A methodology for preparing the reference material of polychlorinated biphenyls (PCBs) in soil is described. The soil sample collected from a polluted area in east of China was dried, grou fid, homogenized, packed and tested on stability and homogeneity. The materials were analyzed by isotope-dilution mass spectrometry. And then the analysis results were validated by four laboratories. The contents of six indicator congeners (C1328, CB52, CB101, CB138, CB153 and CB180) and eight dioxin-like congeners ( CB77, CB81, CB105, CB114, CB118, CB156, CB157, CB167) were certified for this material. The material was intended for use in the method validation and quality control for congener-specific of PCBs in soil or sediments.