硅藻氧同位素比值测定的分步氟化处理方法

引用本文: 李铁军, 李洪伟, 刘秀金, 冯连君. 硅藻氧同位素比值测定的分步氟化处理方法[J]. 分析化学, 2012, 40(12): 1897-1901. doi: 10.3724/SP.J.1096.2012.20497 shu

Citation: LI Tie-Jun, LI Hong-Wei, LIU Xiu-Jin, FENG Lian-Jun. Stepwise Fluorination Method for Determination of Oxygen Isotopic Ratio of Diatoms[J]. Chinese Journal of Analytical Chemistry, 2012, 40(12): 1897-1901. doi: 10.3724/SP.J.1096.2012.20497 shu

硅藻氧同位素比值测定的分步氟化处理方法

通讯作者: 李铁军

基金项目:
本文系中国科学院仪器设备功能开发技术创新项目(No.yg2011001)资助 (No.yg2011001)

摘要: 利用硅酸盐氧同位素制备系统,以BrF₅为氟化剂,对硅藻试样和石英标样进行精细的分步氟化研究,揭示硅藻壳体不同层位氧同位素的变化特征。采用逐步氟化实验,确定了四龙湾玛珥湖沉积硅藻样品在去除25%-28%的外层氧后再完全氟化,IRMS(质谱仪)测定的δ¹⁸O集中度最高。将氟化流程简化为两步,对应的δ¹⁸O差别为0.3‰,测量精度优于±0.5‰。本研究确定了硅藻样品分步氟化方法:第一步,引入0.392 aK mL(a,样品质量(mg);K=0.18)的BrF₅(25℃)气体,在550℃下反应1 h;第二步,系统恢复真空后,引入理论量5倍的BrF₅,在550℃下反应3 h,产出的氧转化为CO₂进行质谱测定,获得硅藻δ¹⁸O特征值。

关键词:

同位素比
/ 硅藻
/ 分步氟化
/ δ¹⁸O

English

Stepwise Fluorination Method for Determination of Oxygen Isotopic Ratio of Diatoms

1.
Key Laboratory of Mineral Resources, Institute of Geology and Geophysics, Chinese Academy of Sciences, Beijing 100029, China

Corresponding author: 李铁军

Received Date: 10 May 2012
Fund Project:
本文系中国科学院仪器设备功能开发技术创新项目(No.yg2011001)资助

Abstract: Determination of the δ¹⁸O value of diatom can obtain the initial information of its oxygen isotopic composition, and also has favorable application prospects in paleoenvironment, paleontology, petroleum exploration and environmental prediction. We carried out eight-step fluorination experiments with BrF₅ reagent on diatom samples and quartz standard to reveal variation of oxygen isotopic composition in different steps. The eight-step fluorination determined the proportion of surface oxygen to be 25%-28%. The δ¹⁸O values obtained from the above processes were all around (35.34±0.15)‰. Then we simplified the eight-step fluorination to two-step fluorination. First, we removed the surface oxygen of specific sedimentary diatoms, and then totally fluoridated the samples. The difference of δ¹⁸O values from eight-step and two-step fluorination experiments on the same samples was only 0.3‰. The accuracy of measurement has reached or preceded the repeated measurement error of ±0.5‰ in the international studies. On the basis of many conditional experiments, the stepwise fluorination methods on the diatoms were established. For diatom samples with weight of a mg, the 0.392 aK mL (K=0.18) BrF₅ were loaded in the first step, and heated to 550℃ for 1 h; and then five times of theoretical quantity of BrF₅ were loaded in the second step after the system regain vacuum, and heated to 550℃ for 3 h. The released oxygen were converted to CO₂, and then analysed by MAT-252 to obtain δ¹⁸O value of diatom samples.

Key words:

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

硅藻氧同位素比值测定的分步氟化处理方法

通讯作者: 李铁军

English

Stepwise Fluorination Method for Determination of Oxygen Isotopic Ratio of Diatoms

Corresponding author: 李铁军

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

硅藻氧同位素比值测定的分步氟化处理方法

通讯作者: 李铁军

English

Stepwise Fluorination Method for Determination of Oxygen Isotopic Ratio of Diatoms

Corresponding author: 李铁军

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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