硝酸-氢氟酸酸溶电感耦合等离子体质谱法测定黑钨矿单矿物中稀土元素
Determination of Rare Earth Elements in Wolframite by Inductively Coupled Plasma-Mass Spectrometry with Nitric Acid-Hydrofluoric Acid Discomposition
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摘要: 黑钨矿单矿物通常混入铬、钙、镁、钴、钪和稀土等元素,属于富含稀土型矿物,准确测定黑钨矿中的稀土元素对判定黑钨矿矿床的成因相当重要。黑钨矿单矿物样品经硝酸-氢氟酸高压密闭溶解,蒸干除去氢氟酸,以硝酸提取使稀土元素进入溶液,钨则以钨酸的形式从溶液中沉淀而分离,采用电感耦合等离子体质谱法测定稀土元素的含量。用Rh、Re双内标校正,有效地降低了分析信号漂移对分析结果的影响;Ba对153Eu干扰、Pr、Ce对157Gd干扰,采用分析软件在线扣除。该方法消除了钨基体元素的干扰,复溶沉淀实验表明残留稀土相对量小于10%,稀土元素的测定值与过氧化钠碱熔法的结果相符。方法加标回收率为94.2%~104.0%,相对标准偏差小于10%,检出限小于0.026 μg/g。方法简便,准确度高,检出限低,适用于黑钨矿单矿物的分析。
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关键词:
- 黑钨矿 /
- 单矿物 /
- 稀土元素 /
- 酸溶 /
- 电感耦合等离子体质谱法
Abstract: Wolframite is the rare earth elements (REEs) bearing mineral and was mixed with Cr, Ca, Mg, Co, Sc and REEs. The accurate measurement of REEs in wolframite is very important to study ore forming in wolframite deposits. A method has been developed for the determination of REEs in wolframite by Inductively Coupled Plasma-Mass Spectrometry. Samples were dissolved by nitric acid-hydrofluoric acid in a sealed bomb under high pressure. The hydrofluoric acid was then evaporated. REEs were dissolved using nitric acid. Tungsten was precipitated from the solution in the form of tungstic acid and the matrix interference of the tungsten substrate was eliminated. By dissolving precipitation it was shown that the relative residual rare earth amount was less than 10%. The results of this method were consistent with the results by sodium peroxide melting. The double internal standards of Rh and Re were applied to reduce the effect by the drift of analytical signals. 153Eu and 157Gd had interferences from Eu, and the polyatomic ion interferences from Gd were calibrated using Ba, Pr and Ce oxides and hydroxides. The interferences from Eu and Gd were calibrated by using pure standard solutions of Ba, Pr and Ce with on-line analysis software. Recoveries ranged from 94.2%-104.0%, detection limits were less than 0.026 μg/g, and the relative standard deviations were better than 10% (n=10). The established method was simple and had a low detection limit with high accuracy.-
Keywords:
- wolframite /
- single /
- mineral /
- rare /
- earth
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杨道兴.用硫氰酸盐光度法测定钨铁、白钨铁、钨精矿中钨含量[J]. 冶金分析,2004,24(Z1): 311-313. 尹德媛,邓冬青.原子吸收光谱法测定钨精矿中的铅[J].光谱实验室,2008,25(6): 1116-1119. 普旭力,王鸿辉,叶淑爱,董清木,邹建龙,杨明坤.波长色散X射线荧光光谱法同时测定钨精矿中主次量组分[J].岩矿测试,2010,29(2):143-147. 王蕾,何红蓼,李冰.碱熔沉淀-等离子体质谱法测定地质样品中的多元素[J]. 岩矿测试,2003,22(2): 86-92. 岩石矿物分析编写组.岩石矿物分析(第四版) 第四分册[M].北京:地质出版社,2011: 317-334, 976-980. 刘湘生.电感耦合等离子体质谱法测定稀土元素的状况与展望[J].分析化学, 1995,23(10): 1218-1224. 曹心德,尹明,王晓蓉,赵贵文.微波消解-电感耦合等离子体质谱法测定土壤中微量稀土元素[J].分析化学,1999,27(6): 679-683. 艾军,胡圣虹,帅琴,余琼卫.预富集电感耦合等离子体质谱法测定地下水中超痕量稀土元素及钪、钇[J].分析化学,2002,10(2): 1226-1230. Liu H S, Wang N F, Xue B, Xu H E, Yan S M. Determination of ultra trace rare earth elements in biological samples by inductively coupled plasma mass spectrometry [J]. Journal of Chinese Mass Spectrometry Society, 2002,23(2): 96-98. Liu H S, Wang N F, Xue B, Xu H E, Yan S M. Determination of ultra trace rare earth elements in biological samples by inductively coupled plasma mass spectrometry [J]. Journal of Chinese Mass Spectrometry Society, 2002,23(2): 96-98.
李春颖.ICP-MS法测定地下水中稀土元素的研究[J].稀土,2007,28(6): 78-80. 李志伟,邰自安,任文岩,高志军,李艳华.微波消解电感耦合等离子体质谱法测定黑色页岩中稀有稀土元素[J].岩矿测试,2010,29(3):259-262 古丽冰,邵宏翔,陈铁梅.电感耦合等离子体质谱法测定商代原始瓷中的稀土[J].岩矿测试,2000,19(1): 70-72. 宋雪洁,刘欣丽,段太成,陈杭亭.电感耦合等离子体质谱法测定高纯氧化钕中的稀土杂质[J].分析化学,2009,37(12): 1743-1748. 姚剑敏,弓振斌,李云春,温裕云,李俊,汪霆.海洋生物体中稀土元素的微波消解电感耦合等离子体质谱测定研究[J].分析测试学报,2007,26(4): 473-478. 张玉学,刘义茂,高思登,何其光.钨矿物的稀土地球化学特征——矿床成因类型的判别标志[J].地球化学,1990,19(1): 11-20. 黄维新;黑钨矿单矿物中化学组份的多元统计分析及其地质意义[J].福州大学学报:自然科学版,1992,20(3): 123-128. [JP3]Fu Y,Wu C D,Guan P,Qu W J, Chen J F.Geochemistry of platinum group and rare earth elements of the polymetallic layer in the lower cambrian, Wengan, Guizhou Province[J].Acta Geologica Sinica, 2009,28(3): 618-627. [JP3]Fu Y,Wu C D,Guan P,Qu W J, Chen J F.Geochemistry of platinum group and rare earth elements of the polymetallic layer in the lower cambrian, Wengan, Guizhou Province[J].Acta Geologica Sinica, 2009,28(3): 618-627.
Cui Y C, Liu J H, Ren X W, Shi X F. Geochemistry of rare earth elements in cobalt-rich crusts from the Mid Pacific Seamount [J]. Journal of Rare Earths, 2009,27(1): 169-176. Cui Y C, Liu J H, Ren X W, Shi X F. Geochemistry of rare earth elements in cobalt-rich crusts from the Mid Pacific Seamount [J]. Journal of Rare Earths, 2009,27(1): 169-176.
黄慧萍,李艳玲,陶德刚,熊采华,方金东.电感耦合等离子体质谱法测定铬铁矿单矿物中痕量稀土元素[J].冶金分析,2005,25(6): 42-45. 李艳玲,熊采华,黄慧萍,陶德刚,方金东.基体分离-电感耦合等离子体质谱测定重晶石中超痕量稀土元素[J].岩矿测试,2005,24(2): 87-92. 黄冬根,廖世军,章新泉,童迎东ICP-MS法测定钨精矿中杂质元素[J].冶金分析,2005,25(2): 42-46.
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