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中国无机分析化学:2019,9(3):23-27
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电感耦合等离子体质谱(ICP-MS)法测定页岩中稀土元素含量
(1.成都市食品药品检验研究院;2.国土资源部页岩气资源勘查重点实验室重庆地质矿产研究院)
Determination of Rare Earth Elements in Shale by Inductively Coupled Plasma Mass Spectrometry
(1.Chengdu Institutes for Food and Drug Control;2.Key Laboratory of Shale Gas Exploration,Ministry of Land and Resources,Chongqing Institute of Geology and Mineral Resources)
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投稿时间:2018-12-12    修订日期:2019-05-07
中文摘要: 本文建立了湿法消解和微波消解两种前处理方法,以铑、铼为内标,采用KED-ICP-MS测定页岩样品中15种稀土元素(镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥和铱)。结果表明,各元素在0 ~ 100ng/mL范围内线性关系良好,相关系数在0.998以上,方法检出限在0.003 ~ 0.034mg/kg之间,相对标准偏差为1.28 % ~ 8.22 % (n=6)。由于页岩样品中有机质含量高,湿法消解时应适当提高高氯酸和硫酸的比例。对比湿法消解和微波消解两种前处理方法,微波消解消耗试剂较少,具有更优的检出限和精密度。
中文关键词: 湿法消解  微波消解  ICP-MS  稀土元素  页岩
Abstract:Two pretreatment methods were established for the determination of 15 rare earth elements (Lu, La, Ce,Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Y) in shale by KED-ICP-MS with microwave digestion and wet digestion. The Rh and Re through the introduction of online as internal standard. The results indicated that the linearity of REES were good in range of 0 ~ 100ng/mL, with the correlation coefficient higher than 0.998 and the detection limit within 0.003 ~ 0.034 mg/kg, the relative standard deviations were between 1.28 % and 8.22 % (n=6). Because of high organic matter content in shale, the proportion of perchloric acid and sulfuric acid should be increased appropriately with wet digestion. The microwave digestion was a rapid and efficient method for sample decomposition with less acid consuming, better detection limit and accuracy precision compared with wet digestion.
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尹庆红,祝秀江,栾进华,龚舟.电感耦合等离子体质谱(ICP-MS)法测定页岩中稀土元素含量[J].中国无机分析化学,2019,9(3):23-27.
YIN Qinghong,ZHU Xiujiang,LUAN Jinhua,GONG Zhou.Determination of Rare Earth Elements in Shale by Inductively Coupled Plasma Mass Spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2019,9(3):23-27.

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