介绍了一种固体发射光谱法测定地球化学样品中高含量锡的分析方法。 研制了一套专用高含量锡光谱标准系列, 以K2S2O7, NaF, Al2O3, 碳粉为缓冲剂, Ge为内标, 样品、 基物、 缓冲剂比例为1∶1∶2。 以弱灵敏线(Sn 242.170 0 nm)作为分析线, 采用垂直电极法, 交流电弧重叠摄谱, 截取曝光, 计算机定量译谱, 同时扣除分析线和内标线背景。 方法测定范围为: 100～22 350 μg·g-1, 检出限为: 16.64 μg·g-1, 精密度为(RSD, n=12): 4.11%～6.46%。 测定了国家一级标准物质, 结果与认定值符合。 本方法可不用稀释直接测定地球化学样品中的高含量锡, 提高了固体发射光谱法测定锡的检出上限, 具有一定的实用价值。

A method for the determination of high content of tin in geochemical samples by solid emission spectrometry was presented. The dedicated high content tin spectrum standard series was developed. K2S2O7, NaF, Al2O3 and carbon powder were used as buffers and Ge was used as internal standard, and the ratio of sample/matrix/buffer is 1∶1∶2. A weak sensitive line (Sn 242.170 0 nm) was used as the analytical line. The technologies of vertical electrodes, AC arc overlap spectrograph, interception of the exposure, quantitative computer translation spectrum and background correction were used. The determination range is 100~22 350 μg·g-1, the detection limit is 16.64 μg·g-1, and the precision is (RSD, n=12) 4.11%~6.46%. The accuracy of the method has been verified by determination of high content of tin in national geochemical standard samples and the results are in agreement with certified value. The method can be used for measurement directly without dilution of high content of tin in geochemical samples, and it greatly improved the detection upper limit for the determination of tin with solid emission spectroscopy and has certain practical value.