The concentration of Co in a sulfamate Ni plating bath is determined by adsorptive stripping voltammetry (AdSV) inammonia buffer pH 9.6 with dimethylglyoxime (DMG) as complexing agent. All reagents have to be added in the order listed below. Special care has to be taken that the measuring solution is mixed well before the complexing agent is added. In case of precipitations of Ni-DMG further dilution of the sample is necessary.