A gas chromatographic assay for quantitative analysis of volatiles in solid materials by discontinuous gas extraction

Summary A method has been developed for the quantitative analysis of volatile compounds in solid samples. The method is based on a stepwise gas extraction of the volatiles with subsequent analysis of the extracted material and is termed discontinuous gas extraction. Any quantitative analysis requires an exhaustive extraction, which, however, is often too time-consuming for routine analysis. It is shown how the total amount of each volatile compound can be calculated from only a few extractions. Such a calculation is possible because for analytical purposes it is the information of the extraction process and not the extracted material that is needed. This method is useful for samples which are insoluble, such as certain polymers or residual solvents in printed foils, and which cannot be analyzed quantitatively by headspace gas chromatography, since no calibration solution can be prepared. It is further shown how discontinuous gas extraction can also be used to calibrate headspace analysis. Thus, both methods combine well together in that discontinuous gas extraction provides the accuracy while the headspace analysis gives convenience and speed of sample throughput, particularly if carried out with an automated headspace analyzer.