电感耦合等离子体质谱法测定地质样品中痕量碲
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摘要
采用HF-HNO3体系密闭溶解样品,用HCl-NaBr-甲基异丁基酮(MIBK)体系对Te进行萃取和反萃取,加入乙醇对测定信号强度进行增敏,以125 Te作为测定同位素,建立了电感耦合等离子体质谱法(ICP-MS)测定地质样品中痕量Te的方法。对溶样条件进行了优化,确定溶样条件如下:采用7.0mL HF与HNO3体积比为1∶3的混合酸,于160℃控温电热板上溶样3h。增敏试验表明,控制测定液中乙醇的体积分数为4%效果最佳。以待测元素质量浓度为横坐标,以待测元素与内标元素的信号强度之比为纵坐标绘制校准曲线,线性相关系数大于0.999 9。方法检出限为0.005 4μg/g。采用实验方法对地质标准物质中痕量Te进行测定,测定结果与认定值基本保持一致,相对标准偏差(RSD,n=12)均在6.7%以内。分别用实验方法与氢化物发生原子荧光光谱法(HG-AFS)对土壤样品1#~4#及铅锌矿样品6#~10#中Te进行测定,结果基本一致。
After the sample was dissolved with HF-HNO3 in closed system,Te was extracted and reextracted with HCl-NaBr-methyl isobutyl ketone(MIBK),and ethanol was added to enhance the intensity of determination signal.Thus,a determination method of trace Te in geological sample by inductively coupled plasma mass spectrometry(ICP-MS)was established with 125 Te as determination isotope.The sample dissolution conditions were optimized as follows:the sample was dissolved with 7.0 mL of HF-HNO3 mixed acid with volume ratio of 1∶3 when it was heated on electric hot plate at 160℃for 3 h.The sensitivity enhancing test indicated that the effect was optimal when the volume fraction of ethanol in determination solution was 4%.The calibration curve was plotted with the mass concentration of test element as x-axis and the signal intensity ratio of test element to internal standard element as y-axis.The linear correlation coefficient was higher than 0.999 9.The detection limit was 0.005 4μg/g.The content of trace Te in certified reference materials of geological sample were determined according to the experimental method,and the results were basically consistent with the certified values.The relative standard deviations(RSD,n=12)were all lower than 6.7%.The content of Te in soil samples(1#-4#)and lead-zinc ore samples(6#-10#)was determined by the experimental method,and the results were consistent with those obtained by hydride generation atomic fluorescence spectrometry(HG-AFS).
After the sample was dissolved with HF-HNO3 in closed system,Te was extracted and reextracted with HCl-NaBr-methyl isobutyl ketone(MIBK),and ethanol was added to enhance the intensity of determination signal.Thus,a determination method of trace Te in geological sample by inductively coupled plasma mass spectrometry(ICP-MS)was established with 125 Te as determination isotope.The sample dissolution conditions were optimized as follows:the sample was dissolved with 7.0 mL of HF-HNO3 mixed acid with volume ratio of 1∶3 when it was heated on electric hot plate at 160℃for 3 h.The sensitivity enhancing test indicated that the effect was optimal when the volume fraction of ethanol in determination solution was 4%.The calibration curve was plotted with the mass concentration of test element as x-axis and the signal intensity ratio of test element to internal standard element as y-axis.The linear correlation coefficient was higher than 0.999 9.The detection limit was 0.005 4μg/g.The content of trace Te in certified reference materials of geological sample were determined according to the experimental method,and the results were basically consistent with the certified values.The relative standard deviations(RSD,n=12)were all lower than 6.7%.The content of Te in soil samples(1#-4#)and lead-zinc ore samples(6#-10#)was determined by the experimental method,and the results were consistent with those obtained by hydride generation atomic fluorescence spectrometry(HG-AFS).
引文
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[12]程秀花,黎卫亮,王海蓉.封闭酸溶样ICP-MS法直接测定地质样品中镓、铟、铊、锗[J].分析试验室,2015,34(10):1204-1208.CHENG Xiu-hua,LI Wei-liang,WANG Hai-rong.Determination of gallium,indium,thallium and germanium in geological samples after pressurized acid digestion by inductively coupled plasma mass spectrometry[J].Chinese Journal of Analysis Laboratory,2015,34(10):1204-1208.
[13]刘红毅,罗大芳,鲍爱华.GFAAS法测定地质样品中痕量银[J].云南地质,2011,30(3):348-352.LIU Hong-yi,LUO Da-fang,BAO Ai-hua.The application of GFAAS method to testing of trace Ag in the geological sample[J].Yunnan Geology,2011,30(3):348-352.
[14]裴玲云.石墨炉原子吸收光谱法测定地质样品中的痕量铂、钯[J].铀矿地质,1993(4):51-57.PEI Ling-yun.The determination of trace platinum and palladium in geological samples by graphite furnace atomic absorption spectrometry[J].Uranium Geology,1993(4):51-57.
[15]张彦斌,程忠洲,李华.硫脲树脂富集-电感耦合等离子体质谱法测定地质样品中的超痕量金、银、铂、钯[J].分析试验室,2006(7):105-108.ZHANG Yan-bin,CHENG Zhong-zhou,LI Hua.Determination of ultra trace gold,silver,platinum and palladium in geochemical samples by inductively coupled plasma mass spectroscopy combined with the thiourea resin preconcentration[J].Chinese Journal of Analysis Laboratory,2006(7):105-108.
