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研究了HCl-HBr排除锡基体、火焰原子吸收光谱法测定无铅锡基焊料中镍的分析方法,确定了测定镍的各项条件。进行试样分解试验,考察了锡、银、铜、铋、锌、锑等主要成分的干扰情况,找到了消除干扰的方法。在优化的实验条件下,镍量在0.05～5.0μg/mL范围内服从比尔定律,方法的检出限为0.014μg/mL。对5个样品进行测定的加标回收率在93.8%～102.5%之间,相对标准偏差为1.2%～7.6%之间。采用HCl、H2O2、HNO3溶解试样,以HCl-HBr排除大量Sn,在稀HNO3介质中,使用空气-乙炔火焰,于原子吸收光谱仪波长232.0nm处,测定了无铅锡基焊料中5.0×10-4%～1.0%Ni含量。
The analytical method for the determination of nickel in lead-free tin-based solder by HCl-HBr exclusion tin matrix and flame atomic absorption spectrometry was studied, and the conditions for nickel determination were determined. The sample decomposition test was carried out to investigate the interference of the main components of tin, silver, copper, bismuth, zinc and antimony, and the method of eliminating interference was found. Beer ’s law was obeyed in the range of 0.05-5.0 μg / mL under the optimal experimental conditions. The detection limit was 0.014 μg / mL. The spiked recoveries of five samples ranged from 93.8% to 102.5% and the relative standard deviations (RSDs) ranged from 1.2% to 7.6%. The sample was dissolved with HCl, H2O2 and HNO3, a large amount of Sn was eliminated with HCl-HBr, air-acetylene flame was used in dilute HNO3 medium, and at the wavelength of 232.0nm of the atomic absorption spectrometer, 5.0 × 10 -4% to 1.0% Ni content.