Abstract：The sample was dissolved in hydrofluoric acid-nitric acid system. Excessive hydrofluoric acid in sample solution was neutralized with saturated boric acid solution. Based on the coloring reaction that dimethylglyoxim could react with nickel to form wine red complex, a determination method of nickel in zirconium and zirconium alloy was established with citric acid as complexing agent, iodine as oxidizing agent, and dimethylglyoxime as coloring agent. The effect of hydrofluoric acid dosage on the determination was emphatically investigated. The results showed that the following amount of hydrofluoric acid could ensure the complete dissolution of sample: 2.5mL of hydrofluoric acid was used when the sample mass was less than 1.0 g, and 5.0mL of hydrofluoric acid was used when the sample mass was 2.0g. The experimental conditions were optimized. Under the optimal experimental conditions, the mass fraction of nickel in range of 0.002%-0.15% was linear to its corresponding absorbance with the correlation coefficient of 0.9999. The detection limit of this method was 0.01μg/mL and the low limit of determination was 0.04μg/mL. The effect of zirconium matrix and coexisting elements on the determination of nickel was investigated. The results showed that the zirconium matrix and coexisting elements had no influence on the determination of nickel. The content of nickel in zirconium alloy certified reference material and four synthetic samples of zirconium and zirconium alloy were determined according to the experimental method. The results were basically consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES). The results of zirconium alloy certified reference material were consistent with the certified values. The relative standard deviation (RSD, n=11) of determination results were between 2.9% and 10.5%.
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