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A method for the quantification of the sum of short chain chlorinated paraffins (SCCPs) by GC–ECNI-MS was developed. This method is suited to the special demands of environmental sediment analysis using an approach of sum determination by multiple regression quantification and is independent of the chlorine content as well as robust against changes in C-number distribution of the SCCPs to be analysed. The method is based on the integration of the signals for two selected m/z values (375 and 423) over the full retention range of the SCCPs. The calibration is performed using three synthetic mixtures representing the variety of SCCP-mixtures as found in environmental samples as well as in technical mixtures. Quantification is performed using a multiple linear regression calibration with two selected m/z value signals achieving an LOQ of 0.6 μg/g sediment. The proposed quantification procedure for sediments was verified by 16 independently prepared and differently composed SCCP-mixtures mimicking a variety of sediment samples quoted in literature. For the analysis of the sediment samples a two-step clean-up was applied comprising a column chromatographic clean-up and GPC. The method allows for a standardized analysis according to the European water framework directive, especially in the case of trend monitoring of sediments.

International audience; A first preliminary interlaboratory trial was planned to prepare ISO/DIS 12010: Water quality - determination of short chain polychlorinated alkanes (SCCP) in water - method using GC/MS and electron capture negative ionisation (ECNI). The task was to determine the sum of short chain polychlorinated n-alkanes with carbon chain lengths of C10-C13 and a chlorine content between 49 and 67% in water by GC-ECNI-MS and quantification by multiple linear regression described in ISO/DIS 12010 as the compulsory method. Distributed samples were obtained from a real water extract spiked with a target concentration of 0.4 micro g/mL sum of SCCP, i.e. the environmental quality target level according to the Water Framework Directive. The interlaboratory trial included the calibration, a column chromatographic clean up, a concentration step and an integration of chromatographic unresolved humps as well as the quantification with multiple linear regression. Reproducibility standard deviations between 21.5 and 22.9% were achieved by 17 participating laboratories from four countries. The method outlined no significant difference of the results between the standard solution and a real water matrix extract. On the basis of this succeeded preliminary interlaboratory trial the final interlaboratory trial for validation of ISO 12010 was prepared in autumn 2010.

International audience; A validation interlaboratory trial was carried out to prepare ISO 12010: Water quality-Determination of short-chain polychlorinated alkanes (SCCP) in water-Method using gas chromatography/mass spectrometry (GC-MS) and electron capture negative ionisation (ECNI). The task was to determine the sum of short-chain polychlorinated n-alkanes with carbon chain lengths of C-10-C-13 and a chlorine content between 49% (g/100 g) and 67% (g/100 g) in water by GC-ECNI-MS. The quantification had to be performed by multiple linear regression as described in ISO/DIS 12010, the compulsory method. Samples distributed were real river samples, and waste water spiked with a target concentration of 0.4 and 0.6 mu g/L for the sum of SCCPs, i.e. a concentration around the environmental quality target level according to the European Water Framework Directive. The different types of water samples tested were surface water with