首页|高压密闭消解-电感耦合等离子体原子发射光谱法测定锂矿中锂

高压密闭消解-电感耦合等离子体原子发射光谱法测定锂矿中锂

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锂矿是重要的国家战略资源,准确测定锂矿中的锂含量对锂矿的采选及加工具有重要的指导意义.使用敞开式混酸消解体系无法彻底消解样品或在消解过程中锂有损失,无法满足准确测定的要求.实验采用硝酸-氢氟酸酸溶体系,于190 ℃采用高压密闭消解样品,能使样品完全消解;选择Li 670.784 nm作为分析线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定锂矿中锂的方法.使用基体匹配法配制标准溶液系列可以消除基体效应对测定的影响;钙、钠、钾、镁、铁、锰、磷等共存元素对锂的测定无影响.锂的质量浓度在0.50~50μg/mL范围内与发射强度呈良好的线性关系,校准曲线线性相关系数为0.999 8;方法检出限为0.003%.将方法应用于锂矿石标准物质和实际样品,标准物质的测定值和认定值基本一致,测定结果的相对标准偏差(RSD,n=12)在0.84%~1.4%之间,相对误差(RE,n=12)在-1.24%~0.51%之间;实际样品中锂测定结果的相对标准偏差(RSD,n=12)在1.6%~2.0%之间,加标回收率在98%~104%之间.
Determination of lithium in lithium ore by inductively coupled plasma atomic emission spectrometry with high-pressure closed digestion
Lithium ore is an important national strategic resource.The accurate determination of lithium content in lithium ore is of great directive significance for the mining and processing of lithium ores.The sample cannot be fully digested in acid mixture system in open environment or there is loss for lithium in digestion process,which cannot meet the requirements of accurate determination.In this study,the sam-ple could be digested completely with nitric acid-hydrofluoric acid system in a high-pressure closed system at 190 ℃.Thus,a method for determination of lithium in lithium ore by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established with Li 670.784 nm as analytical line.The standard so-lution series were prepared by matrix matching method to eliminate the influence of matrix effect on the de-termination.The coexisting elements such as calcium,sodium,potassium,magnesium,iron,manganese and phosphorus had no influence on the determination.The mass concentration of lithium in range of 0.50-50 μg/mL showed good linear relationship with its corresponding emission intensity,and the linear correla-tion coefficient of calibration curve was 0.999 8.The limit of detection of method was 0.003%.The pro-posed method was applied for determination of certified reference materials and samples of lithium ore.For certified reference materials,the results were basically consistent with the certified values,and the relative standard deviations(RSD.n=12)of determination results were between 0.84%and 1.4%,then the rela-tive errors(RE,n=12)were between-1.24%and 0.51%.For lithium ore samples,the RSDs(n=12)of determination results were between 1.6%and 2.0%,and the recoveries were between 98%and 104%.

lithium orelithiumhigh-pressure closed digestioninductively coupled plasma atomic emission spectrometry(ICP-AES)

王晓星、李玲娜、谭伟、徐龙威、苏凌云

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云南省核工业二○九地质大队,云南昆明 650000

锂矿 高压密闭消解 电感耦合等离子体原子发射光谱法(ICP-AES)

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(9)