of networks and networking, and a basic
understanding of the hardware and functions of networks
(cabling types, hubs, switches, routers, static versus dynamic
IP addresses, DNS servers, subnets, gateways, and so forth).
Network- based communications problems can appear with
any of the following symptoms:
• Cannot connect to an instrument
• Intermittent loss of communications with an instrument
• Sudden loss of communications to an instrument

General information
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.

Using DHCP
While the HS can be set to receive its IP address from a
DHCP server, not all data systems support DHCP. In most
cases, if the data system supports DHCP, then the DHCP
server must be set so that either:
• The HS receives a host name, and only the host name is
used for data system connections, or
• The DHCP server provides a static IP address to the HS.
If using DHCP, and there is a communications problem with
the HS, try setting the IP address directly at the front panel
instead.

80 Agilent 7697A Troubleshooting


Communications 7

To Troubleshoot LAN Connectivity Issues


1 At the HS front panel, show the current communications
options: Press [Options], then select Communications. The
display lists the HS IP address information. Note
especially:
• The number of Connections (devices communicating with
the HS). If the number of connections is greater than
expected, another data system or utility is
communicating with the HS.
• The DHCP setting. See “Using DHCP”.
• Record the HS IP address, subnet mask, and gateway.
2 Determine the IP addresses used in the configuration.
Each computer, printer, and instrument on the network
must have a unique IP address. Duplicated addresses
cause conflicts and disrupted communications. To
determine the current computer IP address:
a Click Start…> Run, then in the Open field type cmd. Click
OK.
b Type Ipconfig /all, then press [Enter]. The command lists
communications settings for all network devices in the
computer.
c Record the IP address, subnet mask, and gateway
settings for the PC.
d Check to make sure that you have the same class IP
address and the associated subnet mask in your
network.
3 Record the IP address, subnet mask, and gateway for the
instruments controlled by the data system.
• 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.
• Also record IP addresses for other local devices, such
as networked printers.
4 Compare the collected IP addresses. Make sure that the IP
addresses entered into the data system match the IP
addresses used for the instruments.
5 Check cables and LAN LEDs at each device. Ensure that
all the network cables are plugged in tightly at both ends.

Agilent 7697A Troubleshooting 81


7 Communications

Check the end in the hub/switch and the one in the


network card of the PC or instrument. When properly
connected and working, network cards provide green and
yellow LEDs as a visual indicator of network connectivity.
Look on the back of the NIC adapter of the PC and the
back of the instrument.
• If there is no green LED, there is no connectivity. Look
for a hardware problem such as a disconnected cable,
dead network, defective switch/hub, router, or defective
NIC.
• If there is a red LED lit, there is a problem with the
NIC.
• If the green LED is lit, with a flashing yellow or orange
LED, the network card is properly connected and
working. This condition indicates an active network,
and verifies that the jack in the wall is working.
Disconnect the network cable and confirm that the
network reports it is disconnected. Re- connect the
network cable and confirm the PC reports the connection.
Power cycle the router.
6 Check your firewall settings and make sure that the
firewall is not blocking the incoming and outgoing traffic.
7 You can test to see if the wall jack is having trouble by
plugging your cable into another jack you know is
working. You can also plug another device with a working
network connection, such as a laptop, into the same jack
as the HS.
8 If you see the error message “Service Control Manager
reported an error” when you logon to Windows, this could
indicate a bad NIC card or corrupt software driver for the
NIC card. If this occurs, check the Windows Event Viewer
program for details.
9 Check if the computer's network card is functioning
properly and that TCP/IP is installed correctly as follows:
a Click Start > Run, then type cmd and click OK.
b Type ping 127.0.0.1 and press [Enter]. You should see four
lines that read something like this “Reply from 127.0.0.1:
bytes=32 time<10ms 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
it.

82 Agilent 7697A Troubleshooting


Communications 7

c You might have to reinstall the NIC adapter and the


software drivers that came with it.
d If you are getting a normal ping response, next ping
your PC IP address. You should see four lines that read
something like this “Reply from 192.176.xxx.xxx: bytes=32
time<10ms TTL=64”. A successful ping means TCP/IP is
installed and correctly initialized. If you are getting
anything else, there is a problem with your TCP/IP
protocol. Remove the TCP/IP protocol that you have in
your network configurations and then reinstall it.

