Preliminary interlaboratory trial for ISO/DIS 12010 : determination of short chain polychlorinated alkanes (SCCP) in water
Résumé
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.