火焰原子吸收光谱法测定无铅锡基焊料中镍

Study on the determination of nickel in lead-free tin-based solder by flame atomic absorption special invited review

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。

A method for the determination of nickel in lead-free tin-based solder by flame atomic absorption spectrometry based on the tin-based eliminated by hydrochloric acid and bromic acid was investigated,and the rarious factors influencing the determination were optimized.The interference of the main components such as tin,silver,copper,bismuth,zinc,antimony were also studied through the experiment of decomposing samples,and a method to eliminate the interference was developed.The nickel in the concentration range of 0.05 to 5.0μg/mL obeys Beer＇s Law under the optimized conditions,and the detection limit of the method was 0.014μg/mL.Through the determination of five samples,the relative standard deviations were in the range of 1.2% to 7.6%,while the recoveries of standard addition were in the range of 93.8% to 102.5%.The samples were digested by hydrochloric acid,hydrogen peroxide and nitric acid,in while the main components of tin-based were eliminated by hydrochloric acid with bromic acid.In the nitric acid solution,the nickel in lead-free tin-based solder between 5.0×10-4% and 1.0% was determined at the wavelength of 232.0nm by air-acetylene flame with satisfactory results.