The conditions necessary for the complete decomposition of six organic arsenic compounds, namely methylarsonic acid (MMAA), dimethylarsinic acid (DMAA), trimethylarsine oxide, tetramethylarsonium iodide, arsenocholine bromide (AsC) and arsenobetaine (AB), were investigated. The degree of decomposition of the arsenic compounds was monitored using a hydride generation (HYD) technique, because the response from this system depends strongly on the chemical species of arsenic, with inorganic arsenic (the expected product from these decomposition experiments) giving a much more intense HYD signal than the organic arsenic compounds. The arsenic compounds were decomposed by heating them with three types of acid mixture, namely HNO 3 -HClO 4 , HNO 3 -HClO 4 -HF, or HNO 3 -HClO 4 -H 2 SO 4 . Both MMAA and DMAA were decomposed completely using any of the mixed acids at a decomposition temperature of 200 • C or higher. The HNO 3 -HClO 4 -H 2 SO 4 mixture was the most effective for decomposing AsC and AB, which are the most difficult compounds among all types of organic arsenic compound to decompose and render inorganic. The complete decomposition of AB was only achieved, however, when the temperature was 320 • C or higher, and the sample was evaporated to dryness. When the residue from this treatment was examined by high-performance liquid chromatography combined with inductively coupled plasma atomic emission spectrometry, all of the arsenic was found to be present as arsenic(V). The optimized conditions (HNO 3 -HClO 4 -H 2 SO 4 at 320 • C) for decomposing AB were then used to determine the total amount of arsenic in marine organisms known to contain AB.