偏硼酸锂熔融-电感耦合等离子体发射光谱法测定钨钼矿石中钨钼及11种伴生元素

王力强; 王家松; 魏双; 郑智慷; 吴良英; 张楠; 曾江萍

doi:10.15898/j.cnki.11-2131/td.202103190040

偏硼酸锂熔融-电感耦合等离子体发射光谱法测定钨钼矿石中钨钼及11种伴生元素

Determination of W, Mo and 11 Other Elements in Tungsten-Molybdenum Ores by Inductively Coupled Plasma Optical Emission Spectrometry with Lithium Metaborate Fusion

摘要

摘要: 钨钼矿石是重要的战略性矿产资源，中国是钨钼矿的产出和消费大国，准确、高效地分析钨钼及其共伴生的有益有害元素含量对钨钼矿的矿床评价和综合利用有重要意义。钨钼矿石中钨钼及伴生元素的分析目前主要采用酸溶和碱熔方式消解样品，酸溶方式在处理高钨钼样品时无法克服水解问题，过氧化钠、氢氧化钠等碱熔方式通常会引入大量碱金属，不能完成钾钠的测定。本文建立了一种偏硼酸锂熔融，盐酸-酒石酸超声浸取，电感耦合等离子体发射光谱（ICP-OES）同时测定钨钼矿石中钨钼铜铅锌铝铁钙镁钛锰钾钠的方法。利用偏硼酸锂熔融的强解离作用使样品完全分解，溶液除硼锂外不引入其他金属元素，在盐酸提取液中加入酒石酸络合能够有效抑制钨钼水解，经超声浸取加快了熔块溶解。实验优化了各元素的分析谱线和观测方式，对熔剂用量以及仪器条件进行对比实验以获得最佳条件，采用基体匹配法绘制标准曲线消除了基体效应的影响。标准曲线线性相关系数均大于0.9990，方法检出限为1.34~46.2μg/g，标准物质测定结果的相对误差为0.14%~8.7%，相对标准偏差（RSD，n=10）为1.4%~7.6%。该方法能够准确、高效地完成钨钼矿石样品中多元素的同时测定。

Abstract:
BACKGROUNDTungsten molybdenum ores are strategic mineral resources. China is a large producer and consumer of tungsten and molybdenum ore. Accurate and efficient analysis of tungsten and molybdenum and its associated beneficial and harmful elements is of great significance for the evaluation and comprehensive utilization of tungsten and molybdenum ore deposits. Acid dissolution and alkali fusion are the general digestion methods in tungsten molybdenum ore analysis. However, the acid solution method cannot be used to overcome the hydrolysis problem when treating samples with high content of tungsten and molybdenum, whereas the alkali fusion method such as sodium peroxide and sodium hydroxide usually introduces a large content of alkali metals, so the determination of potassium and sodium cannot be finished.
OBJECTIVESTo find an efficient method for the determination of tungsten, molybdenum and 11 other elements in tungsten molybdenum ore.
METHODSLithium metaborate melting-tartaric acid ultrasonic leaching and inductively coupled plasma-optical emission spectrometry (ICP-OES) was used for the simultaneous determination of tungsten, molybdenum, copper, lead, zinc, aluminum, iron, calcium, magnesium, titanium, manganese, potassium and sodium in tungsten-molybdenum ore. The sample was completely digested by lithium metaborate fusion. No other elements were introduced except for B and Li. Tartaric acid was used to inhibit the hydrolysis of tungsten and molybdenum. Ultrasonic leaching speeds up the dissolution of the frit.
RESULTSThe experiment optimized the analysis spectrum and observation method of each element, compared the amount of flux and instrument conditions to obtain the best conditions, and used the matrix matching method to draw a standard curve to eliminate the influence of the matrix effect. The linear correlation coefficient of the standard curve of each element was greater than 0.9990, the detection limit of the method was 1.34-46.2μg/g, the relative error of measured results was 0.14%-8.7%, the relative standard deviation (RSD, n=10) of the measured results was 1.4%-7.6%.
CONCLUSIONSThis method can accurately and efficiently complete the simultaneous determination of multiple elements in tungsten and molybdenum ore samples.

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