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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. DOI: 10.15898/j.cnki.11-2131/td.201804190047
引用本文: 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. DOI: 10.15898/j.cnki.11-2131/td.201804190047
Sheng-feng MA, Wen-bo ZHAO, Yun ZHU, Hong-bin SUN, Lei WANG, Hong-li WEN. 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
Citation: Sheng-feng MA, Wen-bo ZHAO, Yun ZHU, Hong-bin SUN, Lei WANG, Hong-li WEN. 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

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

  • 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。

     

    Abstract:
    BACKGROUNDTin 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.
    OBJECTIVESTo decompose the tin ore completely, and accurately determine the symbiotic and associated trace elements in ore.
    METHODSHydrogen 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.
    RESULTSThe 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%.
    CONCLUSIONSThe 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.

     

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