An analytical method is described for the determination of trace amounts of sulfur by charged particle activation analysis. The method consists of proton irradiation followed by a rapid radiochemical separation of the product nuclide,34m Cl. This procedure has been applied to a number of pure metal samples which range in sulfur content from 0.3 to 30 ppm. All analyses were repeated several times to ensure consistent results and to better evaluate experimental detection limits and systematic errors. The results indicate that sulfur determinations can be performed at a concentration of less than 1.0 ppm. Activation curves are presented for the reactions S(d,x)34mCl, S(p,x)34mCl, and the interfering reaction35Cl(p, pn)34mCl.