同位素双稀释剂法的原理与应用Ⅱ:应用部分
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摘要
为了使国内研究人员更为深入的了解双稀释剂法的原理和应用,本文以~(74)Se+~(77)Se双稀释剂为例,详细介绍了双稀释剂法在应用过程中所涉及的双稀释剂配比优化、标定及高精度数据获取的方法和流程。并分别通过蒙特-卡洛数值优化方法和实测数据对~(74)Se+~(77)Se双稀释剂进行了配比的优化,得到了两单稀释剂间和双稀释剂与样品间最佳的取值范围:当~(74)Se_(spk)/~(77)Se_(spk)≈1时,~(77)Se_(spike)/~(78)Se_(sample)≈2为最优配比值,但~(77)Se_(spike)/~(78)Se_(sample)在1~4范围内,硒同位素的分析精度不受影响。基于双稀释的优化结果,对NIST SRM 3149、MH495、GBW(E)080215三种Se的标准溶液进行长期测定,相对于NIST SRM3149,δ~(82/76)Se值分别为0.00‰±0.10‰(2SD,n=65),-3.44‰±0.08‰(2SD,n=21)和-7.90‰±0.10‰(2SD,n=21)。通过与标准-样品匹配法和元素内标法获取的数据进行对比,双稀释剂法获取的数据具有更高的准确度和精密度,这为自然界微小同位素分馏过程的研究奠定了基础。
In order to let domestic researchers to deeply understand the principle and application of the isotopic double spike technique,methods and procedures for the proportion optimization and calibration of the double spike and the high precision data acquisition,which are associated with the application of the isotopic double spike technique,have been detailly introduced in this paper by taking the~(74)Se+~(77)Se double spike as an example. On the basis of the result of the Monte Carlo numerical optimization and measured data,the proportion optimization for the~(74)Se +~(77)Se double spike has been carried out. It is obtained that optimized ratios between the double spike and sample is about 2(~(77)Se_(spike)/~(78)Se_(sample)≈2) when the ratio between two single diluents is about 1(~(74)Se_(spk)/~(77)Se_(spk)≈1). If the~(77)Se_(spike)/~(78)Se_(sample)ratios vary from 1 to 4,the analytical precision of Se isotopic values( δ~(82/76)Se) is unaffected. Based on the accurate proportion optimization of the DS,the long-term measured δ~(82/76)Se values of the three standard solutions of NIST SRM 3149,MH495 and GBW( E) 080215 are 0. 00‰±0. 10‰( 2SD,n = 65),-3. 44‰ ± 0. 08‰( 2SD,n = 21),and-7. 88‰ ± 0. 10‰( 2SD,n = 21),respectively.Comparing to data obtained by using the standard-sample matching method and the inside element method,the data obtained by using the double spike technique have relative high accuracy and precision Therefore,the application of double spike can lay the foundation for studying small isotope fractionation process in nature.
In order to let domestic researchers to deeply understand the principle and application of the isotopic double spike technique,methods and procedures for the proportion optimization and calibration of the double spike and the high precision data acquisition,which are associated with the application of the isotopic double spike technique,have been detailly introduced in this paper by taking the~(74)Se+~(77)Se double spike as an example. On the basis of the result of the Monte Carlo numerical optimization and measured data,the proportion optimization for the~(74)Se +~(77)Se double spike has been carried out. It is obtained that optimized ratios between the double spike and sample is about 2(~(77)Se_(spike)/~(78)Se_(sample)≈2) when the ratio between two single diluents is about 1(~(74)Se_(spk)/~(77)Se_(spk)≈1). If the~(77)Se_(spike)/~(78)Se_(sample)ratios vary from 1 to 4,the analytical precision of Se isotopic values( δ~(82/76)Se) is unaffected. Based on the accurate proportion optimization of the DS,the long-term measured δ~(82/76)Se values of the three standard solutions of NIST SRM 3149,MH495 and GBW( E) 080215 are 0. 00‰±0. 10‰( 2SD,n = 65),-3. 44‰ ± 0. 08‰( 2SD,n = 21),and-7. 88‰ ± 0. 10‰( 2SD,n = 21),respectively.Comparing to data obtained by using the standard-sample matching method and the inside element method,the data obtained by using the double spike technique have relative high accuracy and precision Therefore,the application of double spike can lay the foundation for studying small isotope fractionation process in nature.
