采用HNO_3、HF和H_2SO_4溶解矿石样品,在6 mol/L HCl的介质中以乙酸丁酯萃取氯化镓,再加入适量的水从乙酸丁酯中反萃取氯化镓,从而富集痕量镓并使镓与其它干扰元素分离,在波长294.364{114}nm处以电感耦合等离子体原子发射光谱法测定了样液中的镓.对萃取机理、萃取分离技术、干扰元素的消除进行了探讨,并对仪器参数进行了优化.溶液中镓原子发射光谱强度与p(Ga)在0～3μg/mL范围内呈良好的线性关系,校准曲线相关系数为0.999 9,方法检出限为0.052μg/mL.用本方法测定了标准物质中镓的含量,测定值与认定值吻合,相对标准偏差(n=6)为0.85%～1.9%.
Mineral sample was dissolved in HNO_3, HF and H_2SO_4, and gallium trichloride was extracted with n-butyl acetate in 6 mol/L HCl. Then, gallium trichloride was back extracted with water in n-butyl acetate, so that trace amounts of gallium could be enriched and separated from other elements which might interfere with the detection. By inductively coupled plasma atomic emission spectrometry, the content of gallium in the sample was determined at the wavelength of 294.364{114} nm. The mechanism of extraction, technology of extraction and seperation, and elimination of disturbing elements were discussed. The instrument parameters were optimized. There was a good linear relationship between emission intensity of gallium and mass concentration of Ga in the range of 0-3 μg/mL. The correlation coefficient of calibration curve was 0.999 9, and the detection limit of this method was 0.052 μg/mL. The content of gallium in certified reference materials was determined by this method and the results were consistent with the certified values with a relative standard deviation(n = 6)between 0.85%-1.9%.
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