岩矿测试

文章摘要

马生凤,赵文博,朱云,孙红宾,王蕾,温宏利.碘化氨除锡后封闭酸溶-电感耦合等离子体质谱测定锡矿石中的共生和伴生元素[J].岩矿测试,2018,37(6):650-656

MA Sheng-feng,ZHAO Wen-bo,ZHU Yun,SUN Hong-bin,WANG Lei,WEN Hong-li.Determination of Symbiotic and Associated Elements in Tin Ore by ICP-MS Combined with Pressurized Acid Digestion and Detinning Process[J].Rock and Mineral Analysis,2018,37(6):650-656.DOI:10.15898/j.cnki.11-2131/td.201804190047

碘化氨除锡后封闭酸溶-电感耦合等离子体质谱测定锡矿石中的共生和伴生元素

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Determination of Symbiotic and Associated Elements in Tin Ore by ICP-MS Combined with Pressurized Acid Digestion and Detinning Process

投稿时间：2018-04-19 修订日期：2018-06-12

DOI：10.15898/j.cnki.11-2131/td.201804190047

中文关键词: 锡石金属元素除锡率碘化铵电感耦合等离子体质谱法

英文关键词: tin ore metallic element the removal rate of tin ammonium iodide Inductively Coupled Plasma-Mass Spectrometry

基金项目:国家重点研发计划“国家质量基础的共性技术研究与应用”重点专项课题（2016YFF0201604-3）

作者	单位
马生凤	国家地质实验测试中心, 北京 100037
赵文博	国家地质实验测试中心, 北京 100037
朱云	国家地质实验测试中心, 北京 100037
孙红宾	国家地质实验测试中心, 北京 100037
王蕾	国家地质实验测试中心, 北京 100037
温宏利	国家地质实验测试中心, 北京 100037

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中文摘要:

锡矿石是难分解的矿物，主要存在形式是锡石（SnO₂），且共生和伴生元素多，常用的酸溶方法几乎不能溶解SnO₂，从而给锡矿石中的共生与伴生元素的准确测定带来困难。本文基于碘化氨在较低温度下熔融可产生无水状态的碘化氢，利用碘化氢的酸性和氨的还原性分解SnO₂，使Sn呈SnI₄升华分离的原理处理锡矿石。实验中以高纯铂丝作催化剂，加入碘化铵在450℃的马弗炉中分解锡矿石30 min，使得Sn以SnI₄形式挥发，除锡率达到98%以上，再用2 mL氢氟酸和1 mL硝酸封闭溶解残渣，电感耦合等离子体质谱测定钴镍铜铌钽钍铀等24个共生和伴生元素。元素检出限在0.001~2.9 μg/g之间，90%以上元素的相对标准偏差（RSD）小于5%，相对误差小于10%。本方法解决了锡矿石难分解的问题，可测定共存金属元素，也适合测定Sn含量在1.27%~62.49%之间的锡矿石中的微量和痕量元素及锡精矿中的微量元素。

英文摘要:

BACKGROUND: Tin ore is a hard-to-decompose mineral. The main form is cassiterite (SnO₂), and there are many symbiotic and associated elements. The commonly used acid-digestion method can barely dissolve SnO₂, making it difficult for accurate measurement of symbiotic and associated elements in tin ore.
OBJECTIVES: To decompose the tin ore completely, and accurately determine the symbiotic and associated trace elements in ore.
METHODS: Hydrogen iodide can be produced in a non-aqueous state during the melting of ammonium iodide at a lower temperature, and the acidity of hydrogen iodide and the reductive decomposition of SnO₂ by ammonia, and Sn separation by the sublimation of SnI₄ which is the basis of the study. Under the catalysis of a high purity platinum, ammonium iodide was used to decompose cassiterite for 30 minutes in a Maffer furnace at 450℃. Tin was removed in the form of SnI₄ with a removal rate of 98%. The residue was dissolved by 2 mL HF and 1 mL HNO₃ using pressurized acid digestion. Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) was used to accurately determine 24 elements in tin ore.
RESULTS: The element detection limits are from 0.001 to 2.9 μg/g, and more than 90% of the elements have a relative standard deviation (RSD) of less than 5%. The relative error is less than 10%.
CONCLUSIONS: The method solves the problem of tin ore being difficult to decompose, can measure the coexisting metal elements, and is also suitable for determining trace and ultra-trace elements in tin ore with Sn contents between 1.27% and 62.49% and trace elements in tin concentrate.

主管单位：	中国科学技术协会
主办单位：	中国地质学会岩矿测试技术专业委员会国家地质实验测试中心