电感耦合等离子体发射光谱技术测定多金属伴生矿中钨钼铋两种消解方法的对比

党铭铭; 杨萍; 雷勇; 温智敏; 张碧兰

doi:10.15898/j.cnki.11-2131/td.202103050032

电感耦合等离子体发射光谱技术测定多金属伴生矿中钨钼铋两种消解方法的对比

Comparison of Two Different Sample Digestion Methods for Determination of Tungsten, Molybdenum, and Bismuth in Polymetallic Ore by Inductively Coupled Plasma-Optical Emission Spectrometry

摘要

摘要: 当前多金属伴生矿中钨钼铋元素的测定方法主要是传统的硫氰酸钾比色法和EDTA容量法，均为单元素分析，操作过程繁琐，分析效率低，检测周期长，难以满足大批量样品简便、快速的分析要求。本文改进了传统的单元素分析法，对比了盐酸-磷酸-高氯酸-硝酸四酸和盐酸-硝酸-高氯酸三酸两种消解体系，并结合电感耦合等离子体发射光谱法(ICP-OES)，建立了一种同时测定多金属伴生矿中钨、钼、铋的快速分析法。结果表明：合理引入磷酸的四酸消解法对样品的消解更为彻底，钨、钼、铋的测定结果准确度更高，各元素测定值和标准值的相对误差介于-5.36%~-1.39%，精密度较高(RSD ≤ 4.18%)，方法检出限介于0.0027%~0.0037%。本方法应用于分析湖南郴州某地区多金属伴生矿实际样品，各元素加标回收率介于95.0%~103.0%，各项技术指标均优于三酸消解法。本方法提高了分析效率，结果准确可靠，适用于多金属伴生矿样品中钨钼铋及其他主次量元素的批量检测。

Abstract:
BACKGROUNDCurrently, tungsten, molybdenum, and bismuth contents are mainly determined by the traditional potassium thiocyanate colorimetric method and EDTA volumetric method. These methods are based on single-element analysis, which has a complicated operation process, low analysis efficiency, and long detection cycle. It is difficult to meet the requirements of accurate and rapid determination of many samples.
OBJECTIVESTo improve the traditional single-element analysis method for the determination of tungsten, molybdenum, and bismuth in polymetallic ore.
METHODSA rapid method for the simultaneous determination of tungsten, molybdenum, and bismuth in the ore sample was developed by comparing the two digestion methods of HCl-H₃PO₄-HClO₄-HNO₃ and HCl-HClO₄-HNO₃, and was subsequently combined with inductively coupled plasma-optical emission spectrometry.
RESULTSTungsten, molybdenum, and bismuth in the sample were digested more thoroughly using the four-acid digestion method with a reasonable addition of phosphoric acid. The relative error between the determined and certified values of each element ranged from -5.36% to -1.39%, which indicated higher accuracy. The relative standard deviation was ≤ 4.18%, and the detection limits of the method ranged from 0.0027% to 0.0037%. The method was employed for the analysis of actual samples of the polymetallic ore from a certain area in Chenzhou, Hunan Province. The recovery of each element ranged from 95.0% to 103.0%. All the technical indexes were better than those of the three-acid digestion method.
CONCLUSIONSThe developed method significantly improved the analysis efficiency and gave accurate and reliable results. The method has been verified by actual samples and is suitable for batch detection of tungsten, molybdenum, bismuth, and other major and trace elements in the polymetallic ore samples.

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