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測(cè)試項(xiàng)目：Sr同位素測(cè)試對(duì)象：長(zhǎng)石、單斜輝石、磷灰石、碳酸鹽巖等測(cè)試周期：來電詳詢送樣要求：1、樣品靶或巖石薄片，薄片尺寸參見原位主微量元素分析要求；2、長(zhǎng)石樣品Sr含量大于200ppm，單斜輝石樣品Sr含量大于80ppm；3、樣品貧Rb，Rb/Sr含量比低于0.1，大于此范圍的樣品請(qǐng)?zhí)崆案嬷?/p>

詳細(xì)介紹

測(cè)試項(xiàng)目：Sr同位素

測(cè)試對(duì)象：長(zhǎng)石、單斜輝石、磷灰石、碳酸鹽巖等
測(cè)試周期：來電詳詢
送樣要求：1、樣品靶或巖石薄片，薄片尺寸參見原位主微量元素分析要求；2、長(zhǎng)石樣品Sr含量大于200ppm，單斜輝石樣品Sr含量大于80ppm；3、樣品貧Rb，Rb/Sr含量比低于0.1，大于此范圍的樣品請(qǐng)?zhí)崆案嬷?br>完成標(biāo)準(zhǔn)：測(cè)試內(nèi)精度及標(biāo)樣外精度和準(zhǔn)確度確保達(dá)到國(guó)際水平。

方法描述：

20.1長(zhǎng)石，單斜輝石和磷灰石LA-MC-ICP-MS微區(qū)原位Sr同位素比值測(cè)試

微區(qū)原位長(zhǎng)石，單斜輝石和磷灰石Sr同位素比值測(cè)試在武漢上譜分析科技有限責(zé)任公司利用激光剝蝕多接收杯電感耦合等離子體質(zhì)譜（LA-MC-ICP-MS）完成。激光剝蝕系統(tǒng)為Geolas HD（Coherent，德國(guó)），MC-ICP-MS為Neptune Plus（Thermo Fisher Scientific，德國(guó)）。8個(gè)法拉第杯（從L4到H3）被同時(shí)用于接收Kr，Rb，Er⁺⁺，Yb⁺⁺和Sr信號(hào)的離子信號(hào)。Jet+X錐組合被采用以提高儀器靈敏度。激光剝蝕系統(tǒng)使用氦氣作為載氣。分析采用單點(diǎn)模式，激光束斑大小根據(jù)樣品Sr信號(hào)強(qiáng)度調(diào)節(jié)，一般為60-160 μm。激光剝蝕速率為8-15 Hz。激光能量密度固定在~10.0 J/cm²。分析過程配備了信號(hào)平滑裝置以提高信號(hào)穩(wěn)定性和同位素比值測(cè)試精密度（Hu et al. 2015）。全部分析數(shù)據(jù)采用專業(yè)同位素?cái)?shù)據(jù)處理軟件“Iso-Compass”進(jìn)行數(shù)據(jù)處理（Zhang et al., 2020）。Sr同位素干擾校正采用Tong et al.（2016）和Zhang et al.（2018）的方法。校正首先扣除氣體背景Kr干擾。接下來校正方案為（1）監(jiān)控¹⁶⁷Er⁺⁺, ¹⁷³Yb⁺⁺信號(hào)強(qiáng)度，利用Er和Yb天然豐度比值（Berglund and Wieser, 2011），扣除¹⁶⁸Er⁺⁺ 對(duì)⁸⁴Sr，¹⁷⁰Er⁺⁺和¹⁷⁰Yb⁺⁺對(duì)⁸⁵Rb，¹⁷²Yb⁺⁺對(duì)⁸⁶Sr，以及¹⁷⁴Yb⁺⁺對(duì)⁸⁷Sr的干擾;（2）監(jiān)測(cè)⁸⁵Rb信號(hào)強(qiáng)度，利用實(shí)驗(yàn)獲得的經(jīng)驗(yàn)⁸⁷Rb/⁸⁵Rb比值和指數(shù)法則，校正⁸⁷Rb對(duì)⁸⁷Sr的干擾。經(jīng)驗(yàn)⁸⁷Rb/⁸⁵Rb比值通過測(cè)定高Rb且已知⁸⁷Sr/⁸⁶Sr組成的標(biāo)準(zhǔn)樣品獲得。Sr同位素儀器質(zhì)量分餾校正通過指數(shù)法則校正，校正因子利用⁸⁸Sr/⁸⁶Sr = 8.375209估算獲得（Tong et al. 2016, Zhang et al. 2018）。
兩個(gè)天然長(zhǎng)石標(biāo)樣，YG0440（鈉長(zhǎng)石）和YG4301（鈣長(zhǎng)石），作為未知樣品監(jiān)控微區(qū)原位長(zhǎng)石Sr同位素校正方法的可靠性。YG0440和YG4301的化學(xué)組成和Sr同位素組成參見Zhang et al.（2018）。
一個(gè)天然單斜輝石標(biāo)樣，HNB-8（Sr=89.2 µg g^-1），作為未知樣品監(jiān)控微區(qū)原位單斜輝石Sr同位素校正方法的可靠性。HNB-8的化學(xué)組成和Sr同位素組成參見Tong et al.（2016）。
兩個(gè)天然磷灰石標(biāo)樣，Durango和MAD，作為未知樣品監(jiān)控微區(qū)原位磷灰石Sr同位素校正方法的可靠性。Durango和MAD的化學(xué)組成和Sr同位素組成參見Yang et al.（2014）。