If the ping failed with “Request timed out” errors


1 Check the cabling. (Did the cable become unplugged?)
2 Test the cabling connection by disconnecting and
reconnecting the cabling and check the PC for the
network connection status.
3 Check the hub, switch, or router settings. Make sure the
instrument is not connected to the switch or hub cascade
port. Try a different switch or hub.
4 Power off the hub/switch or router and power it back on
again, then repeat the instrument's ping test. Use a
crossover cable (no switch/hub) to one instrument and
ping again.

If ping succeeds, but you still cannot connect


1 Consider if the network is just very busy. If there is too
much traffic on the network, this can interfere with data
acquisition and instrument control. Monitor the collision
lights on the switch or hub.
2 Verify that the same IP address is used in the instrument
and the data system.

Agilent 7697A Troubleshooting 83


7 Communications

3 If the ping request was answered successfully by the


instrument but you cannot connect to the instrument with
your data system, you need to verify that your Windows
TCP/IP settings (especially the subnet mask and gateway
settings) are correct for the selected network. PING only
checks the hardware levels and not the subnet mask or
gateway. The gateway and subnet mask can be incorrect
and you can PING (receive a reply) the instrument but
not connect to the instrument using a data system.
4 The instrument may be in use by another software
application.
5 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.

84 Agilent 7697A Troubleshooting


Communications 7

The GC Does Not Start After the HS Injects


If the HS makes an injection, but the GC does not start a
run, check the following:
• Headspace sampler multiple headspace extraction mode
for this method. Press [Adv Function] and check the
Extraction Mode. If performing concentrating extractions,
the HS only starts a GC run after the final concentrating
injection.
• APG remote cable connection.
• The HS method APG Remote enable setting. If turned off,
the HS will not wait for GC readiness before injecting.
• 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 85


7 Communications

86 Agilent 7697A Troubleshooting


Agilent 7697A Headspace Sampler
Troubleshooting

8
Electronics
To Check the Headspace Sampler Power Configuration 88
To Perform the Instrument Self Test 89
Thermal Shutdowns 90

This section describes how to resolve issues in the


headspace sampler electronics, including temperature
control.

Agilent Technologies 87
8 Electronics

To Check the Headspace Sampler Power Configuration


The headspace sampler must be properly configured for the
local mains voltage supply. To check the current power
configuration of the HS, read the label shown in the back of
the instrument.

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.

88 Agilent 7697A Troubleshooting


Electronics 8

To Perform the Instrument Self Test


The instrument performs its self- test during startup.
1 Turn off the instrument.
2 Wait approximately 1 minute, then turn on the
instrument. If the main status appears in the display, the
instrument passed self- test.

Agilent 7697A
A.01.01

Power on successful

Agilent 7697A Troubleshooting 89


8 Electronics

Thermal Shutdowns
The headspace sampler controls the temperature for areas
including: the vial oven, the sample loop and valve, and the
transfer line. (If using the optional tray chiller, this is
another controlled zone.) If the heated zone is not within its
allowable temperature range (lower than minimum
temperature or higher than maximum temperature), an error
message displays. Depending on the severity of the problem,
the HS may also shut the zone down to prevent damage or
injury. Several things could cause a thermal shutdown:
• A problem with the electrical supply to the instrument.
• A malfunction of the zone control electronics.
• A shorted or open temperature sensor.
• A shorted or open heater.
To recover from this state:
1 Press [Status] and check for additional messages.
2 Press [Temps]. Look for any additional messages.
3 Scroll to the offending thermal zone, then press [Off/No]
to turn off any audible alarm.
4 Check for any issues that may have caused the problem:
• Missing thermal cover over transfer line and six port
valve
• Missing or damaged insulation on transfer line
• Missing external covers on HS
• Sample valve cover installed over heater/sensor cable
5 Power cycle the HS.
6 If the problem does not resolve, contact Agilent for
service.

90 Agilent 7697A Troubleshooting


Electronics 8

Agilent 7697A Troubleshooting 91


Agilent Technologies

© Agilent Technologies, Inc. 2012

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