引文
Arnold T,Schonbachler M,Rehkamper M,Dong S,Zhao F J,Kirk G JD,Coles B J,Weiss D J.2010.Measurement of zinc stable isotope ratios in biogeochemical matrices by double-spike MC-ICPMS and determination of the isotope ratio pool available for plants from soil.Analytical and Bioanalytical Chemistry,398(7-8):3115-3125
Carignan J,Wen H J.2007.Scaling NIST SRM 3149 for Se isotope analysis and isotopic variations of natural samples.Chemistry Geology,242(3-4):347-350
Coath C D,Elliott T,Hin R C.2016.Double-spike inversion for three-isotope systems.Chemical Geology,2017,451:78-89,doi:10.1016/j.chemgeo.2016.12.025
Cumming G L.1973.Propagation of experimental errors in lead isotope ratio measurements using the double spike method.Chemical Geology,11(3):157-165
Dodson M H.1963.A theoretical study of the use of internal standards for precise isotopic analysis by the surface ionization technique:Part I-general first-order algebraic solutions.Journal of Scientific Instruments,40(6):289-295
Elwaer N,Hintelmann H.2007.Comparative performance study of different sample introduction techniques for rapid and precise selenium isotope ratio determination using multi-collector inductively coupled plasma mass spectrometry(MC-ICP/MS).Analytical and Bioanalytical Chemistry,389(6):1889-1899
Gall L,Williams H,Siebert C,Hallida A.2012.Determination of massdependent variations in nickel isotope compositions using double spiking and MC-ICPMS.Journal of Analytical Atomic Spectrometry,27(1):137-145
Gueguen B,Rouxel O,Ponzevera E,Bekker A,Fouquet Y.2013.Nickel isotope variations in terrestrial silicate rocks and geological reference materials measured by MC-ICP-MS.Geostandards and Geoanalytical Research,37(3):297-317
Hamelin B,Manhes G,Albarede F,Allègre C J.1985.Precise lead isotope measurements by the double spike technique:Areconsideration.Geochimica et Cosmochimica Acta,49(1):173-182.
He Y S,Ke S,Teng F Z,Wang T T,Wu H J,Lu Y H,Li S G.2015.High-precision iron isotope analysis of geological reference materials by high-resolution MC-ICP-MS.Geostandards and Geoanalytical Research,39(3):341-356
John S G.2012.Optimizing sample and spike concentrations for isotopic analysis by double-spike ICPMS.Journal of Analytical Atomic Spectrometry,27(12):2123-2131
Johnson T M,Herbel M J,Bullen T D,Zawislanski P T.1999.Selenium isotope ratios as indicators of selenium sources and oxyanion reduction.Geochimica et Cosmochimica Acta,63(18):2775-2783
Maréchal C,Télouk P,Albarède F.1999.Precise analysis of copper and zinc isotopic compositions by plasma-source mass spectrometry.Chemical Geology,156(1-4):251-273
Mead C,Johnson T M.2010.Hg stable isotope analysis by the doublespike method.Analytical and Bioanalytical Chemistry,397(4):1529-1538
Ripperger S,Rehkamper M,Porcelli D,Halliday A N.2007.Cadmium isotope fractionation in seawater-a signature of biological activity.Earth and Planetary Science Letters,261(3-4):670-684
Rouxel O,Ludden J,Carignan J,Marin L,Fouquet Y.2002.Natural variations of Se isotopic composition determined by hydride generation multiple collector inductively coupled plasma mass spectrometry.Geochimica et Cosmochimica Acta,66(18):3191-3199
Rudge J F,Reynolds B C,Bourdon B.2009.The double spike toolbox.Chemical Geology,265(3-4):420-431
Schoenberg R,von Blanckenburg F.2005.An assessment of the accuracy of stable Fe isotope ratio measurements on samples with organic and inorganic matrices by high-resolution multicollector ICP-MS.International Journal of Mass Spectrometry,242(2-3):257-272
Siebert C,Nagler T F,Kramers J D.2001.Determination of molybdenum isotope fractionation by double-spike multicollector inductively coupled plasma mass spectrometry.Geochemistry,Geophysics,Geosystems,2(7):1032
