电感耦合等离子体发射光谱法测定地质样品中的钨、钼、锡

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Determination of W ，Mo，Sn in GCoupled Plasma-Atomiceological Samples by InductivelyEmission SpectrometryXIAO Liqing，TAN Lij uan ，SU Weihan ，DENG Shupei ，DENG Feiyue。

(1.Testing Center of Hunan Geological&Mining Research Institute for Non-Ferrous Metals，Changsha，Hunan 410015 China；2.College of Chemistry and Chemical Engineering，Central South University，Changsha，Hunan 410083 China)Abstract The sample digestion method used in simultaneous quantitative determination of W ，Mo and Snin polymetallic ore (one type of geological exploration samples) by inductively coupled plasma atomicemission spectrometry(ICP-AES)was improved in this article.A new sample digestion method，whichcombined acid desolution and alkaline fusion methods，was proposed.Samples were first dissolved by nitricacid.perchloric acid and hydrofluoric acid.Then the sample was leached with hydrochloric acid(1 1)followe by filtering.After the filtering residue and filter paper were ashed，the sample were digested withalkali fusion method.Finally，the determination of W ，Mo，Sn were accomplished using ICP-AES. Thenew sample digestion method overcomes the two major drawbacks existed in traditional acid sampledigestion and alkali fusion method，which are lower tin content problem in acid sample digestion methodand easy blockage of ICP-AES rectangular pipe and the atomizer often occurred in alkali fusion method。

The inductively coupled plasma-atomic emission spectrometry in conj unction with acid desolution alkalinefusion sample digestion method was validated using the national primary reference materials. Thevalidation results indicated that the precision and accuracy of the method can meet daily analysisrequirements。

Keywords acid digestion；alkali fusion；tungsten；molybdenum；tin；inductively coupled plasma atomicemission spectrometry收稿 日期 ：2012-12-20 修 回日期 ：2013-03-13作者简介 ：肖立青，男，在读研究生，主要从事岩石矿物分析研究。E-mail：782023351###qq.eori136 中国无机分析化学 2013经0 前言钨、钼、锡在自然界易共生或伴生形成多金属矿床，如钨钼矿、钨锡矿、钨钼铋锡萤石矿床等。全面了解化学成分 以及矿物组成 和赋存状态 ，对解决 多金属矿物的分离，取得较好的矿物回收率和经济技术指标至关重要 。相 当于投入-份地质勘查投资 ，却为国家找到了几个金属矿床1]。在地质勘探详查工作中，对岩石矿物样品化学成分分析时也-般需要同时化验钨、钼、锡三种元素。准确高效地测量钨、钼、锡的含量对地质勘查工作者研究分析成矿规律意义十分重大。对于高含量的锡，质量分数 为0.X 以上的矿样，大多采用容量法，如次亚磷酸钠还原-碘酸钾滴定法、铝片还原-碘量法；低含量的锡，质量分数为 0.000 2 ～0.2 ，采用比色法，最常用的是萃取分离，苯芴酮-CTMAB、苯基荧光酮等分光光度法 ]。对钨、钼 的分析，质量分数 叫<0.05 时，经常采用萃取-硫氰酸盐光度法3]、极谱法等。对于高含量的 WO。，质量分数为 0.X 以上的矿样，采用光度法，如硫氰酸盐光度法测定钨量。

这些方法实际应用时操作繁琐，效率低、耗时长，使用的有机试剂有毒、污染环境。电感耦合等离子体发射光谱法(ICP-AES)准确度高、精密度好、测定速度快、操作简单，已经在地质样品的测试中得到广泛应用l4 。在