20.2 In situ Sr isotope analysis of feldspar, clinopyroxene and apatite by using LA-MC-ICP-MS

Sr isotope ratios of feldspars, clinopyroxenes and apatites were measured by a Neptune Plus MC-ICP-MS (Thermo Fisher Scientific, Bremen, Germany) in combination with a Geolas HD excimer ArF laser ablation system (Coherent, Göttingen, Germany) at the Wuhan Sample Solution Analytical Technology Co., Ltd, Hubei, China. The Neptune Plus was equipped with nine Faraday cups fitted with 10¹¹ Ω resistors. The Faraday collector configuration of the mass system was composed of an array from L4 to H3 to monitor Kr, Rb, Er, Yb and Sr. The combination of the high-sensitivity X-skimmer cone and Jet-sample cone was employed. In the laser ablation system, helium was used as the carrier gas for the ablation cell. For a single laser spot ablation, the spot diameter ranged from 60 to 160 μm dependent on Sr signal intensity. The pulse frequency was from 8 to 15 Hz, but the laser fluence was kept constant at ~10 J/cm². A new signal smoothing device (Hu et al. 2015) was used downstream from the sample cell to eliminate the short-term variation of the signal. All data reduction for the MC-ICP-MS analysis of Sr isotope ratios was conducted using “Iso-Compass” software (Zhang et al. 2020). The interference correction strategy was the same as the one reported by Tong et al. (2016) ａnd Zhang et al. (2018). Firstly, the regions of integration for both gas background and sample were selected. Following background correction, which removes the background Kr⁺ signals, no additional Kr peak stripping was applied. Interferences were corrected in the following sequence: (1) the interferences of ¹⁶⁸Er⁺⁺ on ⁸⁴Sr, ¹⁷⁰Er⁺⁺ ａnd ¹⁷⁰Yb⁺⁺ on ⁸⁵Rb, ¹⁷²Yb⁺⁺ on ⁸⁶Sr, and ¹⁷⁴Yb⁺⁺ on ⁸⁷Sr were corrected based on the measured signal intensities of ¹⁶⁷Er⁺⁺, ¹⁷³Yb⁺⁺ ａnd the natural isotope ratios of Er and Yb (Berglund and Wieser, 2011); (2) the isobaric interference of ⁸⁷Rb on ⁸⁷Sr was corrected by monitoring the ⁸⁵Rb signal intensity and a user-specified ⁸⁷Rb/⁸⁵Rb ratio using an exponential law for mass bias. The user-specified ⁸⁷Rb/⁸⁵Rb ratio was calculated by measuring some reference materials with a known ⁸⁷Sr/⁸⁶Sr ratio. Following the interference corrections, mass fractionation of Sr isotopes was corrected by assuming ⁸⁸Sr/⁸⁶Sr = 8.375209 (Tong et al. 2016 and Zhang et al. 2018) and applying the exponential law.
During the LA-MC-ICP-MS analysis, a synthesised clinopyroxene glass (CPX05G, Sr = 518 µg g^-1) was used as monitor to verify the accuracy of the calibration method. Two silicate glasses of StHs6/80-G and T1-G (MPI-DING), that both have high concentration of Rb, were used to calculated a specified 87Rb/85Rb ratio for the Rb interference correction.