Thirlwall M F.2002.Multicollector ICP-MS analysis of Pb isotopes using a207Pb-204Pb double spike demonstrates up to 400×10-6/AMUsystematic errors in Tl-normalization.Chemical Geology,184(3-4):255-279
White W M,Albarède F,Télouk P.2000.High-precision analysis of Pb isotope ratios by multi-collector ICP-MS.Chemical Geology,167(3-4):257-270
Woodhead J D,Hergt J M.1997.Application of the‘double spike'technique to Pb-isotope geochronology.Chemical Geology,138(3-4):311-321
Zhu H L,Zhang Z F,Wang G Q,Liu Y H,Liu F,Li X,Sun W D.2016.Calcium isotopic fractionation during ion-exchange column chemistry and thermal ionisation mass spectrometry(TIMS)determination.Geostandards and Geoanalytical Research,40(2):185-194
Zhu J M,Johnson T M,Clark S K,Zhu X K.2008.High precision measurement of selenium isotopic composition by hydride generation multiple collector inductively coupled plasma mass spectrometry with a74Se-77Se double spike.Chinese Journal of Analytical Chemistry,36(10):1385-1390
Zhu J M,Johnson T M,Clark S K,Zhu X K,Wang X L.2014.Selenium redox cycling during weathering of Se-rich shales:A selenium isotope study.Geochimica et Cosmochimica Acta,126:228-249
Zhu X K,O'Nions R K,Guo Y,Belshaw N S,Rickard D.2000.Determination of natural Cu-isotope variation by plasma-source mass spectrometry:Implications for use as geochemical tracers.Chemical Geology,163(1-4):139-149
Zhu X K,Guo Y,Williams R J P,O'Nions R K,Matthews A,Belshaw N S,Canters G W,de Waal E C,Weser U,Burgess B K,Salvato B.2002.Mass fractionation processes of transition metal isotopes.Earth and Planetary Science Letters,200(1-2):47-62
Zink S,Schoenberg R,Staubwasser M.2010.Isotopic fractionation and reaction kinetics between Cr(Ⅲ)and Cr(Ⅵ)in aqueous media.Geochimica et Cosmochimica Acta,74(20):5729-5745
蒋少涌,陆建军,顾连兴,华仁民,姜耀辉.2001.多接收电感耦合等离子体质谱(MC-ICPMS)测量铜、锌、铁的同位素组成及其地质意义.矿物岩石地球化学通报,20(4):431-433
李津,朱祥坤,唐索寒.2011.双稀释剂法在非传统稳定同位素测定中的应用-以钼同位素为例.岩矿测试,30(2):138-143
谭德灿,朱建明,王静,陶发祥,曾理.2016.同位素双稀释剂法的原理与应用I:原理部分.矿物岩石地球化学通报,35(1):138-145
朱建明,谭德灿,王静,曾理.2015.硒同位素地球化学研究进展与应用.地学前缘,22(5):102-114
Carignan J,Wen H J.2007.Scaling NIST SRM 3149 for Se isotope analysis and isotopic variations of natural samples.Chemistry Geology,242(3-4):347-350
Coath C D,Elliott T,Hin R C.2016.Double-spike inversion for three-isotope systems.Chemical Geology,2017,451:78-89,doi:10.1016/j.chemgeo.2016.12.025
Cumming G L.1973.Propagation of experimental errors in lead isotope ratio measurements using the double spike method.Chemical Geology,11(3):157-165
Dodson M H.1963.A theoretical study of the use of internal standards for precise isotopic analysis by the surface ionization technique:Part I-general first-order algebraic solutions.Journal of Scientific Instruments,40(6):289-295
Elwaer N,Hintelmann H.2007.Comparative performance study of different sample introduction techniques for rapid and precise selenium isotope ratio determination using multi-collector inductively coupled plasma mass spectrometry(MC-ICP/MS).Analytical and Bioanalytical Chemistry,389(6):1889-1899
Gall L,Williams H,Siebert C,Hallida A.2012.Determination of massdependent variations in nickel isotope compositions using double spiking and MC-ICPMS.Journal of Analytical Atomic Spectrometry,27(1):137-145
Gueguen B,Rouxel O,Ponzevera E,Bekker A,Fouquet Y.2013.Nickel isotope variations in terrestrial silicate rocks and geological reference materials measured by MC-ICP-MS.Geostandards and Geoanalytical Research,37(3):297-317
Hamelin B,Manhes G,Albarede F,Allègre C J.1985.Precise lead isotope measurements by the double spike technique:Areconsideration.Geochimica et Cosmochimica Acta,49(1):173-182.
