Many volumetric methods have been reported for the determination of perchlorate. Most of these are indirect, requiring reduction to chloride. Either the chloride is subsequently measured (7-J) or the amount of reductant is determined by back-titration (4, 6, 7). These methods are all subject to interference by other halide salts or reducible substances.Several direct methods have also been reported. A microgravimetric technique using 3,5,6,8-tetramethyl-l,10-phenanthroline to precipitate perchlorate was reported by Brandt and Smith (8). Perchlorate has been determined colorimetrically by Bodenheimer and Weiles (9) in pyridine as the cupric tetrapyridine salt and by Fritz, Abbink, and Campbell (70) as ferrous 1,10-phenanthroline perchlorate in «-butyronitrile. Tetraphenylphosphonium chloride has been used by Nezu (77) as an amperometric titrant for perchlorate. Recently, Morris (72) described the amperometric determination of perchlorate by titration with tetraphenylstibonium sulfate.The use of tetraphenylarsonium ion for perchlorate analysis was reported as early as 1939 by Willard and Smith (13), who proposed a potentiometric back-titration with triiodide. Recently, the reagent was used for the gravimetric determination of ammonium perchlorate by Glover and Rosen (14). Another approach to the use of this reagent for perchlorate determination, herein proposed, incorporates the use of conductance for the titration of perchlorate with tetraphenylarsonium chloride. EXPERIMENTAL Reagents. Tetraphenylarsonium chloride (J. T. Baker Chemical Co.) and tetraphenylarsonium chloride hydrochloride (Eastman Organic Chemical Co. and Hach Chemical