工作场所空气中锡及其无机化合物测定样品前处理方法的改进
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摘要
目的对样品前处理方法进行改进,建立火焰原子吸收光谱法快速、准确测定滤膜中锡及其无机化合物的样品前处理方法。方法本法使用1 ml浓盐酸比色管加塞60℃水浴30 min消化样品,消化后样品溶液用去离子水定容至10 ml。结果锡浓度0.0～160.0 mg/L范围内线性关系良好,相关系数r=0.999 9(n=6),检出限为0.3 mg/L,定量下限为1.0 mg/L,样品最低检出浓度为0.03 mg/m~3,最低定量浓度为0.1 mg/m~3,加标回收率为98.5%～99.5%,批内相对标准偏差(RSD)为0.9%～1.5%,批间RSD为0.9%～2.3%。对锡质控样进行测试,结果符合要求。结论利用本样品前处理方法测定滤膜中锡及其无机化合物,方法简便,精密度、准确度高,结果满意。
Objective To improve the sample pretreatment method, then to establish a sample pretreatment method for rapid and accurate determination of tin and its inorganic compounds in filter membrane by flame atomic absorption spectrometry. Methods The samples were digested with 1 ml concentrated colorimetric by tubes, then heated in water-bath at 60 ℃ for 30 min. After digestion, the sample solution was fixed to 10 ml with deionized water. Results The method showed that a good linear relationship was obtained in the range of 0.0-160.0 mg/L, and the correlation coefficient was 0.999,9(n=6). The detection limit was 0.3 mg/L and the lower limit of quantitation was 1.0 mg/L. The lowest detection concentration was 0.03 mg/m~3, and the lowest quantitative concentration 0.1 mg/m~3. The recoveries were 98.5%-99.5%. The within-run relative standard deviation(RSD) ranged from 0.9% to 1.5%, and the between-run RSD from 0.9% to 2.3%. The tin quality control samples were tested, and the results met the requirements. Conclusions The improved method with new sample pretreatment procedure is simple, precise and accurate for the determination of tin and its inorganic compounds in the filter membrane, and the result is satisfactory.
Objective To improve the sample pretreatment method, then to establish a sample pretreatment method for rapid and accurate determination of tin and its inorganic compounds in filter membrane by flame atomic absorption spectrometry. Methods The samples were digested with 1 ml concentrated colorimetric by tubes, then heated in water-bath at 60 ℃ for 30 min. After digestion, the sample solution was fixed to 10 ml with deionized water. Results The method showed that a good linear relationship was obtained in the range of 0.0-160.0 mg/L, and the correlation coefficient was 0.999,9(n=6). The detection limit was 0.3 mg/L and the lower limit of quantitation was 1.0 mg/L. The lowest detection concentration was 0.03 mg/m~3, and the lowest quantitative concentration 0.1 mg/m~3. The recoveries were 98.5%-99.5%. The within-run relative standard deviation(RSD) ranged from 0.9% to 1.5%, and the between-run RSD from 0.9% to 2.3%. The tin quality control samples were tested, and the results met the requirements. Conclusions The improved method with new sample pretreatment procedure is simple, precise and accurate for the determination of tin and its inorganic compounds in the filter membrane, and the result is satisfactory.
引文
[1]应英,汤鋆,冯靓,等.原子吸收法测定滤膜中锡的方法学研究[J].中国卫生检验杂志,2011,21(3):2181-2182.
[2]高俊敏,建英,郑泽根.有机锡的人体暴露分析[J].环境与健康杂志,2005,22(1):72-75.
[3]蒋光愉,韦树娇,李小萍,等.有色金属锡粉尘致实验动物肺损伤的病理观察[J].中华劳动卫生职业病杂志,2012,30(8):561-566.
[4]汤利民,肖雄斌,何卫红,等.一起急性有机锡职业中毒事故的调查[J].实用预防医学,2008,15(4):1131.
[5]中华人民共和国卫生部. GBZ/T160. 22-2004工作场所空气有毒物质测定锡及其化合物[S].北京:人民卫生出版社,2004:1-2.
[6]郭晓婧,郭佳明,梁嘉斌,等.滤膜中锡样品原子吸收测定法前处理方法改进研究[J].职业卫生与应急救援,2015,33(4):238-239,256.
[7]宋臻鹏.火焰原子吸收法对滤膜中锡及其化合物测定的探讨[J].中国卫生检验杂志,2013,23(5):1094-1095.
[8]姚浔平,姚珊珊,王立.滤膜中锡测定方法的改进及不确定度评定[J].环境与职业医学,2015,32(4):370-372,378.
[9]中华人民共和国卫生部. GBZ/T 210. 4-2008职业卫生标准制定指南第4部分:工作场所空气中化学物质测定方法[S].北京:人民卫生出版社,2008:1-10.
[10]中华人民共和国国家卫生和计划生育委员会. GBZ/T 300. 26-2017工作场所空气有毒物质测定锡及其无机化合物[S].北京:人民卫生出版社,2018:1-7.
[11]黄峰,王红琴.火焰原子吸收法对滤膜中锡及其化合物的测定[J].中国卫生检验杂志,2015,25(3):789-790.
[12]郝恩,金凤,白慧芝,等.滤膜中锡测定样品处理方法的改进[J].中国卫生检验杂志,2011,21(5):1094-1095.
[2]高俊敏,建英,郑泽根.有机锡的人体暴露分析[J].环境与健康杂志,2005,22(1):72-75.
[3]蒋光愉,韦树娇,李小萍,等.有色金属锡粉尘致实验动物肺损伤的病理观察[J].中华劳动卫生职业病杂志,2012,30(8):561-566.
[4]汤利民,肖雄斌,何卫红,等.一起急性有机锡职业中毒事故的调查[J].实用预防医学,2008,15(4):1131.
[5]中华人民共和国卫生部. GBZ/T160. 22-2004工作场所空气有毒物质测定锡及其化合物[S].北京:人民卫生出版社,2004:1-2.
[6]郭晓婧,郭佳明,梁嘉斌,等.滤膜中锡样品原子吸收测定法前处理方法改进研究[J].职业卫生与应急救援,2015,33(4):238-239,256.
[7]宋臻鹏.火焰原子吸收法对滤膜中锡及其化合物测定的探讨[J].中国卫生检验杂志,2013,23(5):1094-1095.
[8]姚浔平,姚珊珊,王立.滤膜中锡测定方法的改进及不确定度评定[J].环境与职业医学,2015,32(4):370-372,378.
[9]中华人民共和国卫生部. GBZ/T 210. 4-2008职业卫生标准制定指南第4部分:工作场所空气中化学物质测定方法[S].北京:人民卫生出版社,2008:1-10.
[10]中华人民共和国国家卫生和计划生育委员会. GBZ/T 300. 26-2017工作场所空气有毒物质测定锡及其无机化合物[S].北京:人民卫生出版社,2018:1-7.
[11]黄峰,王红琴.火焰原子吸收法对滤膜中锡及其化合物的测定[J].中国卫生检验杂志,2015,25(3):789-790.
[12]郝恩,金凤,白慧芝,等.滤膜中锡测定样品处理方法的改进[J].中国卫生检验杂志,2011,21(5):1094-1095.