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
Page 2
Broad Solvent Front (or Major Component)
Troubleshooting of GC Systems
Page 3
Broad Solvent Front
Technique
Installation problem
Large injection volume
Very slow injection rate
Leak in the injector
Troubleshooting of GC Systems
Page 4
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
Page 5
Broad Solvent Front
Sample Related
Dirty sample
Mixed sample solvent
Impure solvent
Column temperature < solvent BP
Troubleshooting of GC Systems
Page 6
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
Page 7
Injection technique - erratic
Which peaks?
Early or late?
Trends?
Troubleshooting of GC Systems
Page 8
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
Page 9
A Real Troubleshooting Example
No Peaks
30
28
26
24
22
20
18
16
14
10
20
30
40
50
Troubleshooting of GC Systems
Page 10
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
Page 11
Peaks !!
30
28
26
24
22
20
18
16
14
0
10
20
30
40
50
Troubleshooting of GC Systems
Page 12
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
Page 13
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
Page 14
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
Page 15
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
Page 16
Peak Fronting
Shark Fin Shaped
Overload
More pronounced with large solute and
phase polarity differences
Troubleshooting of GC Systems
Page 17
Peak Fronting
Other
Compound very soluble in
injection solvent
Column installation
Injection technique
Co-elution
Mixed sample solvent
Troubleshooting of GC Systems
Page 18
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
Page 19
Effect of Sample Overload on
Retention Time and Peak Tailing
1400 ng
7 ng
10
11
min
Troubleshooting of GC Systems
Page 20
10
Loss of Resolution
Separation
Peak Width
Resolution is a function of separation and peak width
Troubleshooting of GC Systems
Page 21
Loss of Resolution
Separation Decrease
Different column temperature
Column contamination
Co-elution
Different column?
Troubleshooting of GC Systems
Page 22
11
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
Page 23
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
Page 24
12
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
Page 25
Spiking Baseline
Particles entering the detector
Random: poor connection
Regular: nearby "cycling" equipment
Troubleshooting of GC Systems
Page 26
13
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
Page 27
Flat-Topped Peaks
Maximum detector signal exceeded
Maximum recorder signal exceeded
Excessive sensitivity settings
Troubleshooting of GC Systems
Page 28
14
Quantitation Problems
System
Detector problem (stability)
Outside detector's linear range
Recorder settings
Activity (adsorption)
Troubleshooting of GC Systems
Page 29
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
Page 30
15
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
Page 31
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@[Link]
Troubleshooting of GC Systems
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