Abstract: The study established volumetric method to determine nickel content in coarse gold.Through condition test,the minimum sample weight,the dosage of dimethylglyoxime to precipitate nickel and the manner of precipitate dissolution were determined.The RSD of the determination results is ＜2.00 %.The recovery rate of reference material is 98.05 %-100.38 %.The accuracy and precision are good.The method is suitable for batch determination of nickel content in coarse gold.