石墨炉原子吸收光谱法测定锡铅焊料中铝
发布时间：2019-04-01 16:33
【摘要】：以硝酸(1+2)-盐酸(1+1)溶解样品,采用盐酸沉淀大部分铅及银,在16g/L柠檬酸、0.12mol/L盐酸介质中,取澄清液直接采用石墨炉原子吸收光谱法测定锡铅焊料中铝。结果表明:在选定的酸度介质中,不需要挥锡,锡也不会水解;大部分铅及银以氯化物形态沉淀于底部,无需用盐酸处理的脱脂棉-纸浆过滤分离银及铅沉淀,直接取澄清液进行测定即可;样品溶液保持清亮时间长,样品中锡及共存元素不干扰测定。方法线性范围为3.00~100.00μg/L,检出限为4.04μg/L。将方法应用于锡铅焊料标准物质中铝的测定,结果与认定值或GB/T10574.13—2003采用的电感耦合等离子体原子发射光谱法(ICP-AES)一致,相对标准偏差为6.2%~8.9%。
[Abstract]:The samples were dissolved with nitric acid (1 + 2)-hydrochloric acid (1 + 1), most of the lead and silver were precipitated by hydrochloric acid, and in the medium of 16 g/ L of citric acid and 0.12 mol/ L hydrochloric acid, the aluminum in the tin-lead solder was determined by the method of graphite furnace atomic absorption spectrometry. The results show that, in the selected acidity medium, tin and tin are not needed to be hydrolyzed, most of the lead and silver are precipitated on the bottom in a chloride form, and the silver and lead precipitation is not required to be separated by the non-absorbent cotton-paper pulp treated with hydrochloric acid, and the clear liquid can be directly taken for measurement; The sample solution is kept clear for a long time, and the tin and coexistent elements in the sample do not interfere with the measurement. The linear range of the method is 3.00-100.00. m u.g/ L and the detection limit is 4.04. m u.g/ L. The method is applied to the determination of the aluminum in the standard substance of the tin lead solder, and the result is consistent with the determination value or the inductively coupled plasma atomic emission spectroscopy (ICP-AES) adopted in GB/ T10574.13-2003, and the relative standard deviation is 6.2%-8.9%.
【作者单位】： 云南锡业集团公司研究设计院;
【分类号】：TG42;O657.31
[Abstract]:The samples were dissolved with nitric acid (1 + 2)-hydrochloric acid (1 + 1), most of the lead and silver were precipitated by hydrochloric acid, and in the medium of 16 g/ L of citric acid and 0.12 mol/ L hydrochloric acid, the aluminum in the tin-lead solder was determined by the method of graphite furnace atomic absorption spectrometry. The results show that, in the selected acidity medium, tin and tin are not needed to be hydrolyzed, most of the lead and silver are precipitated on the bottom in a chloride form, and the silver and lead precipitation is not required to be separated by the non-absorbent cotton-paper pulp treated with hydrochloric acid, and the clear liquid can be directly taken for measurement; The sample solution is kept clear for a long time, and the tin and coexistent elements in the sample do not interfere with the measurement. The linear range of the method is 3.00-100.00. m u.g/ L and the detection limit is 4.04. m u.g/ L. The method is applied to the determination of the aluminum in the standard substance of the tin lead solder, and the result is consistent with the determination value or the inductively coupled plasma atomic emission spectroscopy (ICP-AES) adopted in GB/ T10574.13-2003, and the relative standard deviation is 6.2%-8.9%.
【作者单位】： 云南锡业集团公司研究设计院;
【分类号】：TG42;O657.31
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