The determination of arsenic and antimony by hydride generation inductively coupled plasma atomic emission spectrometry is discussed, A comparison is made of different procedures for eliminating redox (HNO3) and transition metal interferences; two pre-reduction agents, three continuous-flow systems and two gas-liquid separators were studied. The prereduction agents were KI and thiourea, which were added in a continuous-flow mode either before or after the introduction of tetrahydroborate. The spray chamber served as a gas-liquid separator; alternatively a U-tube separator was used. In the recommended system, 10% m/v thiourea is added to the sample stream before 1.0% m/v tetrahydroborate is introduced, using the spray chamber as a gas-liquid separator. Thiourea eliminated the oxidation interference from HNO3 and also the interference from 50 mg l(-1) of Ag+, Cu2+, Ni2+ and Fe3+.