High Pressure Sealed Digestion-Determination of 50 Elements in Geochemical Samples by Inductively Coupled Plasma Mass Spectrometry
摘 要
选择电感耦合等离子体质谱法测定地球化学样品中50种元素的含量。取0.100 0 g样品,置于高压密闭消解罐的聚四氟乙烯(PTFE)内胆中,加入氢氟酸3 mL及硝酸1 mL,放入密闭钢套中,拧紧。在150℃下消解2 h,待冷却降压后取出内胆,加入高氯酸0.25 mL,于150℃加热蒸发至白烟冒尽。加入硝酸1 mL和水1 mL,将内胆置于钢套中,于150℃再次密闭消解12 h。自然冷却,将内胆中溶液转移至PTFE比色管中,加水定容至10.0 mL,摇匀。分取此母液1.00 mL,置于10 mL PTFE比色管中,用约φ 2.2%硝酸溶液稀释至10.0 mL,保持溶液中硝酸浓度在3%左右。此溶液用于测定(S1组)Li、Be、V等28种元素和(S2组)Sc、Y、La等16种元素。另取母液1.00 mL,置于10 mL PTFE比色管中,加入φ 10%氢氟酸溶液2滴,500 g·L-1的酒石酸溶液1.0 mL,用约φ 2.5%硝酸溶液稀释至10.0 mL,摇匀。此溶液供测定(S3组)Ti、Zr、Nb等6种元素。对质谱干扰较严重的被测元素分别建立了11个校准方程用于校准相关测定数据。用所提出方法分析了6种地球化学国家一级标准物质(GBW 07359,GBW 07360,GBW 07361,GBW 07408,GBW 07427,GBW 07446),对其中与本方法有关的50种元素进行测定,所得结果与认定值相符,达到了地质矿产实验室测试质量规范的要求。
Abstract
ICP-MS was applied to the determination of 50 elements in geochemical sample. The sample (0.100 0 g) was digested with 3 mL of HF and 1 mL of HNO3 in the PTFE-liner of the pressurized hermetically-sealed digestion system at 150℃ for 2 h. After cooling and de-pressurizing, the liner was taken out and 0.25 mL of HClO4 was added to the digested solution, and the mixed solution was evaporated by heating at 150℃ until ending of the acid-fuming. 1 mL each of HNO3 and H2O was added, and the liner was replaced into the steel case of the digestor and the mixture in the liner was digested once more at 150℃ for 12 h. After natural cooling, the solution in the liner was transferred to a 10 mL PTFE colorimetric tube, and its volume was made up to 10.0 mL with water. A aliquot of 1.0 mL was taken from this mother sample solution and transferred to another 10 mL PTFE colorimetric tube and its volume was diluted to 10.0 mL with φ 2.2% HNO3 solution to keep the concentration of HNO3 at ca. φ 3%. This solution was used for MS determination of 28 elements (including Li, Be, V and etc. as shown in S1) and of 16 elements (including Sc, Y, La and etc. as shown in S2). Another aliquot of 1.0 mL was taken from the mother solution and placed into another 10 mL PTFE colorimetric tube, 2 drops of φ 10% HF solution and 1 mL of 500 g·L-1 tartaric acid solution were added, and its volume was diluted to 10.0 mL with ca. φ 2.5% HNO3 solution. This solution was used for determination of the remaindering 6 elements (including Ti, Zr, Nb and etc. as shown in S3). Eleven equations were established for calibration of errors of determined values of the respective 11 elements due to MS interferences. The proposed method was applied to the analysis of 6 CRMs of GBW 07359, GBW 07360, GBW 07361, GBW 07408, GBW 07427 and GBW 07446 in which the related 50 elements was determined giving results in consistency with the certified values, and meeting with the requirements for testing quality given in the management standard for geological laboratories.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201907017
所属栏目 专题报道(电感耦合等离子体质谱法)
基金项目 中国地质科学院地球物理地球化学勘查研究所中央级公益性科研院所基本科研业务费专项资金资助项目(AS2016P03)
收稿日期 2018/11/17
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备注于亚辉,高级工程师,硕士,主要从事岩矿分析测试方法研究工作,68523749@qq.com
引用该论文: YU Yahui,LIU Jun,LI Xiaohui,HAN Zhixuan,HU Jiazhen,WANG Ying,WU Zhe,CHENG Yi. High Pressure Sealed Digestion-Determination of 50 Elements in Geochemical Samples by Inductively Coupled Plasma Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(7): 833~839
于亚辉,刘军,李小辉,韩志轩,胡家祯,王盈,毋喆,程祎. 高压密闭消解-电感耦合等离子体质谱法测定地球化学样品中的50种元素[J]. 理化检验-化学分册, 2019, 55(7): 833~839
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【2】王君玉,吴葆存,李志伟,等.敞口酸溶-电感耦合等离子体质谱法同时测定地质样品中45个元素[J].岩矿测试, 2011,30(4):440-445.
【3】田衎,刑书才,杨郡,等.土壤/沉积物中重金属元素分析的前处理技术研究进展[J].光谱实验室, 2012,29(1):247-251.
【4】侯振辉,王晨香.电感耦合等离子体质谱法测定地质样品中35种微量元素[J].中国科学技术大学学报, 2007,37(8):940-944.
【5】陈永欣,黎香荣,韦新红,等.微波消解-电感耦合等离子体质谱法测定土壤和沉积物中痕量稀土元素[J].岩矿测试, 2011,30(5):560-565.
【6】田娟娟,杜慧娟,潘秋红,等.电热板消解与密闭罐消解对土壤中49种矿质元素ICP-MS法检测的影响[J].分析测试学报, 2009,28(3):319-325.
【7】何红蓼,李冰,韩丽荣,等.封闭压力酸溶-ICP-MS法分析地质样品中47个元素的评价[J].分析实验室, 2002,21(5):8-12.
【8】王北洪,马智宏,付伟利.密封高压消解罐消解-原子吸收光谱法测定土壤重金属[J].农业工程学报, 2008,24(S2):255-259.
【9】张琪,刘琳娟.高压密闭消解-原子吸收光度法同时测定土壤中的铜、锌、铅、镉、镍、铬[J].化学分析计量, 2007,16(5):48-50.
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【17】FIELD M P, LAVIGNE M, MURPHY K R, et al. Direct determination of P, V, Mn, As, Mo, Ba and U in seawater by SF-ICP-MS[J]. Journal of Analytical Atomic Spectrometry, 2007,22(9):1145-1151.
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【22】刘晔,第五春荣,柳小明,等.密闭高温高压溶样ICP-MS测定56种国家地质标准物质中的36种痕量元素:对部分元素参考值修正和定值的探讨[J].岩矿测试, 2013,32(2):221-228.
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