Improvement of quality control of speciation analysis using hyphenated techniques - A decade of progress within the European Community

The awareness of a need for an improved control of environmental contamination levels has led to the development of new hyphenated techniques for the determination of a wide variety of chemical species (e.g., organotins, methyl-mercury, alkyl-lead compounds etc.). These techniques generally involve many analytical steps such as extraction, derivatisation, separation and detection which have to be carried out in such a way that the speciation is not changed during the analytical process. The need for evaluating the method's performance has led the BCR programme of the European Commission (now Standards, Measurements and Testing Programme) to conduct series of interlaboratory studies during the last decade. These projects followed a step-by-step approach for the evaluation of different steps of the analytical methods used, e.g., simple solutions to test the detection, cleaned extract to evaluate the separation, spiked samples to test the extraction and natural samples to evaluate the whole analytical procedures. These collaborative projects allowed most of the sources of errors related to either a technique or a laboratory to be detected and removed. This paper gives an account of discussions of possible errors occurring in speciation analysis and presents examples of technical scrutiny of hyphenated techniques using chromatography as applied to the determination of tributyltin, methyl-mercury and trimethyllead.