电感耦合等离子体质谱法测定华阳川铀铌铅多金属矿中铀
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摘要
采用HF-HNO_3-HClO_4敞开酸溶,HNO_3-H_2O_2复溶的方法进行样品前处理,选用10μg/L 185 Re作内标,建立了电感耦合等离子体质谱法(ICP-MS)测定陕西华阳川铀铌铅多金属矿中铀的方法。实验表明,在选定的实验条件下,铀的质量浓度在10~100ng/mL范围内与其质谱强度呈良好的线性关系,校准曲线的相关系数为0.999 9,方法检出限为0.007μg/g。采用实验方法测定铀质量分数为8.46~1 255μg/g华阳川多金属矿石样品,6次平行测定的相对标准偏差(RSD)为0.71%~1.8%。采用实验方法分析一系列与华阳川铀铌铅多金属矿样成分相似的铀矿石标准物质,相对误差小于2.5%。采用标准方法 EJ/T 267.5—1984和实验方法进行方法对照,结果表明对质量分数大于200μg/g的华阳川多金属矿样品,二者的分析结果基本一致。
After the sample was pretreated by dissolution with HF-HNO3-HClO4 in open system and redissolution with HNO3-H2 O2,a determination method of uranium in Huayangchuan polymetallic ore in Shaanxi was established by inductively coupled plasma mass spectrometry(ICP-MS)with 10μg/L185 Re as internal standard.The results indicated that the mass concentration of uranium in range of 10-100 ng/mL showed good linear relationship with its mass intensity under the selected experimental conditions.The linear correlation coefficient of calibration curve was 0.999 9.The detection limit of method was 0.007μg/g.The experimental method was applied to determination of Huayangchuan polymetallic ore samples with mass fraction of uranium in range of 8.46-1 255μg/g.The relative standard deviations(RSD)for six parallel determination were between 0.71%-1.8%.The proposed method was applied to determination of uranium ore certified reference materials which have similar mineral composition with Huayangchuan polymetallic ore.The relative errors were less than 2.5%.The proposed method was also compared with standard method of EJ/T 267.5-1984.The results indicated that the determination values of uranium by the above two methods were consistent for Huayangchuan polymetallic ore samples with uranium content larger than 200μg/g.
After the sample was pretreated by dissolution with HF-HNO3-HClO4 in open system and redissolution with HNO3-H2 O2,a determination method of uranium in Huayangchuan polymetallic ore in Shaanxi was established by inductively coupled plasma mass spectrometry(ICP-MS)with 10μg/L185 Re as internal standard.The results indicated that the mass concentration of uranium in range of 10-100 ng/mL showed good linear relationship with its mass intensity under the selected experimental conditions.The linear correlation coefficient of calibration curve was 0.999 9.The detection limit of method was 0.007μg/g.The experimental method was applied to determination of Huayangchuan polymetallic ore samples with mass fraction of uranium in range of 8.46-1 255μg/g.The relative standard deviations(RSD)for six parallel determination were between 0.71%-1.8%.The proposed method was applied to determination of uranium ore certified reference materials which have similar mineral composition with Huayangchuan polymetallic ore.The relative errors were less than 2.5%.The proposed method was also compared with standard method of EJ/T 267.5-1984.The results indicated that the determination values of uranium by the above two methods were consistent for Huayangchuan polymetallic ore samples with uranium content larger than 200μg/g.
引文
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[13]杨金辉,张小毅.电感耦合等离子体质谱法测定煤中11种元素[J].冶金分析,2013,33(9):8-13.YANG Jin-hui,ZHANG Xiao-yi.Determination of eleven elements in coal by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2013,33(9):8-13.
[14]王琛,赵永刚,张继龙,等.流动注射-电感耦合等离子体质谱联用分析土壤样品中的铀[J].质谱学报,2010,31(1):34-37.WANG Chen,ZHAO Yong-gang,ZHANG Ji-long,et al.Determination of uranium in soil samples by flow injection-ICP-MS[J].Journal of Chinese Mass Spectrometry Society,2010,31(1):34-37.
