Five agricultural crops were treated with OO‐diethyl O‐(3,5,6‐trichloro‐2‐pyridyl) phosphorothioate (chlorpyrifos) granular or emulsifiable concentrate formulations at dosages from 0.5 to 6.0 kg (a.i.)/ha and at different periods before harvest. Chlorpyrifos residues were determined by gas chromatography after extraction and sweep co‐distillation clean‐up. Low residue levels were found. The average values in lettuce were 0.046 and 0.070 part/million, in sugar beet leaves 0.037 to 0.128 part/million and roots <0.005 to 0.038 part/million; no chlorpyrifos was detected in carrots, potatoes and cured tobacco leaves at the limit of the method (0.005 part/million).