电感耦合等离子体质谱(ICP-MS)法测定页岩中稀土元素含量
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摘要
建立了湿法消解和微波消解两种前处理方法处理页岩样品,以铑、铼为内标,采用KED-ICPMS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,相对标准偏差为1.3%～8.2%(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、精密度和准确度。
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—100 ng/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 1.3% and 8.2%(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,precision and accuracy compared with wet digestion.
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—100 ng/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 1.3% and 8.2%(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,precision and accuracy compared with wet digestion.
引文
[1]中华人民共和国自然资源部.2017中国土地矿产海洋资源统计公报[R].2017.
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[11]戴雪峰,董利明,蒋宗明.电感耦合等离子体质谱(ICP-MS)法测定地质样品中重稀土元素和钍、铀[J].中国无机分析化学中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2016,6(4):20-25.
[12]张亚峰,冯俊,唐杰,等.基于五酸溶样体系-ICP-MS同时测定地质样品中稀土元素等46种元素[J].质谱学报(Journal of Chinese Mass Spectrometry Society),2016,37(2):186-192.
[13]章连香,冯先进.八级杆碰撞/反应池(ORS)-电感耦合等离子体质谱(ICP-MS)法测定复杂矿物中的稀土元素[J].中国无机分析化学中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2017,7(2):22-26.
[14]李丽君,王娜.电感耦合等离子体质谱法测定高岭土中的15中稀土元素[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis),2017,53(6):689-692.
[15]王小如.电感耦合等离子体质谱原理应用实例[M].北京:化学工业出版社,2005.
[16]中华人民共和国国土资源部.DZ 0130-2006地质矿产实验室测试质量管理规范[S].北京:中国标准出版社,2006.
[2]王中刚,于学元,赵振华,等.稀土元素地球化学[M].北京:科学出版社,1989.
[3]MCLENNAN S M.Rare earth elements in sedimentary rocks:influence of provenance and sedimentary processes[J].Review in Mineralogy,1989,21(1):169-200.
[4]刘宝珺,张锦泉.沉积成岩作用[M].北京:科学出版社,1992.
[5]陈亮,刘春莲,庄畅,等.三水盆地古近系下部湖湘沉积的稀土元素地球化学及其古气候意义[J].沉积学报(Acta Sedimentologica Sinica),2009,27(6):1155-1162.
[6]李佐臣,裴先治,李瑞保,等.西秦岭糜署岭花岗岩体年代学、地球化学特征及其构造意义[J].岩石学报(Acta Petrologica Sinica),2013,29(8):2617-2634.
[7]赵平,李爱民,刘建中,等.应用ICP-MS研究黔西南地区构造蚀变体稀土元素地球化学特征[J].岩矿测试(Rock and Mineral Analysis),2016,36(1):89-96.
[8]张茜,余谦,王剑,等.应用ICP-MS研究川西南马门溪龙龙马溪组泥页岩稀土元素特征及沉积环境[J].岩矿测试(Rock and Mineral Analysis),2018,37(2):217-224.
[9]王佩佩,李霄,宋伟娇.微波消解-电感耦合等离子体质谱法测定地质样品中稀土元素[J].分析实验室(Chinese Journal of Analysis Laboratory),2016,35(2):235-240.
[10]孙朝阳,杨凯,代小吕,等.电感耦合等离子体质谱(ICP-MS)法测定岩石中的稀土元素[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2015,5(4):48-52.
[11]戴雪峰,董利明,蒋宗明.电感耦合等离子体质谱(ICP-MS)法测定地质样品中重稀土元素和钍、铀[J].中国无机分析化学中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2016,6(4):20-25.
[12]张亚峰,冯俊,唐杰,等.基于五酸溶样体系-ICP-MS同时测定地质样品中稀土元素等46种元素[J].质谱学报(Journal of Chinese Mass Spectrometry Society),2016,37(2):186-192.
[13]章连香,冯先进.八级杆碰撞/反应池(ORS)-电感耦合等离子体质谱(ICP-MS)法测定复杂矿物中的稀土元素[J].中国无机分析化学中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2017,7(2):22-26.
[14]李丽君,王娜.电感耦合等离子体质谱法测定高岭土中的15中稀土元素[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis),2017,53(6):689-692.
[15]王小如.电感耦合等离子体质谱原理应用实例[M].北京:化学工业出版社,2005.
[16]中华人民共和国国土资源部.DZ 0130-2006地质矿产实验室测试质量管理规范[S].北京:中国标准出版社,2006.