[15]郭东发,张彦辉,武朝晖,等.高分辨电感耦合等离子体质谱法测定铀矿石样品中234 U/238 U,230 Th/232 Th和228 Ra/226 Ra同位素比值[J].岩矿测试,2009,28(2):101-107.GUO Dong-fa,ZHANG Yan-hui,WU Zhao-hui,et.al.Determination of 234 U/238 U,230 Th/232 Th,228 Ra/226 Ra ratios in uranium ores by high-resolution inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2009,28(2):101-107.
[16]谢胜凯,郭冬发,谭靖,等.国产电感耦合等离子体质谱仪测定地球化学样品中稀土和铀钍元素的含量[J].分析仪器,2013(5):27-31.XIE Sheng-kai,GUO Dong-fa,TAN Jing,et al.Determination of rare earth elements,U and Th in geochemical samples by inductively coupled plasma mass spectrometry[J].Analytical Instrumentation,2013(5):27-31.
[17]赵晓光,聂亚峰,张爱红,等.电感耦合等离子体质谱法测定水中铀钍元素的含量[J].化学分析计量,2016,25(5):28-31.ZHAO Xiao-guang,NIE Ya-feng,ZHANG Ai-hong,et al.Determination of 238 U and 232 Th in water by inductively coupled plasma mass spectrometry[J].Chemical Analysis and Meterage,2016,25(5):28-31.
[18]倪文山,姚明星,高小飞,等.电感耦合等离子体质谱法测定铀铌铅矿重选流程样品中铀[J].冶金分析,2017,37(5):25-29.NI Wen-shan,YAO Ming-xing,GAO Xiao-fei,et.al.Determination of uranium in gravity concentration process sample of uranium-niobium-lead ore by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2017,37(5):25-29.
[2]王江波,李卫红,惠争卜,等.陕西华阳川铀铌铅矿床地质特征[J].矿物学报,2013(增刊):248-249.WANG Jiang-bo,LI Wei-hong,HUI Zheng-bu,et al.Geological characteristics of the Huayangchuan U-Nb-Pb deposit,Shaanxi Province[J].Acta Mineral Sinica,2013(Suppl.):248-249.
[3]李清贞,张延安.激光荧光法测定中高含量铀[J].岩矿测试,1989,8(3):212-215.LI Qing-zhen,ZHANG Yan-an.Laser-induced fluorometry for the direct determination of U in solid samples[J].Rock and Mineral Analysis,1989,8(3):212-215.
[4]张桂英,董亚妮,李力争.地球化学样品中铀的激光荧光法测定[J].陕西地质,2003,21(2):107-110.ZHANG Gui-ying,DONG Ya-ni,LI Li-zheng.Laser fluorescence spectrometry for determination of uranium in geochemical sample[J].Geology of Shaanxi,2003,21(2):107-110.
[5]张燮,罗明标,周天元.选择性溶解-钒酸盐滴定法测定铀矿石及含铀岩石中六价铀[J].华东地质学院学报,2000,23(4):309-312.ZHANG Xie,LUO Ming-biao,ZHOU Tian-yuan.Determination of U(VI)in uranic ores and uraniferous rock by selective solubility-barium salt titration[J].Journal of East China Geological Institute,2000,23(4):309-312.
[6]杜浪,李玉香,马雪,等.偶氮胂Ⅲ分光光度法测定微量铀[J].冶金分析,2015,35(1):68-71.DU Lang,LI Yu-xiang,MA Xue,et al.Determination of micro uranium by arsenazoⅢspectrophotometry[J].Metallurgical Analysis,2015,35(1):68-71.
[7]李碧玉,阮琼,胡秋芬,等.2-(2-喹啉偶氮)-5-二甲氨基苯酚光度法测定铀的研究[J].化学研究与应用,2005,17(2):233-234.LI Bi-yu,RUAN Qiong,HU Qiu-fen,et al.Study on spectrophotometric determination of uranium in ore with 2-(2-quinolylazo)-5-dimthylaminophenol[J].Chemical Research and Application,2005,17(2):233-234.
