Methods are described for quantitative extraction of arsenic(III), antimony(III) and bismuth(III) with potassium ethyl xanthate-carbon tetrachloride. The optimum acidity conditions are 0.1-0.2 M hydrochloric acid for arsenic, 1.8-2.5 M hydrochloric acid for antimony and pH 1.5-4.0 for bismuth. From the organic extracts arsenic and antimony are estimated by conventional iodometric methods while bismuth is determined spectrophotometrically at 400 nm. The effect of acidity, reagent concentration, period of extraction and diverse ions are discussed. The infra-red spectra are also described. © 1968 Springer-Verlag.