GC Troubleshooting Tips

BASIC STEPS SYMPTOMS AND SOLUTIONS Split Peaks Response Variation

Follow these basic troubleshooting steps to isolate problems related to the sample, injector, detector, and column. Good chromatography is critical to obtaining accurate, reproducible results. Causes Solutions Causes Solutions
Check the obvious explanations first and change only one thing at a time until you identify and resolve the problem. Coelutions, asymmetric peaks, baseline noise, and other issues are common Mismatched
• Adjust solvent or stationary phase to • Check sample concentration.
solvent/stationary
challenges in the GC laboratory. These analytical problems and others can phase polarity
allow wetting. Sample issues • Check sample preparation procedure.
Check the Obvious: be overcome by troubleshooting your separations using the tips below. • Check sample decomposition/shelf life.
• Add surface area, such as wool, to the inlet
• Power supply • Gas purity • Syringe condition Incomplete vaporization liner to enhance vaporization. • Replace syringe.
Syringe problems
• Electrical connections • Gas flows • Sample preparation • Use proper injector temperature. • Check autosampler operation.

• Signal connections • Temperature settings • Analytical conditions Sample loading capacity • Inject less sample (dilute, use split injection, • Verify signal settings and adjust if needed.
Poor Resolution exceeded reduce injection volume).
Electronics
• Repair or replace cables or boards.
Fast autosampler injection • Use wool or slow injection speed.
Identify the Cause: Causes Solutions
into open liner
Dirty or damaged
detector
• Perform detector maintenance or
replace parts.

• Define the problem clearly; for example, “Over the last 4 days, only the phenols in my sample have been tailing.” Non-selective • Choose appropriate stationary phase and
Flow/temperature • Verify steady flow rates and temperatures, then
stationary phase column dimensions.
settings wrong or variable adjust settings and/or replace parts if needed.
• Review sample and maintenance records to identify trends in the data or problem indicators, such as area counts • Optimize carrier gas linear velocity and
Poor efficiency • Remove contamination and use properly
decreasing over time or injector maintenance not being performed as scheduled. GC oven temperature program.
Carryover/Ghost Peaks Adsorption/reactivity
deactivated liner, seal, and column.

• Use a logical sequence of steps to isolate possible causes. Sample overload

• Adjust sample concentration or amount
• Check for leaks at all connections and repair
on column. Leaks
connections as needed.
Causes Solutions
Document Work and Verify System Performance: Incorrect analytical • Verify temperature program, flow rates,
and column parameters. Contaminated syringe • Replace rinse solvent. • Verify injection technique and change back to
conditions used Change in sample
or rinse solvent original technique.
• Document all troubleshooting steps and results; this may help you identify and solve the next problem faster. Injection 1 • Rinse or replace syringe. introduction/injection
• Check that split ratio is correct.
method
• Always inject a test mix and compare to previous data to ensure restored performance. • Inject a smaller amount. • Verify that the splitless hold time is correct.
• Use a liner with a large internal diameter.
• Increase head pressure (i.e., flowrate) to
Poor Retention Time Reproducibility contain the vapor cloud.

EXAMPLE TROUBLESHOOTING SEQUENCE

Backflash (sample volume
• Use slower injection rate.
exceeds liner volume)
• Lower inlet temperature. No Peaks
Causes Solutions • Increase split flow.
• Leak check injector and press-fit connections.
An analyst observed that no peaks appeared during a GC-FID analysis. The flowchart below shows a logical Injection 2
• Use liner with packing.
Causes Solutions
Leaks • Replace critical seals (i.e., septa, O-rings, • Use pressure-pulse injection.
progression of steps that can be used to identify the cause and correct the problem. inlet disc, etc.) • Plugged syringe; clean or replace syringe.
Injection problems
• Extend analysis time to • Verify there is sample in the syringe.
• Maintain inlet liner and GC column.
Last analysis ended allow all components • Injecting into wrong inlet; reset autosampler.
There is flow Syringe works Analyte adsorption • Use properly deactivated liners, too soon and/or matrix interferences
Flame is lit.
and the column
is not broken.
and contains
sample.
END seals, and columns. to elute. • Verify carrier gas is flowing.

