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By Grob R

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E. bound to the matrix in the same way as the unknown) which is preferably labelled (radioactive labelling would allow verification of the recovery) would be necessary. Such materials not being available, the extraction method used should be validated by other independent methods. Supercritical extractions could be the methods of choice. g. for butyltins [34,35], and seem to offer good possibilities for extracting the species without alteration. These various comments clearly underline that validation of extraction procedures has still not been achieved.

In the best case, each critical step of the procedure should be evaluated in an adapted exercise. The individual steps may be studied with a series of different materials in a stepwise manner. g. pure solutions andor mixtures of compounds in solution, which are used to test the performance of the detector. g. raw extract, purified extract) enables testing the separation andor clean-up steps, whereas solid samples are used to test the entire procedure. Spiked samples can be analysed to evaluate the extraction procedure, keeping in mind that a complete recovery of a spiked analyte does not mean that the same performance will be achieved with a naturally bound determinand (conversely, if a poor recovery is obtained with a spiked sample, one can assume that this procedure will not work with a natural sample).

The outcome of the different exercises is discussed among all participants in technical meetings, in particular to identify random and/or systematic errors in the procedures. Whereas random errors can be detected and minimized by intralaboratory measures, systematic errors can only be identified and eliminated by comparing results with other laboratories/techniques. When all steps have been successfully evaluated, i. e. all possible sources of systematic error have been removed and the random errors have been minimized, the methods can be considered as valid.

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Modern practice of gas chromatography by Grob R


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