Differential pulse polarography (DPP) can be successfully13; employed for the simultaneous determination of palladium and nickel in electroplating baths. Both palladium and nickel give peaks in ammonical chloride and ammonical tartrate media which are seperated by about 250 mV. When the nickel to palladium ratio exceeds 100, EDTA may be added to complex nickel and thus remove the interference13; due to excess nickel. In the the presence of large amounts of palladium, dimethyl glyoxime is used to enhance the peak current of nickel, the palladium peak in ammonium chloride buffer at pH 9.0 is not affected by the presence of either EDTA or dimenthly glyoxime. Thus it is possible to dterminepalladium and nickle simultaneouisly and in the presence of excess of each other.