Resolution/integration • Avoid sample overload. Broken column • Replace column.

YES YES YES YES issues
Column installed into • Re-install column.
Incorrect column/oven • Verify column temperature and wrong injector or
Is the flame lit? Is there adequate Is the sample reaching
temperature program oven temperature program.
High Bleed detector
column flow? the column? Incorrect or variable carrier • Verify the carrier gas flow and linear velocity. • Signal not recorded; check detector cables
No peaks Test/Check: gas flow rate/linear velocity Repair or replace parts if neccessary. and verify that detector is turned on.
Are there
• Water condensation? Test/Check: Test/Check: Re-inject Causes Solutions Detector problems
from FID • Detector gases on?
peaks? • Detector gas turned off or wrong flow rates
• Column flow? • Syringe plugged or broken? Poor control of oven • Confirm GC oven program falls within Improper column • Increase conditioning time and/or temperature.
• Column installed correctly? • Broken column? used; turn detector on and/or adjust
• Sample in syringe? temperature programming instrument manufacturer’s recommendation. conditioning
• Plugged FID jet? flow rates.
Incorrect oven • Extend GC oven equilibration time. • Trim column and/or heat to maximum
equilibration time temperature to remove contaminants.
NO Return detector to NO NO Contamination • Replace carrier gas and/or detector gas filters.
operating condition If manual injection, delay • Use autosampler or standardize manual
and light flame. Verify Repair or replace • Clean injector and detector.
between pushing start and injection procedure.
condensation is gone,
Adjust flow or
replace column.
syringe; ensure
syringe is filling.
actual injection
• Check for oxygen leaks across the entire system
Broad Peaks
gases are on, and Leak in system and
column is correctly oxidation of stationary and replace seals and/or filters.
installed. phase • Replace column. Causes Solutions
• Minimize dead volume in the GC system;
High dead volume verify proper column installation, proper
Fronting Peaks connectors, proper liners, etc.

Causes Solutions
Unstable Baseline (Spiking, Noise, Drift) Low flow rates
• Verify injector and detector flow rates and
adjust if needed.
Incompatible stationary • Choose appropriate stationary phase. • Verify make-up gas flow and adjust if needed.
phase Causes Solutions
Slow GC oven program • Increase GC oven programming rate.
• Reduce amount injected, dilute sample. • Leak check connections and replace seals
Spiking Carrier gas leak or if needed.
Column overloading • Increase column inner diameter and/or contamination Poor analyte/solvent • Lower GC oven start temperature.
film thickness. • Replace carrier gas and/or detector gas filters. focusing

Injector or detector • Clean system and perform regular • Reduce retention of compounds by
Column film is too thick
contamination maintenance. decreasing film thickness and length.

Column contamination • Condition, trim, and rinse column. Sample carryover • See Carryover/Ghost Peaks solutions.
Tailing Peaks or stationary phase bleed
• Replace septum.
Causes Solutions Septum coring/bleed • Inspect inlet liner for septa particles and
Noise replace liner if needed.
• Use properly cleaned and deactivated liner,
Adsorption due to surface seal, and column. Loose cable or circuit • Clean and repair electrical connections.
activity or contamination • Trim inlet end of column. board connections
• Replace column if damaged.
• Verify flow rates are steady and reproducible;
Variable carrier gas or may need to replace or repair flow controller.
Adsorption due to chemical • Derivatize compound. detector gas flows
composition of compound Drift • Leak check system.

• Check for leaks at all connections, replace • Allow enough time for detector temperatures
Leak in system Detector not ready
For an in-depth discussion on how to choose the right column and critical seals if needed. and flows to equilibrate.
improve your chromatographic results, visit www.restek.com • Minimize dead volume.
Installation issues • Verify that the column is cut properly (square).
• Download our Guide to GC Column Selection and Optimizing Separations
(lit. cat.# GNBR1724- UNV) • Verify correct installation distances.
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• Request our Simplifying Column Selection poster (GNWC1612-UNV) Lit. Cat.# GNWC1723-UNV All rights reserved.
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