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王蕾, 张保科, 马生凤, 赵怀颖, 郭琳. 封闭压力酸溶-电感耦合等离子体光谱法测定钨矿石中的钨[J]. 岩矿测试, 2014, 33(5): 661-664.
引用本文: 王蕾, 张保科, 马生凤, 赵怀颖, 郭琳. 封闭压力酸溶-电感耦合等离子体光谱法测定钨矿石中的钨[J]. 岩矿测试, 2014, 33(5): 661-664.
Lei WANG, Bao-ke ZHANG, Sheng-feng MA, Huai-ying ZHAO, Lin GUO. Determination of Wolfram in Tungsten Ore by Pressurized Acid Digestion-Inductively Coupled Plasma-Atomic Emission Spectrometry[J]. Rock and Mineral Analysis, 2014, 33(5): 661-664.
Citation: Lei WANG, Bao-ke ZHANG, Sheng-feng MA, Huai-ying ZHAO, Lin GUO. Determination of Wolfram in Tungsten Ore by Pressurized Acid Digestion-Inductively Coupled Plasma-Atomic Emission Spectrometry[J]. Rock and Mineral Analysis, 2014, 33(5): 661-664.

封闭压力酸溶-电感耦合等离子体光谱法测定钨矿石中的钨

Determination of Wolfram in Tungsten Ore by Pressurized Acid Digestion-Inductively Coupled Plasma-Atomic Emission Spectrometry

  • 摘要: 由于钨在酸性介质中极易发生水解生成水合三氧化钨,通常将钨矿石样品碱熔后采用重量法、光度法等传统方法进行测定,但这些方法操作繁琐,称样量较大(0.1~0.5 g)。本文采用封闭压力酸溶分解样品,钨矿石样品在170℃密闭20 h,然后迅速溶解于10%氢氟酸和5%浓硝酸的混合酸中,使钨形成稳定的易溶解的六价配合物,用耐氢氟酸进样系统的电感耦合等离子体光谱仪测定其中钨的含量,方法精密度为1.5%~6.4%(RSD,n=10),检出限为0.039~0.042 μg/g。方法经钨矿石国家标准物质验证,测定值与标准值一致;与分光光度法对照,测定结果吻合。本方法有效地解决了钨在酸性介质中极易水解的问题,溶样时间相对较短(20 h),无需进行赶酸、复溶等步骤,操作简单,可满足钨含量在0.015%~50%范围的钨矿石的日常分析要求。

     

    Abstract: Tungsten is prone to hydrolysis of hydrated tungsten oxide in acidic medium, so it is usually measured using traditional methods of weight method and spectrophotometry after alkaline fusion, which needs complex operation and large sampling size (0.1-0.5 g). A new method of analysis of tungsten ores has been established by using pressurized acid digestion and a hydrofluoric acid system for Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) and is described in this paper. Tungsten ores were effectively decomposed at 170℃ for 20 h, and then the samples were quickly dissolved in mixed acids of 5% hydrofluoric acid and 10% nitric acid. Tungsten in the form of the stable eutectic hexavalent complexes was determined by ICP-AES with a hydrofluoric acid resistant device. The detection limits of this method are 0.039-0.042 μg/g. Both the accuracy and precision of the method were validated by analyzing standard reference materials GBW 07240, GBW 07241, with 1.53%-6.42% (RSD, n=10). The results were in good agreement with the certified values of the national standard materials. This method can effectively solve the problems of tungsten hydrolysis easily in acidic medium. The operation is simple and has a relatively short digestion time of 20 h. The method can be used to analyze tungsten content in the range of 0.015%-50%.

     

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