工作场所空气中锡及其无机化合物样品预处理方法的改进

Improvement of the Preprocessing Method for Tin and Its Inorganic Compounds in the Air of Workplace

目的对工作场所空气中锡及其无机化合物样品的预处理方法进行改进。方法样品置于10mL比色管中,加入1 mL浓盐酸置于90℃管式电热消解仪加热10～15min,取下放冷用去离子水定容至10mL经浓盐酸消化后,采用原子吸收分光光度计或原子荧光分光光度计进行测定。结果原子荧光分光光度计法在0.1～300μg/L浓度范围内线性关系良好,相关系数r=0.9996;检出限和定量下限分别为0.46μg/L和0.78μg/L,加标平均回收率为99%～102%;批内精密度为1.6%～2.98%;批间精密度为3.3%～5.5%。原子吸收分光光度计法在5～200μg/mL浓度范围内线性关系良好,相关系数r=0.9998;加标平均回收率为97%～101%;批内精密度为1.0%～1.5%;批间精密度为3.1%～5.5%。两方法对样品检测结果无显著性差异。结论两种方法均适用于工作场所空气中锡及其无机化合物的测定。

Objectives To improve the preprocessing method for tin and its inorganic compounds in the air of workplace. Methods Tin and its inorganic compounds in the air of workplace were collected by filter membrane, a sample was placed in a 10 mL co[orimetric tube, 1 mL concentrated hydrochloric acid was added and the tube was heated at 90℃ for 10 - 15 min, and then diluted with deionized water after cooling. Atomic absorption spectrophotometer （AAS） or atomic fluorescence spectrophotometer （AFS） was used for the detection of tin and its inorganic compounds in the solution. Results The linearity of AFS was good at the range of 0. 1 - 300 μg/L with a correlation coefficient of 0. 9996; the LOD and LOQ were 0.46 μg/L and 0.78 μg/L,＇respectively. The recovery was ranged from 99% to 102% , the RSD of intra-and inter-batch precision were 1.6% - 2.98% and 3.3% - 5.5% , respectively. The linearity of AAS was good at the range of 5 - 200 μg/mL with a correlation coefficient of 0. 9998. The recovery was ranged from 97% to 101% , the RSD of intra- and inter-batch precision were 1.0% - 1.5% and 3.1% -5.5% , respectively. Conclusions The linear range, sensitivity and precision of both methods were suitable for the detection of tin and its inorganic compounds in the air of workplace.