A procedure for the quantification of the PCB marker congeners 28, 52, 101, 138, 153, 180 in plastic waste form the recycling of cables in the range of content between 0.1 mgkg(-1) and 20 mgkg(-1) was validated. Representative reference materials for laboratory analyses were produced using granulates from different recycling processes. The method development included aspects of grinding, sieving, homogenising as well as the comparison of extraction methods and chromatographic conditions. The validated procedure foresees grinding of the technical sample to an upper particle size limit of 0.50mm followed by extraction with an unpolar solvent such as n-hexane and gas chromatographic determination. LOD and LOQ for individual congeners ranged between 0.01 mgkg(-1) and 0.08 mgkg(-1). Electron capture detection (ECD) and mass selective detection (MS) were equivalent if chromatographic conditions were appropriately selected. The application of MS was advantageous in presence of significant amounts of interfering components which have been found in some cables. Three reference materials containing the marker congeners in the range of 0.1 mgkg(-1)-5 mgkg(-1) were submitted to a final validation intercomparison with 23 selected field laboratories using the developed method. Relative reproducibility standard deviations varied between 15% and 33%.