A modified oxygen flask technique is described for determining As in organic compounds, the conventional Pt supports being replaced by Al spirals or steel gauzes, which resist attack by As during the vigorous combustion. A favorable gravimetric factor is ensured by the quantitative precipitation of the As as ammonium uranyl arsenate and subsequent ignition, under controlled conditions, to the black triuranium octaoxide, U/sub 3/O/sub 8/. Phosphate and vanadate form similar insoluble ammonium uranyl salts, and the method is not directly applicable to organic compounds containing these elements without prior separation. (auth)