岩矿测试2025，Vol.44Issue(6)：1156-1165,10.DOI:10.15898/j.ykcs.202503270061
硝酸-氢氟酸微波消解-电感耦合等离子体发射光谱法测定钨钼矿石中钨钼铜锌
Determination of W,Mo,Cu and Zn in Tungsten-Molybdenum Ores by Inductively Coupled Plasma-Optical Emission Spectrometry after Microwave Digestion with Nitric Acid-Hydrofluoric Acid
摘要
Abstract
Tungsten-molybdenum ore represents a crucial and valuable mineral resource in China,characterized by its abundant associated elements.Accurate and rapid analysis of key elements(W,Mo)and associated elements(Cu,Zn)holds significant importance for the exploitation and sustainable development of tungsten-molybdenum ore deposits.In acidic environments,W and Mo are prone to hydrolysis.Current national and industry standard analytical methods for tungsten-molybdenum ores predominantly employ alkali fusion for sample pretreatment.While alkali fusion effectively suppresses hydrolysis,it introduces alkali metal matrices that may interfere with the analytical instrument's precision and potentially elevate the lower detection limit.In this work,a microwave digestion method was developed using a mixed acid system of nitric acid and hydrofluoric acid.Samples were digested at 180℃for 45min and were directly dissolved in a medium containing 2%HF and 1%HNO3,followed by determination using inductively coupled plasma-optical emission spectrometry(ICP-OES)equipped with a HF-resistant sample introduction system.The precision of the method(RSD)was 1.38%-3.46%(n=11)and the detection limits of this method were 1.91μg/g to 4.40μg/g.Validation using certified reference materials(CRMs)and real-world samples confirmed agreement between measured and certified values for CRMs,as well as consistency with results obtained by national standard methods and closed-vessel acid digestion.This method effectively suppresses the hydrolysis of W and Mo,while circumventing the drawbacks of alkali fusion methods,such as complex matrix interferences and elevated background values caused by the introduction of excessive salts.Moreover,it significantly reduces reagent consumption and experimental duration by eliminating the need for time-consuming steps such as acid evaporation and redissolution.The streamlined protocol is operationally simple and suitable for the determination of batch tungsten-molybdenum ore samples.关键词
微波消解/钨钼矿石/硝酸/氢氟酸/电感耦合等离子体发射光谱法Key words
microwave digestion/tungsten-molybdenum ores/nitric acid/hydrofluoric acid/inductively coupled plasma-optical emission spectrometry分类
化学化工引用本文复制引用
孙红宾,王蕾,臧慧媛,郭琳,于汀汀,马生凤..硝酸-氢氟酸微波消解-电感耦合等离子体发射光谱法测定钨钼矿石中钨钼铜锌[J].岩矿测试,2025,44(6):1156-1165,10.基金项目
国家重点研发计划项目(2021YFC2903000) （2021YFC2903000）
中国地质科学院基本科研业务费项目(CSJ-2022-09) （CSJ-2022-09）
