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Troubleshooting of

GC Systems
Techniques, Tips, and Tricks

Daron Decker
Chromatography Technical Specialist

Troubleshooting of GC Systems
Agilent Restricted
Page 1

Logical Troubleshooting
G

Troubleshooting Starts with Isolating the problem


Is it injection, flow, column, detection, electronic or some combination?
Know what can and cant cause the symptom and what to do about it
Broad Solvent Peak Injector Problems, Technique, Sample Problems
Split Peaks Injector Problems, Mixed Solvent
No Peaks Wasnt Introduced, Wasnt Detected
Bonus Peaks In Sample or Back Flash
Response Changes Activity, Inlet Discrimination, Detector Problem
Peak Tailing Flow Path or Activity
Peak Fronting Overload or Solubility Mismatch
Shifting Retention Leaks, Column Aging, Contamination or Damage
Loss of Resolution Peak Broadening, Separation Decreasing
Baseline Disturbances Column Bleed, Contamination, Temperature
Noisy or Spiking Baseline Electrical or Contaminated Detector
Negative or Flat-topped Peaks Detector Problems
Quantitation Problems Activity, Inlet or Detector Problems
Troubleshooting of GC Systems

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Broad Solvent Front (or Major Component)

Troubleshooting of GC Systems
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Broad Solvent Front


Technique

Installation problem
Large injection volume
Very slow injection rate
Leak in the injector

Troubleshooting of GC Systems
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Broad Solvent Front


Injector Parameters

Split ratio too low


Purge off for split injection
No or long purge activation time (splitless)
Injector temperature too low/high

Troubleshooting of GC Systems
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Broad Solvent Front


Sample Related

Dirty sample
Mixed sample solvent
Impure solvent
Column temperature < solvent BP

Troubleshooting of GC Systems
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Split Peaks

Injector problem (poor sample intro)


Mixed sample solvent (polarity difference)
Sample in syringe needle
Sample degradation in injector
Injection technique - erratic
Troubleshooting of GC Systems
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Injection technique - erratic

Which peaks?

Early or late?

Trends?

Troubleshooting of GC Systems
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No Peaks
Detector/recorder not operational
Plugged syringe/plunger not moving
Wrong injector or detector
Broken column
Huge leak
No carrier gas flow
No column
Troubleshooting of GC Systems
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A Real Troubleshooting Example


No Peaks

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Troubleshooting of GC Systems
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Logical Steps Taken to Find Peaks


(most of our problems are leaks and plugs)
Is the flame Lit?

put glass piece over FID outlet----Answer in this case, Water condenses

look at output in instrument guage-- is the digital value greater than 0.0?
Answer in this case is approximately 16.2 pico amps

Is there flow through the column?


disconnect column from detector and measure flow with bubble solution or meter

Answer in this case was YES THERE IS FLOW


Assess the observations
I

Flame is lit and we have flow from end of column

Hypothesis: Sample not getting on column-syringe plugged?

Take syringe out and make injection manually on a dry paper towel
Answer towel stayes dry (Syringe was clogged with septum)
Pull plunger out top, add solvent and replace plunger will usually dislodge septum particle
(should hear a little pop)
If you cant dislodge plug, Replace syringe
Reassemble the Injector & Re-inject

Troubleshooting of GC Systems
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Peaks !!
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Troubleshooting of GC Systems
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Bonus Peaks or Ghost Peaks

Contamination in injector, column or carrier gas


Carry-over from a backflash or previous sample
Septum bleed

Troubleshooting of GC Systems
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Peak Response
All Change in Size

INJECTOR
Leaky syringe
Split ratio set incorrectly
Wrong purge activation time
Septum purge flow too high
Injector temperature too low

DETECTOR response problem


Attenuation value
High background signal
Detector zeroed at a high signal level
Troubleshooting of GC Systems
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Peak Response
Some Change in Size

Adsorption of active compounds (-OH, -NH, -SH) by liner,


column or contaminants
Decomposition or evaporation from sample
Inlet Temperature Change Discrimination

Troubleshooting of GC Systems
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Peak Tailing

Reversible adsorption of active compounds


(-OH, -NH, -SH) by liner, column or contaminants
Flow path problem - dead volume, obstruction, poor
installation, or severe column contamination

Miscellaneous - overloading of PLOT columns, co-elution,


polarity mismatch between phase, solute or solvent, and some
compounds always tail
Troubleshooting of GC Systems
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Peak Fronting
Shark Fin Shaped

Overload
More pronounced with large solute and
phase polarity differences

Troubleshooting of GC Systems
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Peak Fronting
Other

Compound very soluble in


injection solvent
Column installation
Injection technique
Co-elution
Mixed sample solvent

Troubleshooting of GC Systems
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Retention Time Shift


Leak in the septum
Change in gas velocity

2.00

Change in injection solvent

4.75

2.75

Large change in sample


concentration

5.50

Change in temperature

3.25

4.00

Loss of stationary phase


Contamination
Damaged stationary phase

Troubleshooting of GC Systems
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Effect of Sample Overload on


Retention Time and Peak Tailing

1400 ng

7 ng

10

11

min
Troubleshooting of GC Systems

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Loss of Resolution

Separation

Peak Width

Resolution is a function of separation and peak width

Troubleshooting of GC Systems
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Loss of Resolution
Separation Decrease

Different column temperature


Column contamination
Co-elution
Different column?

Troubleshooting of GC Systems
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Loss of Resolution
Peak Broadening

Change in carrier gas velocity


Column contamination
Column degradation
Injector (split flow, liner, installation)
Detector (flow, installation)

Troubleshooting of GC Systems
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Baseline Disturbances
Sudden Changes, Wandering, or Drifting

WANDER
Column or detector not fully conditioned
Changes in carrier and detector gas flows
Valves switching, leaks

Detector thermal or current instability


GC/MS scan range change
Contamination

DRIFT
Troubleshooting of GC Systems
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Noisy Baseline
MILD

SEVERE
Contamination, gas, detector, etc.
Column in detector flame
Incorrect detector gas flows
Air leak - ECD, TCD
Detector electronics malfunction
Troubleshooting of GC Systems
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Spiking Baseline

Particles entering the detector


Random: poor connection
Regular: nearby "cycling" equipment

Troubleshooting of GC Systems
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Negative Peaks

Normal for TCD, ECD


All peaks - check recorder
connection and settings
Dirty or old cell if after large
peaks with ECD

Troubleshooting of GC Systems
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Flat-Topped Peaks

Maximum detector signal exceeded


Maximum recorder signal exceeded
Excessive sensitivity settings

Troubleshooting of GC Systems
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Quantitation Problems
System

Detector problem (stability)


Outside detector's linear range
Recorder settings
Activity (adsorption)

Troubleshooting of GC Systems
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Quantitation Problems
Technique or Conditions

Injection technique or conditions


Syringe worn
Baseline disturbances
Co-elution
Matrix effects
Sample evaporation leaky vials
Sample decomposition
Troubleshooting of GC Systems
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Troubleshooting Tips
1. Isolate the problem.
(Blank Run, Inject Un-retained Compound, Jumper Tube Test)

2. Change only one variable at a time.


3. Compare before/after chromatograms.
(Peak shape, response, retention, baseline rise, background, etc.)

4. Utilize Technical Support.

Troubleshooting of GC Systems
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TECHNICAL SUPPORT
1-800-227-9770, #4, #1
1-972-699-6423 (Daron)
1-877-874-0307 (toll free)
281-997-9107 (FAX)

E-mail:
Daron_Decker@Agilent.com

Troubleshooting of GC Systems
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