This paper reports determination of arsenic, antimony and selenium in different matrices using atomic absorption spectrometry, with atomisation in a graphite tube and with generation of hydrides. The actual state of atomic absorption spectrometry as the method of determining As, Sb and Se is described on the basis of literature data. The effects of interference in determinations by atomic absorption spectrometry, and the problems related to sample preparation to determinations (extraction, mineralisation, concentration) are discussed. The application of flow injection analysis in atomic absorption spectrometry with hydride generation is described. The effectiveness of atomic absorption spectrometry in speciation determinations of arsenic, antimony and selenium applied alone and in combination with chromatographic methods is shown.