Ag and Au were determined in highly pure Ag and Au samples by dissolving a sample in (1 + 3) HCl, rinsing the HCl-treated sample with distilled H2O, and then placing the residue in an electrode. The spectral line intensity of each element was measured and was compared with those of a standard sample with known amounts Ag and Au which was treated the same as the sample. There was a good agreement between the results obtained by this method and those obtained from argentometric titration (Ag determination) and gravimetric method (Au determination).