Department of Chemistry, Presidency College, Calcutta (India.) Manuscript received 31 July 1978, revised 6 November 1979, accepted 9 September 1980 A rapid method for the amperometric determination of Ag(I), Au(III), Hg(II) and Pd(Il) with thiosalicylamide at the rotatiog platinum electrode has been developed. Thus, 0.409 to 3.191 mg Ag(0.252-1.960 mM), 0.085 to 4.275 mg Au(0.0216- 1.080 mM), 0.420 to 6.970 mg Hg(0.131-2.170 mM) and 0.071 to 1.860 mg Pd(0.0475- 1.240 mM) are amperometrically determined in acid medium using thiosalicylamide as a complexing agent. All the four metals are determined in presence of large number of diverse ions, e.g., Cd(II), Zn(II), Pb(II), Mn(II), Ni(II), Co(II), Cr(III), Fe(III), AI(III), As(lll), Sb(lll), Bi(lll), V(V), Zr(IV), etc. The relative mean errors in the determination of Ag, Au, Hg and Pd are found to be 0.078%, 0.935%, 1.362% and 0.434% respectively. The voltammetry of thiosalicylamide at a rotating platinum electrode is also investigated.