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Citation: MA Yu-Hua, HE Ming, ZENG You-Shi, ZHAO Jian-Chang, PANG Yi-Jun, QIN Lai-Lai, DENG Ke, LIU Jia-Yu, ZHANG Qin, YANG Guo, MA Zhao-Wei, LIU Wei, LI Yan. Sample Preparation for Quantitation of Non-exchangeable Organically Bound Tritium in Tree Rings by Accelerator Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(4): 620-626. doi: 10.19756/j.issn.0253-3820.171349 shu

Sample Preparation for Quantitation of Non-exchangeable Organically Bound Tritium in Tree Rings by Accelerator Mass Spectrometry

MA Yu-Hua ^1,2,3, ,
HE Ming ⁴ ,
ZENG You-Shi ¹ ,
ZHAO Jian-Chang ⁴ ,
PANG Yi-Jun ⁴ ,
QIN Lai-Lai ^1,2 ,
DENG Ke ^1,2 ,
LIU Jia-Yu ^1,2 ,
ZHANG Qin ^1,2 ,
YANG Guo ^1,2 ,
MA Zhao-Wei ^1,2 ,
LIU Wei ¹ ,
LI Yan ^1,3

1.
Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800, China;
2.
University of Chinese Academy of Sciences, Beijing 100049, China;
3.
School of Physical Science and Technology, Shanghai Tech University, Shanghai 201210, China;
4.
China Institute of Atomic Energy, Beijing 102413, China

Received Date: 17 October 2017
Revised Date: 28 February 2019

Fund Project: This work was supported by the National Natural Science Foundation of China (No.11705265).

Tree rings can reflect the environmental conditions during tree growing period. The celluloses of tree rings will not be reutilized for energy. The nonexchangeable organically bound tritium (NE-OBT) in celluloses has no liquidity and no exchange with other things, so it can accurately reflect the historical tritium level in the local environment. The measurement of NE-OBT in tree rings using accelerator mass spectrometer (AMS) needs only 10 mg of celluloses and a 200-s measurement time, which is more suitable compared with liquid scintillation counter (LSC). In this study, the principle of sample preparation for AMS NE-OBT measurement of tree rings was systematically studied. Through modification of the extraction methods for cellulose, the purity of cellulose was raised from 64.8% to 83.9%. With the developed two-step method, the cellulose was transformed into titanium hydride which could be measured using accelerator mass spectrometry directly. By strictly controlling the combustion cellulose amounts between 10.00 and 10.05 mg, extending the combustion time from 4 h to 10 h, strictly controlling the water transfer time in the vacuum system above 1 min and the cold trap temperature between -88℃ to -80℃, and cooling down with an open door, etc., the isotopic fraction effect during sample pretreatment was depressed and stabilized. Measurement results of 10⁵-10⁷ TU standard samples by LSC and AMS were treating with linear regression on the double logarithmic axis. After fitting, the correlation coefficient R² reached 0.99912. These results proved that the prepared sample by this method could be used for measurement by accelerator mass spectrometry. Accurate measurement could be obtained after calibration with multi-level standards.
- Accelerator mass spectrometry,
- Tree rings,
- Cellulose extraction method,
- Non-exchangeable organically bound tritium,
- Isotope fractionation
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