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[目的]对GBZ/T 160.22《工作场所空气中锡及其化合物浓度的测定》中滤膜中锡的原子吸收光谱测定方法进行改进,建立快速、准确测定滤膜中锡的方法。并对滤膜中锡的测定结果进行不确定度评定。[方法]用3.0 m L盐酸和0.5 m L硝酸消解滤膜,火焰原子吸收法测定。并分析其测定不确定度的主要来源,按照JJF 1059.1—2012的有关规定对测定结果的不确定度进行评定。[结果]锡在0~60μg/m L范围内线性关系良好,相关系数r>0.999,方法的检出限为0.87μg/m L,加标回收率为100.8%~102.6%,相对标准偏差为1.5%~3.9%。不确定度的评定结果显示,测定结果的不确定度主要来源于样品前处理、标准溶液、标准曲线和仪器测定重复性等方面。[结论]改进后的方法稳定性及准确度均优于国标方法,更适用于滤膜中锡的含量测定。
[Objective] The research aimed to improve the method of determination of tin in the filter membrane by GBZ / T 160.22 “Determination of tin and its compounds concentration in workplace air”, and establish a rapid and accurate method for the determination of tin in the filter membrane. The uncertainty of the determination of tin in the filter was evaluated. [Method] The membrane was digested with 3.0 mL hydrochloric acid and 0.5 mL nitric acid and determined by flame atomic absorption spectrometry. And analyze the main sources of uncertainty in the measurement, according to the relevant provisions of JJF 1059.1-2012 on the determination of the uncertainty of the assessment. [Result] The calibration curve of tin in the range of 0-60 μg / m L was good with the correlation coefficient r> 0.999. The detection limit was 0.87 μg / m L and the recoveries were 100.8% -102.6%. The relative standard deviations 1.5% ~ 3.9%. Uncertainty assessment results show that the uncertainty of the measurement results mainly from the sample pretreatment, standard solution, the standard curve and the instrument to determine the repeatability and so on. [Conclusion] The stability and accuracy of the improved method are better than the national standard method, more suitable for the determination of tin content in the filter membrane.