2023·11分析与检测76ModernChemicalResearch当代化工研究碱熔-电感耦合等离子体质谱法测定钨矿石和钼矿石中的钨钼*黄朝文莫凯敏(湖南省矿产资源调查所湖南423000)摘要:试样经过氧化钠熔融,取上层清液酸化,酸化后溶液经稀释20倍后,直接上ICP-MS测定。本方法总盐度为0.12g/L,完全满足质谱仪常见注意事项中样品的总盐度必须严格控制在1g/L以下,仪器信号稳定,基体干扰小。本方法检出限钨为0.002%,钼为0.002%,测定范围为0.005%~4.0%。本方法适用于钨矿石和钼矿石中钨钼的测定,准确度高、稳定性好。样品基体引起的仪器响应抑制或者增强效益和仪器漂移通过内标补偿,用国家标准物质进行验证,测定值与标准值的相对误差小于5%(n=6),完全满足了测试要求。关键词:钨;钼;碱熔;钨矿石;钼矿石;电感耦合等离子体质谱法中图分类号:O657文献标识码:ADOI:10.20087/j.cnki.1672-8114.2023.11.023DeterminationofTungstenandMolybdenuminTungstenOreandMolybdenumOrebyInductivelyCoupledPlasma-massSpectrometrywithAlkaliFusionHuangChaowen,MoKaimin(Hu'nanProvincialInstituteofMineralResources,Hu'nan,423000)Abstract:Thesampleismeltedbysodiumperoxide,thesupernatantisacidifiedbyhydrochloricacid,thenthesolutionisdiluted20timesanddeterminedbyICP-MSdirectly.Thetotalsalinityofthismethodis0.12g/L.Thetotalsalinityofthesamplemustbestrictlycontrolledbelow1g/LinordertomeettherequirementsofMassSpectrometer,thesignaloftheinstrumentisstableandthematrixinterferenceissmall.Thelimitofdetectionis0.002%forTungstenand0.002%forMolybdenum.Therangeofdetectionis0.005%~4.0%.Themethodissuitableforthedeterminationoftung-stenandMolybdenumintungstenoreandmolybdenumorewithhighaccuracyandgoodstability.Theinstrumentresponsesuppressionorenhance-mentbenefitandinstrumentdriftcausedbysamplematrixarecompensatedbyinternalstandard.Therelativeerrorbetweenthemeasuredvalueandthestandardvalueislessthan5%(n=6).Keywords:tungsten;molybdenum;alkalifusion;tungstenore;molybdenumore;inductivelycoupledplasma-massspectrometry目前常用分光光度法和极谱法测定钨矿石、钼矿石中的钨钼,其中钨矿石和钼矿石耐酸性强,酸溶难于消解完全,碱熔融光度法操作繁琐,极谱法只适用于低含量的试样。因...