高压微波消解-电感耦合等离子体质谱法测定地质样品中分散元素镓铟铊锗碲镉
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摘要
建立灵敏度高、准确度高的分散元素分析方法一直是地质样品分析的重点。采用高压微波消解法以HF-HNO_3体系处理样品,选择~(205 )Tl、~(125 )Te、~(69 )Ga、~(74 )Ge、~(115)In、~(114 )Cd作为测量同位素,采用校正方程在线校正了~(74 )Ge、~(115)In的同量异位素干扰,采用离线校正方式校正了~(114)Sn对~(114)Cd的同量异位素干扰,建立了电感耦合等离子体质谱法(ICP-MS)测定地质样品中分散元素Ga、In、Tl、Ge、Te、Cd的方法。对称样量、高压微波消解条件、浸取酸种类进行了优化。结果表明,在优化的实验条件下,校准曲线的相关系数均不小于0.999 7,检出限为0.005～0.093μg/g,测定下限为0.017～0.31μg/g。按照实验方法对土壤成分分析标准物质、水系沉积物成分分析标准物质、安山岩岩石成分分析标准物质中Ga、In、Tl、Ge、Te、Cd平行测定12次,各元素测定值与认定值基本一致,相对标准偏差(RSD)均不大于8.5%,相对误差不大于9.1%。采用实验方法对土壤样品进行分析,测定结果与封闭酸溶-ICP-MS测定Ga、In和Tl,氢化物发生原子荧光光谱法测定Ge,乙醇增敏-ICP-MS测定Te,石墨炉原子吸收光谱法测定Cd的结果基本吻合。
The establishment of a highly sensitive and accurate analytical method for disperse elements has aways been the focus of geological sample analysis.The samples were treated by high-pressure microwave digestion in HF-HNO_3system.~(205 )Tl,~(125 )Te,~(69 )Ga,~(74 )Ge,~(115)In,~(114)Cd were selected as the measured isotopes.The isobaric interference of ~(74 )Ge and ~(115)In was corrected by the online calibration equation,while the isobaric interference of ~(114)Sn to ~(114)Cd were corrected by offline interference correction.A method for the determination of disperse elements of Ga,In,Tl,Ge,Te and Cd in geological samples by inductively coupled plasma mass spectrometry(ICP-MS)has been developed.The mass of samples,conditions of highpressure microwave digestion,and leaching acid species were optimized.The results show that under the optimized experimental conditions,the correlation coefficient of the calibration curve is not less than 0.9997,with the detection limit ranges from 0.005 to 0.093μg/g,and the low limit of determination from 0.017to 0.31μg/g.The proposed method was applied for the 12 times parallel determination of Ga,In,Tl,Ge,Te and Cd in the composition analysis standard substances of soil,water sediment,and andesite rock.The analytical results were basically consistent with the certified values,with the relative standard deviations(RSD)were not more than 8.5% and the relative errors were not more than 9.1%.The soil samples were analyzed by experimental methods.The results were basically consistent with the determination of Ga,In and Tl by closed acid dissolution-ICP-MS,determination of Ge by hydride generation atomic fluorescence spectrometry,determination of Te by ethanol sensitization-ICP-MS and the determination of Cd by graphite furnace atomic absorption spectrometry.
The establishment of a highly sensitive and accurate analytical method for disperse elements has aways been the focus of geological sample analysis.The samples were treated by high-pressure microwave digestion in HF-HNO_3system.~(205 )Tl,~(125 )Te,~(69 )Ga,~(74 )Ge,~(115)In,~(114)Cd were selected as the measured isotopes.The isobaric interference of ~(74 )Ge and ~(115)In was corrected by the online calibration equation,while the isobaric interference of ~(114)Sn to ~(114)Cd were corrected by offline interference correction.A method for the determination of disperse elements of Ga,In,Tl,Ge,Te and Cd in geological samples by inductively coupled plasma mass spectrometry(ICP-MS)has been developed.The mass of samples,conditions of highpressure microwave digestion,and leaching acid species were optimized.The results show that under the optimized experimental conditions,the correlation coefficient of the calibration curve is not less than 0.9997,with the detection limit ranges from 0.005 to 0.093μg/g,and the low limit of determination from 0.017to 0.31μg/g.The proposed method was applied for the 12 times parallel determination of Ga,In,Tl,Ge,Te and Cd in the composition analysis standard substances of soil,water sediment,and andesite rock.The analytical results were basically consistent with the certified values,with the relative standard deviations(RSD)were not more than 8.5% and the relative errors were not more than 9.1%.The soil samples were analyzed by experimental methods.The results were basically consistent with the determination of Ga,In and Tl by closed acid dissolution-ICP-MS,determination of Ge by hydride generation atomic fluorescence spectrometry,determination of Te by ethanol sensitization-ICP-MS and the determination of Cd by graphite furnace atomic absorption spectrometry.
引文
[1]何恬叶,张颖红,胡子文.微波消解ICP-OES法测定土壤样品中22种元素[J].分析试验室,2018,37(1):84-87.HE Tian-ye,ZHANG Ying-hong,HU Zi-wen.Determination of 22elements in soil by ICP-OES with microwave digestion[J].Chinese Journal of Analysis Laboratory,2018,37(1):84-87.
[2]黄子敬,陈孟君,邓华阳,等.微波消解-ICP-MS混合模式测定动植物源食品中11种金属元素[J].分析试验室,2017,36(1):24-28.HUANG Zi-jing,CHEN Meng-jun,DENG Hua-yang,et al.Determination of 11trace elements in animal and plant origin food by microwave digestion with ICP-MS in mixed mode[J].Chinese Journal of Analysis Laboratory,2017,36(1):24-28.
