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A rapid and precise method of determining traces of nickel in foods and biological materials and in ferrous materials has been developed.The optimum range is 5 to 80 micrograms and in this range the determinations are accurate to *5%. Nickel is separated from interfering dements by a solvent extraction of the dimethylglyoxime salt of divalent nickel, and is determined by spectrophotometric measurement of the yellow diethyldithiocarbamate complex.