TABLE III

Partial List of Potential Problems That Can Occur in the Headspace-GC/MS Analysis on Aqueous Extracts (VOC Analysis) That Could Lead to Omission of Compounds, with a Suggestion on How to Potentially Avoid These Omissions

Headspace-GC/MS on AQUEOUS EXTRACTS
Type of ProblemDescription of ProblemPotential OmissionsHow to Avoid Omissions
Sample preparation – Sample introductionCompounds with high water solubility will poorly partition into the headspace, reducing sensitivityLow MW Acids, Alcohols, Amines, thiols, etc. …Low MW Acids: Aqueous extracts via Ion Chromatography
Amines & thiols: Use orthogonal analytical methods that show a sufficient response for these compounds (LC/MS ESI; derivatization GC/MS)
Verify the results of the neat Headspace-GC/MS analyses
ChromatographyCompounds eluting in the solvent peak (when analyzing WFI/Alcohol-mixes)Isomers of pentene, pentane, diethyl ether, isomers of pentadiene, ethyl formate, carbon disulfide, acetonitrile, etc. …Verify the results of the neat Headspace-GC/MS analyses
Consider Mass Spectral Deconvolution options in combination with an Internally Developed Mass Spectral Database
ChromatographyReactive compounds may hydrolyze or polymerize in aqueous sample.Silanes, conversion of trimethylsilanol to hexamethyl-disiloxane, 1,2-ethanediol diformate to methyl formate and ethanol, etc. …Verify the results of the neat Headspace-GC/MS analyses