He Y S,Ke S,Teng F Z,Wang T T,Wu H J,Lu Y H,Li S G.2015.High-precision iron isotope analysis of geological reference materials by high-resolution MC-ICP-MS.Geostandards and Geoanalytical Research,39(3):341-356
John S G.2012.Optimizing sample and spike concentrations for isotopic analysis by double-spike ICPMS.Journal of Analytical Atomic Spectrometry,27(12):2123-2131
Johnson T M,Herbel M J,Bullen T D,Zawislanski P T.1999.Selenium isotope ratios as indicators of selenium sources and oxyanion reduction.Geochimica et Cosmochimica Acta,63(18):2775-2783
Maréchal C,Télouk P,Albarède F.1999.Precise analysis of copper and zinc isotopic compositions by plasma-source mass spectrometry.Chemical Geology,156(1-4):251-273
Mead C,Johnson T M.2010.Hg stable isotope analysis by the doublespike method.Analytical and Bioanalytical Chemistry,397(4):1529-1538
Ripperger S,Rehkamper M,Porcelli D,Halliday A N.2007.Cadmium isotope fractionation in seawater-a signature of biological activity.Earth and Planetary Science Letters,261(3-4):670-684
Rouxel O,Ludden J,Carignan J,Marin L,Fouquet Y.2002.Natural variations of Se isotopic composition determined by hydride generation multiple collector inductively coupled plasma mass spectrometry.Geochimica et Cosmochimica Acta,66(18):3191-3199
Rudge J F,Reynolds B C,Bourdon B.2009.The double spike toolbox.Chemical Geology,265(3-4):420-431
Schoenberg R,von Blanckenburg F.2005.An assessment of the accuracy of stable Fe isotope ratio measurements on samples with organic and inorganic matrices by high-resolution multicollector ICP-MS.International Journal of Mass Spectrometry,242(2-3):257-272
Siebert C,Nagler T F,Kramers J D.2001.Determination of molybdenum isotope fractionation by double-spike multicollector inductively coupled plasma mass spectrometry.Geochemistry,Geophysics,Geosystems,2(7):1032
Thirlwall M F.2002.Multicollector ICP-MS analysis of Pb isotopes using a207Pb-204Pb double spike demonstrates up to 400×10-6/AMUsystematic errors in Tl-normalization.Chemical Geology,184(3-4):255-279
White W M,Albarède F,Télouk P.2000.High-precision analysis of Pb isotope ratios by multi-collector ICP-MS.Chemical Geology,167(3-4):257-270
Woodhead J D,Hergt J M.1997.Application of the‘double spike'technique to Pb-isotope geochronology.Chemical Geology,138(3-4):311-321
Zhu H L,Zhang Z F,Wang G Q,Liu Y H,Liu F,Li X,Sun W D.2016.Calcium isotopic fractionation during ion-exchange column chemistry and thermal ionisation mass spectrometry(TIMS)determination.Geostandards and Geoanalytical Research,40(2):185-194
Zhu J M,Johnson T M,Clark S K,Zhu X K.2008.High precision measurement of selenium isotopic composition by hydride generation multiple collector inductively coupled plasma mass spectrometry with a74Se-77Se double spike.Chinese Journal of Analytical Chemistry,36(10):1385-1390
Zhu J M,Johnson T M,Clark S K,Zhu X K,Wang X L.2014.Selenium redox cycling during weathering of Se-rich shales:A selenium isotope study.Geochimica et Cosmochimica Acta,126:228-249
Zhu X K,O'Nions R K,Guo Y,Belshaw N S,Rickard D.2000.Determination of natural Cu-isotope variation by plasma-source mass spectrometry:Implications for use as geochemical tracers.Chemical Geology,163(1-4):139-149
Zhu X K,Guo Y,Williams R J P,O'Nions R K,Matthews A,Belshaw N S,Canters G W,de Waal E C,Weser U,Burgess B K,Salvato B.2002.Mass fractionation processes of transition metal isotopes.Earth and Planetary Science Letters,200(1-2):47-62
Zink S,Schoenberg R,Staubwasser M.2010.Isotopic fractionation and reaction kinetics between Cr(Ⅲ)and Cr(Ⅵ)in aqueous media.Geochimica et Cosmochimica Acta,74(20):5729-5745
蒋少涌,陆建军,顾连兴,华仁民,姜耀辉.2001.多接收电感耦合等离子体质谱(MC-ICPMS)测量铜、锌、铁的同位素组成及其地质意义.矿物岩石地球化学通报,20(4):431-433
李津,朱祥坤,唐索寒.2011.双稀释剂法在非传统稳定同位素测定中的应用-以钼同位素为例.岩矿测试,30(2):138-143
谭德灿,朱建明,王静,陶发祥,曾理.2016.同位素双稀释剂法的原理与应用I:原理部分.矿物岩石地球化学通报,35(1):138-145
朱建明,谭德灿,王静,曾理.2015.硒同位素地球化学研究进展与应用.地学前缘,22(5):102-114