A simple and rapid differential pulse anodic stripping method for simultaneous determination of cadmium, lead, copper, antimony and bismuth in high purity arsenic and arsenous oxides is described. The most suitable supporting electrolyte is found to be 2M HCI. This method is suitable for the determination of Cd, Sb, Bi (0.1 μg g^-I), Cu(0.3 μg g^-I) and Pb(O.S μg g^-I) (with about 100mg as sample) with a re lat ive standard deviation of 15-20%.