Headspace Gas Chromatography/ Mass Spectrometry

Approaches

Solid or liquid samples are sealed in headspace vials.  Water or a high-boiling organic solvent may be added to the vial to dissolve the sample and facilitate release of volatile compounds to the gas phase. 

The headspace vials are typically heated to drive partitioning of volatiles from the solid or liquid phase into the gas phase.  Sample vials can be agitated during heating.

Sampling of the headspace for GC/MS injection  is usually performed via a heated gas-tight syringe.  If greater sensitivity is required, solid phase micro-extraction (SPME) can be used to concentrate volatiles prior to GC/MS analysis.

 

Sample Considerations

Virtually any sample that can be made to fit into a headspace vial can be tested.  However, the sample matrix itself should not be highly volatile.

The required sample size for headspace GC/MS is inversely proportional to the concentration(s) of volatile compound(s) that must be detected or quantified.

A sample size of 0.1 to 10 g is typical for headspace GC/MS.  Quantitative analysis usually requires a larger sample amount because a standard addition method is used.

Samples for quantitative headspace GC/MS should be homogeneous with respect to the concentration of volatiles.

Contact us to talk through your specific sample considerations and chromatography testing needs.

Experience

Work we've done:

• Identification and quantification of residual solvents in packaging materials for food contact or pharmaceutical applications
• Odor analysis in polyolefin packaging film
• Identification and quantification of volatile organic compounds (VOC’s) present in polymers used for medical implants
• Identification of compounds responsible for off-odor in post-consumer recycled carpet
• Residual solvents in pharmaceutical actives and excipients
• Quantification of residual blowing agents in polyolefin foam
• Identification of off-gas products from combustion or pyrolysis of polymers