【引用本文】 刘圣华, 史慧霞, 蒋雅欣, 等. 加速器质谱14C分析石墨制备技术研究进展[J]. 岩矿测试, 2019, 38(5): 584-598. doi: 10.15898/j.cnki.11-2131/td.201807100082
LIU Sheng-hua , SHI Hui-xia , JIANG Ya-xin , et al. Research Progress on Graphite Target Preparation for Accelerator Mass Spectrometry 14C Analysis[J]. Rock and Mineral Analysis, 2019, 38(5): 584-598. doi: 10.15898/j.cnki.11-2131/td.201807100082

加速器质谱14C分析石墨制备技术研究进展

1. 中国地质大学(北京)地球科学与资源学院, 北京 100083;

2. 中国地质科学院水文地质环境地质研究所, 河北 石家庄 050061;

3. 天津大学表层地球系统科学研究院, 天津 300072

收稿日期: 2018-07-10  修回日期: 2019-04-28 

基金项目: 中国地质科学院基本科研业务费资助项目(YYWF201517,SK201603)

作者简介: 刘圣华,硕士,研究实习员,主要从事同位素分析研究。E-mail:cuglsh@hotmail.com。。

Research Progress on Graphite Target Preparation for Accelerator Mass Spectrometry 14C Analysis

1. School of Earth Sciences and Resources, China University of Geosciences(Beijing), Beijing 100083, China;

2. Institute of Hydrology and Environmental Geology, China Academy of Geological Sciences, Shijiazhuang 050061, China;

3. Institute of Surface-Earth System Science, Tianjin University, Tianjin 300073, China

Received Date: 2018-07-10
Revised Date: 2019-04-28

摘要:加速器质谱(AMS)是进行14C同位素分析的主要技术手段,而高精度低本底加速器质谱14C分析主要受样品制备技术限制,因此探讨如何提高石墨制备的稳定性和控制碳污染降低本底将有助于产出高质量14C分析数据,突破14C测年上限(约5.0万年),进一步拓宽14C年代学和同位素示踪的应用范畴。本文详细阐述了催化还原法(H2/Fe法、Zn/Fe法和Zn-TiH2/Fe法)制备石墨样品的真空装置和主要工作原理,指出了微量样品石墨制备过程中同位素分馏、石墨产率、束流强度以及精密度与样品量之间存在严重的依赖关系及其抑制方法。着重探讨了石墨制备技术实验条件(还原剂、催化剂、温度等)的优化选择及其与石墨产率、同位素分馏、束流性能之间的内在联系,总结分析了碳污染来源并探寻合适的碳污染控制技术。目前的研究表明最佳实验条件为:H2/Fe法宜采用还原剂H2/CO2(体积比2~2.5),催化剂为源自氢还原单质铁粉(-325目球粒,Fe/C=2~5),温度500~550℃;Zn/Fe法宜采用还原剂Zn/C(质量比50~80),催化剂为源自氢还原单质铁粉(-325目球粒,Fe/C=2~5),Zn反应管温度400~450℃,Fe反应管温度500~550℃。碳污染来源于制备过程中的各个方面,除采用高温除碳的方式外还可采用适当的数学模型加以校正,但还需要更多详细的实验工作来加强现有认识,以期更好地消除碳污染对测试结果的影响。对测年目标组分不稳定的样品(如地下水中的溶解无机碳)应避免样品直接暴露于大气,以减少野外采样过程中现代大气CO2对测量结果的影响。

关键词: 加速器质谱, 14C, 石墨制备, 微量样品, 碳污染

Research Progress on Graphite Target Preparation for Accelerator Mass Spectrometry 14C Analysis

KEY WORDS: accelerator mass spectrometry, radiocarbon, graphite preparation, small (ultra-small) sample, carbon contamination

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加速器质谱14C分析石墨制备技术研究进展

刘圣华, 史慧霞, 蒋雅欣, 徐胜, 刘冰冰