Agilent 7697A Troubleshoting
Agilent 7697A Troubleshoting
Agilent 7697A Troubleshoting
Headspace Sampler
Troubleshooting
Agilent Technologies
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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
4 Leaks
Leak Check General Procedure 34
Flow Paths 36
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
7 Communications
Troubleshooting Headspace Sampler Communications 80
General information 80
Using DHCP 80
To Troubleshoot LAN Connectivity Issues 81
8 Electronics
To Check the Headspace Sampler Power Configuration 88
To Perform the Instrument Self Test 89
Thermal Shutdowns 90
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
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.
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.
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).
Gas configuration
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.
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
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.
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).
3
Log Entries and Errors
Sequence Log Entries 26
Event Log Entries (Errors) 28
Maintenance Log Entries 30
Tray Error Messages 31
Agilent Technologies 25
3 Log Entries and Errors
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
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.
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.
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.
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.
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
Agilent Technologies 33
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
SV2 PS
PV1
FS
PS
SV1
PV2
4
3
Sample loop 5
Transfer line 2
1 6
Vial pressurization
gas HS carrier control module
Vent Carrier gas
PV1
FS
Flow control module
PS
PV1
FS
PS
SV1
PV2
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
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.
5
1
4
3
1
2
G4556A G4557A
SV2 PS
PV1
FS
PS
SV1
PV2
4
3
5
Transfer Sample loop 2
line
1 6
40 mL/min
SV2 PS
PV1
FS
PS
SV1
PV2
4
3
5
Transfer Sample loop 2
line
1 6
40 mL/min
SV2 PS
40 mL/min
PV1
FS
PS
SV1
PV2
6 port valve
4
3
5
Transfer 2
line
1 6
SV2 PS
PV1
FS
PS
SV1
PV2
4
3
Sample loop 5
Transfer 2
line
1 6
SV2 PS
PV1
FS
PS
SV1
PV2
4
3
5
Transfer Sample loop 2
line
1 6
Figure 8 Flow paths: Vial leak test, stage 2: Test 6PORT (STANDBY)
SV2 PS
PV1
FS
PS
SV1
PV2
4
3
5
Transfer Sample loop 2
line
1 6
Figure 9 Flow paths: Vial leak test, stage 3: Test 6PORT (INJECT)
2
7
1
4
3
1
2
G4556A G4557A
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.
SV2 PS
PV1
FS
PS
SV1
PV2
4
3
5
Transfer Sample loop 2
line
1 6
Figure 10 Flow paths: Cross port leak test, stage 1: Test 6PORT
(STANDBY)
SV2 PS
PV1
FS
PS
SV1
PV2
4
3
5
Transfer Sample loop 2
line
1 6
Figure 11 Flow paths: Cross port leak test, stage 2: Test 6PORT (INJECT)
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
Agilent Technologies 59
5 Vial Handling
Z-axis assembly
Gripper inside
Z-axis assembly
Gantry
Vial shown
on shutter
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 If there is a broken vial in the oven, the oven will contain sharp,
broken glass as well the contents of any sample material.
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
Agilent Technologies 73
6 Pressures and Flows
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.
7
Communications
Troubleshooting Headspace Sampler Communications 80
To Troubleshoot LAN Connectivity Issues 81
The GC Does Not Start After the HS Injects 85
Agilent Technologies 79
7 Communications
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.
8
Electronics
To Check the Headspace Sampler Power Configuration 88
To Perform the Instrument Self Test 89
Thermal Shutdowns 90
Agilent Technologies 87
8 Electronics
Agilent 7697A
A.01.01
Power on successful
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.