We report the results of polychlorinated biphenyls (PCBs) in the urban surficial soil of East Chicago, Indiana, USA, from thirty-three sites. PCB congeners were measured using tandem mass spectrometry (GC-MS/MS) in multiple reaction monitoring mode (MRM), a method that provides a high-level selectivity and sensitivity for PCBs in complex environmental samples. One hundred and seventy-one individual PCB congeners were detected and measured. The concentration of total PCB ranged from 20 to 1700 ng/g dry weight. Soil total organic carbon (TOC) was also measured using a Total Organic Carbon Analyzer and reported here. As QA/QC and using the same analytical method as for the soil samples, results from certified standard reference sediments (SRM 1944, National Institutes of Standards and testing) are also reported.