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

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/m³,最低定量浓度为0.1 mg/m³,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。

Improvement of sample pretreatment for measurement of tin and its inorganic compounds in air of workplace

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/m³, and the lowest quantitative concentration 0.1 mg/m³. 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.