[3]赵小龙,燕娜,侍金敏,等.微波消解-电感耦合等离子体质谱法测定镍精矿中Ga、Ge、Se、Cd、In、Te、La和Tl[J].理化检验:化学分册,2017,53(9):1031-1035.ZHAO Xiao-long,YAN Na,SHI Jin-min,et al.Determination of Ga,Ge,Se,Cd,In,Te,La and Tl in nickel concentrates by ICP-MS combined with microwave digestion[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2017,53(9):1031-1035.
[4]赵朝辉,李可及,邹利平,等.ICP-MS同时测定土壤样品中的镓铟锗[J].矿产综合利用,2012(3):52-54.ZHAO Chao-hui,LI Ke-ji,ZOU Li-ping,et al.Simultaneous determination of Ga,In and Ge in soil samples by ICP-MS[J].Multipurpose Utilization of Mineral Resources,2012(3):52-54.
[5]黎卫亮,程秀花,张明祖,等.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,et al.Determination of gallium,indium,thallium,germanium and tellurium in geological samples by inductively coupled plasma mass spectrometry with ethanol as a signal enhancer[J].Metallurgical Analysis,2014,34(3):13-18.
[6]程秀花,黎卫亮,王海蓉,等.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,et al.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.
[7]张世涛.电感耦合等离子体质谱法测定铅锌矿中镓铟锗铊[J].化学与黏合,2014,36(6):460-462.ZHANG Shi-tao.Determination of Ga,In,Ge and Tl in lead-zinc ore by ICP-MS[J].Chemistry and Adhesion,2014,36(6):460-462.
[8]易晓明,李建文.电感耦合等离子体质谱法测定镉同位素时锡、钯、银等元素的干扰及其分离方法研究[J].冶金分析,2008,28(9):7-10.YI Xiao-ming,LI Jian-wen.Study on interference and separation of tin,palladium and silver in the determination of cadmium isotopes by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2008,28(9):7-10.
[9]陈波,刘洪青,刑应香.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.
[10]孙朝阳,董利明,贺颖婷,等.电感耦合等离子体质谱法测定地质样品中钪镓锗铟镉铊时的干扰及其消除方法[J].理化检验:化学分册,2016,52(9):1026-1030.SUN Chao-yang,DONG Li-ming,HE Ying-ting,et al.Elimination of interferences in ICP-MS determination of Sc,Ga,Ge,In,Cd and Tl in geological samples[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2016,52(9):1026-1030.
[11]岩石矿物分析编委会.岩石矿物分析[M].4版.北京:地质出版社,2011.
[2]黄子敬,陈孟君,邓华阳,等.微波消解-ICP-MS混合模式测定动植物源食品中11种金属元素[J].分析试验室,2017,36(1):24-28.HUANG Zi-jing,CHEN Meng-jun,DENG Hua-yang,et al.Determination of 11trace elements in animal and plant origin food by microwave digestion with ICP-MS in mixed mode[J].Chinese Journal of Analysis Laboratory,2017,36(1):24-28.
[3]赵小龙,燕娜,侍金敏,等.微波消解-电感耦合等离子体质谱法测定镍精矿中Ga、Ge、Se、Cd、In、Te、La和Tl[J].理化检验:化学分册,2017,53(9):1031-1035.ZHAO Xiao-long,YAN Na,SHI Jin-min,et al.Determination of Ga,Ge,Se,Cd,In,Te,La and Tl in nickel concentrates by ICP-MS combined with microwave digestion[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2017,53(9):1031-1035.
[4]赵朝辉,李可及,邹利平,等.ICP-MS同时测定土壤样品中的镓铟锗[J].矿产综合利用,2012(3):52-54.ZHAO Chao-hui,LI Ke-ji,ZOU Li-ping,et al.Simultaneous determination of Ga,In and Ge in soil samples by ICP-MS[J].Multipurpose Utilization of Mineral Resources,2012(3):52-54.
[5]黎卫亮,程秀花,张明祖,等.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,et al.Determination of gallium,indium,thallium,germanium and tellurium in geological samples by inductively coupled plasma mass spectrometry with ethanol as a signal enhancer[J].Metallurgical Analysis,2014,34(3):13-18.
[6]程秀花,黎卫亮,王海蓉,等.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,et al.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.
[7]张世涛.电感耦合等离子体质谱法测定铅锌矿中镓铟锗铊[J].化学与黏合,2014,36(6):460-462.ZHANG Shi-tao.Determination of Ga,In,Ge and Tl in lead-zinc ore by ICP-MS[J].Chemistry and Adhesion,2014,36(6):460-462.
[8]易晓明,李建文.电感耦合等离子体质谱法测定镉同位素时锡、钯、银等元素的干扰及其分离方法研究[J].冶金分析,2008,28(9):7-10.YI Xiao-ming,LI Jian-wen.Study on interference and separation of tin,palladium and silver in the determination of cadmium isotopes by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2008,28(9):7-10.
[9]陈波,刘洪青,刑应香.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.
[10]孙朝阳,董利明,贺颖婷,等.电感耦合等离子体质谱法测定地质样品中钪镓锗铟镉铊时的干扰及其消除方法[J].理化检验:化学分册,2016,52(9):1026-1030.SUN Chao-yang,DONG Li-ming,HE Ying-ting,et al.Elimination of interferences in ICP-MS determination of Sc,Ga,Ge,In,Cd and Tl in geological samples[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2016,52(9):1026-1030.
[11]岩石矿物分析编委会.岩石矿物分析[M].4版.北京:地质出版社,2011.