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利用样品处理过程中,试液加入内标混匀后不需精确定容的特点,通过过滤分离沉淀、减少基体影响,采用硝酸酸化、避免氯离子干扰进行方法改进。样品经氢氧化钠熔融,热水提取,过滤分离沉淀,硝酸酸化后加入铑内标,粗略定容,电感耦合等离子体质谱仪测定,建立了一套快速、准确、批量测定地球化学样品中锡的方法。该方法经国家一级标准物质验证,分析结果与标准值吻合,相对标准偏差(RSD,n=6)落在4.8%~9.6%之间,方法检出限为锡:0.27μg/g。该方法操作简单、快速、易于掌握,线性范围宽,准确度和精密度均能满足地质找矿需要,已成功应用于本中心大批量地球化学样品锡元素的测定。
In the process of sample processing, the test solution is mixed with an internal standard solution without the need of precise volumetric content. The precipitate is separated by filtration to reduce the influence of the matrix, and nitric acid is used for acidification to avoid the interference of chloride ions. The sample was dissolved in sodium hydroxide, hot water was extracted, the precipitate was separated by filtration, nitric acid was added rhodium internal standard, rough volume, inductively coupled plasma mass spectrometry determination, established a set of rapid, accurate, batch determination of geochemical samples of tin Methods. The method was validated by the national standard reference materials. The analytical results were consistent with the standard values. The relative standard deviations (RSDs, n = 6) fell between 4.8% and 9.6%. The detection limit was 0.27μg / g. The method is simple, rapid and easy to grasp. The linear range, accuracy and precision can meet the geological prospecting requirements. The method has been successfully applied to the determination of tin in high-volume geochemical samples.