A study of the direct current and dtierentlal pulse polarographlc behavlour of metal complexes, especially nickel(H), of Arnpuxlhn and Amoxycdhn at the dropping mercury electrode, IS described In 1 M sodium acetate at pH 8 0, the mckel(II) complex IS supenor to those of cobalt(II), copper( and nndI1) m pmdmg dtierential pulse peaks which at -0 865 V and -0 840 V for Amplcdlm and Amoxycdlm respectwely anth respect to the Ag/AgCl, sat KCl reference electrode at 25"C, are well separated from those of excess metal ion Smtable workmg conditions of pH, lomc strength m sodium acetate supportmg electrolyte, temperature and time of measurement tier rmxlng of reactants were established for the mckel(II) systems As the temperature of reaction and measurement 1s increased, the dlfferentml pulse peak near -0 850 V decreases roughly exponentially with tune at t 25Β°C Tests showed that single electron reversible reduction occurs m the mckel(I1) complexes For quantitative determmatlon by the dtierential pulse techmque, linear calibration graphs were obtamed over concentration ranges 3 0 x 10e7 M to 3 0 x lo-' M and 4 0 X 10e7 M to 2 0 X lo-' M for Amplcdhn and Amoxycdhn, respectwely, ~th coefficients of vanatlon from 2 to 3% for 6 detennmatlons in the nuddle of the caliiratlon ranges Good agreement was found between results obtamed by the dlfferentlal pulse method and three methods from the Bnttlsh or US Pharmacopoelas