Carbon is determined in gold layers electroplated on brass, by deuteron activatin analysis using the12C/d, n/13N reaction. The results range from 2 to 1300 g.g–1 and the relative standard deviation from 0.9 to 13%. It is quantitatively shown that the hardness of the gold increases with the carbon concentration and that the carbon concentration decreases with increasing plating temperature and increases to a certain limit with the plating current density.