Two natural feldspar megacrysts, YG0440 (albite) and YG4301 (anorthite) were used as the unknown samples to verify the accuracy of the calibration method for in situ Sr isotope analysis of feldspars. The chemical and Sr isotopic compositions of YG0440 and YG4301 have been reported by Zhang et al. (2018).
A natural clinopyroxene megacryst (Cpx, HNB-8) with a low Sr concentration (89.2 µg g^-1) was analyzed as the unknown sample for in situ Sr isotope analysis of Cpx samples. The chemical and Sr isotopic compositions of HNB-8 have been reported by Tong et al. (2016).
Two natural apatites, Durango and MAD were used as the unknown samples for in situ Sr isotope analysis of apatites. The chemical and Sr isotopic compositions of Durango and MAD have been reported by Yang et al. (2014).
References
Hu, Z.C., Zhang, W., Liu, Y.S., Gao, S., Li, M., Zong, K.Q., Chen, H.H., Hu, S.H., 2015. “Wave” Signal-Smoothing and Mercury-Removing Device for Laser Ablation Quadrupole and Multiple Collector ICPMS Analysis: Application to Lead Isotope Analysis. Analytical Chemistry, 87(2), 1152–1157.
Liu, Y.S., Gao, S., Hu, Z.C., Gao, C.G., Zong, K.Q. and Wang, D.B., 2010. Continental and oceanic crust recycling-induced melt-peridotite interactions in the Trans-North China Orogen: U-Pb dating, Hf isotopes and trace elements in zircons of mantle xenoliths. Journal of Petrology, 51(1–2): 537–571.
Tong X.R., Liu Y.S., Hu Z.C., Chen H.H., Zhou L., Hu Q.H., Xu R., Deng L.X., Chen C.F., Yang L., Gao S., 2016. Accurate determination of Sr isotopic compositions in clinopyroxene and silicate glasses by LA-MC-ICP-MS. Geostandards and Geoanalytical Research, 40(1): 85–99.
Zhang, W., Hu, Z., Liu, Y., Wu, T., Deng, X., Guo, J., Han Zhao, 2018. Improved in situ Sr isotopic analysis by a 257 nm femtosecond laser in combination with the addition of nitrogen for geological minerals. Chemical Geology, 479: 10–21.
Berglund M. and Wieser M.E. (2011) Isotopic compositions of the elements 2009 (IUPAC Technical Report). Pure and Applied Chemistry, 83, 397–410.
Yang Y.H., Wu F.Y., Yang J.H., Chew D.M., Xie L.W., Chu Z.Y., Zhang Y.B., Huang C., 2014. Sr and Nd isotopic compositions of apatite reference materials used in U-Th-Pb geochronology. Chemical Geology, 385: 35–55.
Zhang W., Hu Z.C., Liu Y.S. (2020). Iso-Compass: new freeware software for isotopic data reduction of LA-MC-ICP-MS. J. Anal. At. Spectrom., 2020, 35, 1087–1096.

關(guān)鍵詞：標(biāo)準(zhǔn) 等離子體質(zhì)譜