[2]王瑞侠,陆蓉,陆光汉.碲的分析方法研究进展[J].冶金分析,2012,32(8):31-37.WANG Rui-xia,LU Rong,LU Guang-han.Research progress on analytical methods of tellurium[J].Metallurgical Analysis,2012,32(8):31-37.
[3]藏树良,邓桂春,刘兴芝.稀散元素化学与应用[M].北京:中国石化出版社,2008:4-23.
[4]方国桢,刘黎,方建生.高敏连续分光光度法测定矿泉水中不同价态的痕量碲[J].食品与发酵工业,1994(6):16-21.FANG Guo-zhen,LIU Li,FANG Jian-sheng.Highly sensitive and sequential determination of different valence of traces tellurium in mineral water samples by spectrophotometry[J].Food and Fermentation Industries,1994(6):16-21.
[5]李志伟,纪朋.碲的分析测试方法研究进展[J].化学工程师,2013(4):45-47.LI Zhi-wei,JI Peng.Research progress on analytical methods of tellurium[J].Chemical Engineer,2013(4):45-47.
[6]郭小伟,郭旭明.氢化物发生-无色散原子荧光分析法进展及在环境分析中的应用[J].上海环境科学,1995,14(7):28-31.GUO Xiao-wei,GUO Xu-ming.Progress of hydride generation-nondispersive atomic fluorescence spectrometry and the prospects of its application to environmental analysis[J].Shanghai Environmental Science,1995,14(7):28-31.
[7]黎卫亮,程秀花,张明祖.乙醇增强-电感耦合等离子体质谱法测定地质样品中镓铟铊锗碲[J].冶金分析,2014,34(3):13-18.LI Wei-liang,CHENG Xiu-hua,ZHANG Ming-zu.Determination of gallium,indium,thallium.germanium and tellurim in geological samples by inductively coupled plasma mass spectrometry with ethanol as a signal enhancer[J].Metallurgical Analysis,2014,34(3):13-18.
[8]董静,储溱,李策,等.碲的分离富集与分析研究进展[J].资源环境与工程,2010,24(1):85-88.DONG Jing,CHU Qin,LI Ce,et al.Separation&enrichment of tellurium and progress of analytical study[J].Resources Environment&Engineering,2010,24(1):85-88.
[9]肖凡,刘金巍,王永清.萃取/反萃取分离富集-氢化物无色散原子荧光法测定复杂地质样品中的痕量碲[J].光谱学与光谱分析,2009,29(4):1123-1126.XIAO Fan,LIU Jin-wei,WANG Yong-qing.Separation and preconcentration by extracation and antiextracation-determination of trace Te in complex geological samples by hydride generation atomic fluorescence spectrometry[J].Spectroscopy and Spectral Analysis,2009,29(4):1123-1126.
[10]韩丽荣,李冰,马新荣.乙醇增强-电感耦合等离子体质谱法直接测定地质样品中碲[J].岩矿测试,2003,22(2):98-101.HAN Li-rong,LI Bing,MA Xin-rong.Direct determination of tellurium by inductively coupled plasma mass spectrometry with ethanol as a signal enhancer[J].Rock and Mineral Analysis,2003,22(2):99-101.
[11]陈波,刘洪青,邢应香.电感耦合等离子体质谱法同时测定地质样品中锗硒碲[J].岩矿测试,2014,33(2):192-196.CHEN Bo,LIU Hong-qing,XING Ying-xiang.Simultaneous determination of Ge,Se and Te in geological samples by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2014,33(2):192-196.
[12]程秀花,黎卫亮,王海蓉.封闭酸溶样ICP-MS法直接测定地质样品中镓、铟、铊、锗[J].分析试验室,2015,34(10):1204-1208.CHENG Xiu-hua,LI Wei-liang,WANG Hai-rong.Determination of gallium,indium,thallium and germanium in geological samples after pressurized acid digestion by inductively coupled plasma mass spectrometry[J].Chinese Journal of Analysis Laboratory,2015,34(10):1204-1208.
[13]刘红毅,罗大芳,鲍爱华.GFAAS法测定地质样品中痕量银[J].云南地质,2011,30(3):348-352.LIU Hong-yi,LUO Da-fang,BAO Ai-hua.The application of GFAAS method to testing of trace Ag in the geological sample[J].Yunnan Geology,2011,30(3):348-352.
[14]裴玲云.石墨炉原子吸收光谱法测定地质样品中的痕量铂、钯[J].铀矿地质,1993(4):51-57.PEI Ling-yun.The determination of trace platinum and palladium in geological samples by graphite furnace atomic absorption spectrometry[J].Uranium Geology,1993(4):51-57.
[15]张彦斌,程忠洲,李华.硫脲树脂富集-电感耦合等离子体质谱法测定地质样品中的超痕量金、银、铂、钯[J].分析试验室,2006(7):105-108.ZHANG Yan-bin,CHENG Zhong-zhou,LI Hua.Determination of ultra trace gold,silver,platinum and palladium in geochemical samples by inductively coupled plasma mass spectroscopy combined with the thiourea resin preconcentration[J].Chinese Journal of Analysis Laboratory,2006(7):105-108.