[8]吴涛,康厚军,石正坤.微波消解样品-电感耦合等离子体原子发射光谱法测定土壤中铀[J].理化检验:化学分册,2013,49(2):219-221.WU Tao,KANG Hou-jun,SHI Zheng-kun.ICP-AES determination of uranium in soil with micro-wave assisted digestion[J].Phyisical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(2):219-221.
[9]刘先国,杨问华,方金东,等.电感耦合等离子体发射光谱法直接测定地质试样中铀[J].1997,16(4):296-298.LIU Xian-guo,YANG Wen-hua,FANG Jin-dong,et al.Determination of uranium in geological samples by ICPAES[J].Rock and Mineral Analysis,1997,16(4):296-298.
[10]经辉.X射线荧光光谱法同时测定矿石中铀和钍[J].中国无机分析化学,2015,5(3):34-40.JING Hui.Simultaneous determination of uranium and thorium in ores by X-ray fluorescence spectrometry[J].Journal of Inorganic Analytical Chemistry,2015,5(3):34-40.
[11]逯克思.X射线荧光光谱法测定岩石中铀和钍[J].分析试验室,2010,29(Suppl.):33-35.
[12]戴雪峰,董利明,蒋宗明.电感耦合等离子体质谱(ICPMS)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,2016,6(4):20-25.DAI Xue-feng,DONG Li-ming,JIANG Zong-ming.Determination of heavy rare earth element,Th and U in geological samples by inductively coupled plasma-mass spectrometry[J].Journal of Inorganic Analytical Chemistry,2016,6(4):20-25.
[13]杨金辉,张小毅.电感耦合等离子体质谱法测定煤中11种元素[J].冶金分析,2013,33(9):8-13.YANG Jin-hui,ZHANG Xiao-yi.Determination of eleven elements in coal by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2013,33(9):8-13.
[14]王琛,赵永刚,张继龙,等.流动注射-电感耦合等离子体质谱联用分析土壤样品中的铀[J].质谱学报,2010,31(1):34-37.WANG Chen,ZHAO Yong-gang,ZHANG Ji-long,et al.Determination of uranium in soil samples by flow injection-ICP-MS[J].Journal of Chinese Mass Spectrometry Society,2010,31(1):34-37.
[15]郭东发,张彦辉,武朝晖,等.高分辨电感耦合等离子体质谱法测定铀矿石样品中234 U/238 U,230 Th/232 Th和228 Ra/226 Ra同位素比值[J].岩矿测试,2009,28(2):101-107.GUO Dong-fa,ZHANG Yan-hui,WU Zhao-hui,et.al.Determination of 234 U/238 U,230 Th/232 Th,228 Ra/226 Ra ratios in uranium ores by high-resolution inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2009,28(2):101-107.
[16]谢胜凯,郭冬发,谭靖,等.国产电感耦合等离子体质谱仪测定地球化学样品中稀土和铀钍元素的含量[J].分析仪器,2013(5):27-31.XIE Sheng-kai,GUO Dong-fa,TAN Jing,et al.Determination of rare earth elements,U and Th in geochemical samples by inductively coupled plasma mass spectrometry[J].Analytical Instrumentation,2013(5):27-31.
[17]赵晓光,聂亚峰,张爱红,等.电感耦合等离子体质谱法测定水中铀钍元素的含量[J].化学分析计量,2016,25(5):28-31.ZHAO Xiao-guang,NIE Ya-feng,ZHANG Ai-hong,et al.Determination of 238 U and 232 Th in water by inductively coupled plasma mass spectrometry[J].Chemical Analysis and Meterage,2016,25(5):28-31.
[18]倪文山,姚明星,高小飞,等.电感耦合等离子体质谱法测定铀铌铅矿重选流程样品中铀[J].冶金分析,2017,37(5):25-29.NI Wen-shan,YAO Ming-xing,GAO Xiao-fei,et.al.Determination of uranium in gravity concentration process sample of uranium-niobium-lead ore by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2017,37(5):25-29.