Sampling (“scrape test”) and analytical procedures were defined to determine PCBs in sorbing solid surfaces such as wall plaster. After sampling, samples were extracted by means of a mechanical device. Following steps included clean-up on a multilayer chromatographic column and assessment with macrobore capillary gas chromatography equipped with an electron capture detector. Mean recovery yields were ≥75% for PCB levels from 2.00 to 7000μ g/m2(0.550-1940 μg/kg). Intralaboratory tests performed by two independent operators yielded: (a) maximum deviation from expected value, 25%; (b) maximum deviation between operators, 17%; and (c) maximum variation coefficient, 20%. Background PCB levels in wall surface layer samples were≥ 2.9μig/m2 (≥ 0.81 μ*g/kg). The analytical procedure tested with agricultural topsoil samples provided mean recovery yields >65% for PCB levels ≥ 500jig/kg (≥ 50 mg/m2). © 1990, Taylor & Francis Group, LLC. All rights reserved.