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摘要
针对分析大批量的区域地质调查和多金属勘查任务,分别建立了过氧化钠碱熔-ICP-MS、高压密闭消解-ICP-MS和粉末压片-WD-XRF 3种分析方法测定土壤、水系沉积物和岩石样品中15种稀土元素。3种方法的检出限分别为0.011~0.173、0.001 2~0.009 7、0.06~5.42 μg/g,高压密闭消解-ICP-MS法的检出限明显优于碱熔ICP-MS法和粉末压片WD-XRF法;3种方法测定的国家标准物质稀土元素的相对误差(RE%)分别为-6.5~6.6、-11.2~3.6、-9.7~12.7,精密度(RSD%)分别为2.4~8.8、2.8~8.2、2.4~9.4,均满足DZ/T 0258—2014《多目标区域地球化学调查规范(1:250 000)》的要求。实验表明,粉末压片-WD-XRF法受到检出限高的限制,不能应用于测定稀土含量极低的地质样品,高压密闭酸溶-ICP-MS法测定矿物结构复杂的岩石样品时,个别测定结果严重低于标准值。验证了碱熔ICP-MS法在实际工作中的可行性,测定值最接近真实值,最适合进行分析大批量的区域地质调查和多金属勘查任务。
Abstract
In the light of a large number of regional geological surveys and polymetallic survey tasks,sodium peroxide alkali fusion-ICP-MS,high-pressure closed digestion-ICP-MS and pressed powder pellet-WD-XRF methods are respectively established to determine 15 rare earth elements in soil,stream sediments and rock samples.Detection limits of three methods are 0.011-0.173 μg·g-1,0.001 2-0.009 7 μg·g-1,and 0.06-5.42 μg·g-1.Detection limit of high-pressure closed digestion-ICP-MS method is significantly better than that of other two methods.Relative errors (RE%)by three methods are -6.5-6.6,-11.2-3.6 and -9.7-12.7,respectively.The precisions (RSD%) are 2.4-8.8,2.8-8.2,and 2.4-9.4,respectively.Both accuracy and precision meet the requirements of DZ/T 0258—2014 "Specifications for Geochemical Investigations in Multi-Target Areas (1:250 000)".Experimental results show that the pressed powder pellet-WD-XRF method is limited by its high detection limit and cannot be used to determine geological samples with extremely low rare earth content.When high-pressure closed digestion-ICP-MS method is used to determine rock samples with complex mineral structure,the individual measurement results are seriously lower than the standard value.The feasibility of alkali fusion-ICP-MS in practical work has been verified and the measured values close to the true values,which is the most suitable for the analysis of large-scale regional geological survey and polymetallic survey tasks.
关键词
电感耦合等离子体质谱法
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碱熔
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稀土元素
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地质样品
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波长色散X射线荧光光谱法
Key words
inductively coupled plasma mass spectrometry
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alkali fusion
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rare earth elements
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geological samples
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wavelength-dispersive X-ray fluorescence spectrometry
ICP-MS法和WD-XRF法测定地质样品中稀土元素的方法研究[J].
现代化工, 2021, 41(3): 244-250 DOI:10.16606/j.cnki.issn0253-4320.2021.03.050