1150 Troubleshooting

1150 Troubleshooting
1150 Troubleshooting
Most of the problems associated with sampling valves are related to peak
broadening in transfer lines and inlets, sample adsorption by the valve or
transfer lines, leaks, and perturbations in the baseline.
Chromatographic symptoms
Troubleshooting valves and their related plumbing is primarily a matter of
systematic checking and verification of unimpaired mechanical operation of
any moving part. This requires an understanding of how the valve functions
internally and how the plumbing is configured. A plumbing diagram is
essential for effective troubleshooting.
The following “symptom-cause” list gives the most commonly encountered
problems found with valves and their solution.
Table 1150-1
Troubleshooting valve related chromatographic problems
Possible cause
Lost peaks (degradation)
Valve or transfer lines too hot
Reduce temperature 50°C, reevaluate
Transfer line activity
Use nickel or Hastelloy tubing
Lost or tailing peaks
Valve or transfer line too cold
Increase temperatures 50°C, reevaluate
Baseline perturbation
Slow valve rotation
Increase actuator pressure
Rotor distorted
Replace rotor
Sample/column pressure too
Add back-pressure regulator to sample
Column overload
Use smaller sample loop
Increase split flow
Flow too slow
Increase column flow
Increase split flow
System voids
Check connections
Reduce volume of connecting tubing
Peak tailing broad peaks
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Chromatographic symptoms
Loss of sensitivity or excessive drift
Several possible causes exist for overall deterioration of the chromatogram.
Contamination in the valve requires a thorough cleaning.
Internal leakage requires a complete disassembly and inspection of the
mating surfaces.
Poor temperature control may require a full check of electronic and
thermal components.
Lack of proper conditioning techniques, columns, etc.
Failure or deterioration of other components (columns, detectors, etc.).
Loss of peaks in specific areas of the chromatogram
Entire sections of chromatographic data can be lost due to a valve that does
not rotate or one that rotates improperly. Other than obvious component
failures (solenoid, actuator, etc.), improper adjustments and misalignments
cause most problems.
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Check that adequate air (about 482 kPa or 70 psi) is supplied.
Check the valve. Is it rotating?
If the valve rotates, check for proper alignment of the actuator,
mechanical binding or slippage of connecting parts.
Check for blocked flow paths with valve in both positions.
Agilent 6890 Gas Chromatograph Service Manual
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Chromatographic symptoms
Extraneous peaks
Air peaks are sometimes seen in a chromatogram when leakage occurs
because the valve rotor does not seal properly. These leaks may not be
detectable using the soap-bubble method.
If a leak is suspected but cannot be located with soap bubbles, a pressure
check will determine definitely if a leak exists. Extraneous peaks can occur
due to contamination or improper conditioning of the valve. If leaks are not
apparent, clean or condition the valve.
Other causes, totally unrelated to the valve, may produce similar symptoms.
Impure carrier gas (i.e., containing water) can cause extraneous peaks.
Peak broadening and tailing
Voids in the flow system (valve and connecting tubing) cause tailing and peak
broadening. Use inlets and liners with small internal diameters and connect
the valve to the inlet or column with short lengths of connecting tubing of
narrow inner diameter.
If early-eluting peaks are too broad, stationary phase or thermal focusing
effects should be used with packed-column ports or increased split flows
when capillary split inlets are used. Inlets should be equipped with narrow
inner diameter liners, and narrow-bore connecting tubing should be used
between the valve and inlet.
Baseline shifts
Baseline perturbations are caused by changes in column flow as the valve is
rotated and as the sample loop equilibrates to system pressure. Slow valve
rotation momentarily stops carrier gas flow and, when the valve stops
rotating, a sudden increase in flow occurs which slowly returns to the set
point. Check actuator pressure (usually 40 to 75 psi), valve rotor tension, and
valve temperature to ensure that the valve rotates as quickly as possible. A
restrictor or backpressure regulator can be added to the sample vent line to
maintain the sample loop at system pressure. This will reduce the time it
takes for the flow to stabilize after the valve is switched.
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Chromatographic symptoms
Baseline upsets
Frequently, baseline upsets may be seen on chromatograms when valves are
switched. These upsets are caused by pressure changes within the system,
injections of large volume samples, or by changing the amount of restriction
in the flow path. These upsets will become more of a problem when high
sensitivity is required. Addition of a fixed restriction downstream from the
valve may help minimize the upset. Changes in column length may also help
reduce the upsets.
Fixed restrictors are used immediately before flame detectors to prevent
flameout and are used in some instances to prevent pressure surges from
damaging TCD filaments. An adjustable restrictor (needle valve) can also be
used where a matched restriction is desired but not for preventing pressure
or flow surges.
Often confused with baseline upsets, an offset is a shift in the baseline that
does not return quickly to the original level. Baseline offsets may be caused
by air leaks but more commonly are due to a change in gas purity or flow rate
in the detector. Poor carrier gas or improperly conditioned filters and traps
should be suspected whenever offsets occur.
Variation in peak area and retention time
The amount of sample contained in the loop and, therefore, the amount
injected onto the column is affected by loop pressure and temperature.
Variations in pressure and temperature lead to variability in peak areas. Flow
restrictors or back-pressure regulators help to maintain constant loop
pressure, and valve boxes help maintain temperature.
Leaks can occur in the valve itself or at any of the connecting points with
transfer lines. Leaks usually cause area irreproducibility, retention times
changes, and increases in the area of air peaks (with thermal conductivity
detectors). Leaks in rotors can sometimes be fixed by tightening the nuts
holding the rotor in the valve body. Leaks in connections are usually found
with an electronic leak detector or with a liquid leak detection fluid (e.g.,
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Pressure check
Pressure check
Leak checking the plumbing involved in a valve system must be done carefully
and methodically. The pressure check method below will indicate, but
sometimes not isolate, a leak in the flow path. Since this method does not
necessarily isolate the leak, other leak check methods may be needed to locate
the leak specifically.
Each valve in a system has two flow paths, ON and OFF. A leak sometimes
occurs in only one of these two positions. Check both.
Disconnect the detector from the valve system.
Cap the valve system at its outlet and pressurize to 689 kPa (100 psi).
Allow 2 to 5 minutes for pressure to equilibrate. If your instrument has
flow control, it should read zero flow.
Turn off the gas supply at the source.
Generally, the pressure will drop quickly for approximately 30 to 60
seconds, then stabilize. After this initial pressure drop, the gauge should
not indicate more than a 7 to 14 kPa (1 to 2 psi) drop during a 10 minute
5a. If no leak is indicated, actuate all valves and repeat steps 2 to 4.
5b. If a leak does show up, try to pinpoint the source using a soap bubble
meter. Do not assume that the leak exists only at the valve. Often plumbing
connections such as unions or bulkhead fittings are at fault. See Valve
Box should it become necessary to expose the valve system.
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If the leak cannot be found easily, divide the system in half and repeat
the pressure check. Continue dividing in halves, and pressure check until
the leak is isolated.
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Pressure check
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