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

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: LI Tie-Jun,
Received Date: 10 May 2012
Available Online: 6 August 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 (No.yg2011001)

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.
- Isoope ratio,
- Diatom,
- Stepwise fluorination,
- δ¹⁸O value
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沈阳化工大学材料科学与工程学院沈阳 110142