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钽内标X射线荧光光谱法测定钨精矿中WO_3
引用本文:普旭力,王鸿辉,叶淑爱,董清木,朱桂容,王彩云,魏丽英.钽内标X射线荧光光谱法测定钨精矿中WO_3[J].分析试验室,2010,29(4).
作者姓名:普旭力  王鸿辉  叶淑爱  董清木  朱桂容  王彩云  魏丽英
作者单位:1. 厦门出入境检验检疫局,厦门,361012
2. 厦门钨业有限公司,厦门,361012
基金项目:国家质检总局重大课题(2008IK265);;厦门出入境检验检疫局课题(2007XK04)项目资助
摘    要:提出了以钽为内标波长色散X射线荧光光谱法测定钨精矿中WO3的新方法。以Na2B4O7和Li2B4O7(质量比65:35)的混合物作为熔剂,Ta2O5为内标,同时加入LiNO3为氧化剂,在1200℃下进行熔融制样,最后将本方法应用于实际样品的分析,结果表明,以钽作为内标测定WO3,不仅可以在很大程度上降低实验操作和仪器测量带来的偏差,也可以消除基体效应的影响。方法用于测定白钨精矿和黑钨精矿中WO3,其准确度和精密度优于重量分析法。

关 键 词:钨精矿  X射线荧光光谱法  内标法  熔融制样  

Determination of WO_3 in tungsten concentrate using tantalum internal standard X-ray fluorescence spectrometry
PU Xu-li,WANG Hong-hui,YE Shuai,DONG Qing-mu,ZHU Gui-rong,WANG Cai-yun,WEI Li-ying.Determination of WO_3 in tungsten concentrate using tantalum internal standard X-ray fluorescence spectrometry[J].Chinese Journal of Analysis Laboratory,2010,29(4).
Authors:PU Xu-li  WANG Hong-hui  YE Shuai  DONG Qing-mu  ZHU Gui-rong  WANG Cai-yun  WEI Li-ying
Institution:1.Xiamen Entry-Exit Inspection and Quarantine Bureau;Xiamen 361026;2.Xiamen Tungsten Co.Ltd.;Xiamen 361026
Abstract:A method has been developed for the X-ray fluorescence determination of WO_3 in tungsten concentrate. The samples are fused with mixture flux of sodium tetraborate and lithium tetraborate (65∶35) at 1200℃, and tantalum pentoxide was added as the internal standard. After cooling the cast bead, the W Lα and TaLα fluorescence emission intensity was determined by X-ray fluorescence spectrometry. The standard calibration beads were prepared with specpure tungsten trioxide. Tungsten contents of the samples are found by comparing the measured intensity ratio between sample beads and standard calibration beads. The experiment results show that with tantalum as the internal standard, not only the errors introduced by experimental operation and machine measurement can be depressed greatly, but also the matrix effect can be eliminated. The proposed method provides simple, rapid operation and high precision, and can be used for the determination of the tungsten content in both worfremite and scheelite accurately. The accuracy and precision of the method are found to be superior to those of the classical gravimetric method.
Keywords:Tungsten concentrate  X-ray fluorescence spectrometry  Internal standard  Fusion sampling  
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