The possible volatilization of As(III, V), Sb(III, V), and Se(IV, VI) from mixtures of HCI04/HF is investigated. It is shown that there are no losses with Sb and Se irrespective of the initial oxidation state, and with As(V). As(III) is partially or totally lost by volatilization; this can be avoided by oxidizing As with HCI04. The oxidation state of all three elements after the HCI04/HF treatment is determined. These results lead to a recommended procedure for the dissolution of siliceous materials in which As, Sb, or Se are to be determined.Silicates are often dissolved for analytical purposes by a mixture of HF and HC104 (1, 2). However, it is not clear from the literature (3, 4) if in the course of this operation, which comprises partial or total evaporation of the solution, there are losses of traces of As, Sb, and Se. The usefulness of some existing literature data is restricted, because (a) the oxidation state and the weight of the elements used in an experiment are not stated ( 5), (b) the possibility of absorption by platinum vessels-which was demonstrated for Se (6)-is often not taken into account (5, 7,8), (c) it is often not possible to decide if the observed losses are really due to volatilization and not to some other step in the procedure used.The volatilization of Se from different solutions was studied by Bock and Jacob (9), but the system HF/HC104 has received