【引用本文】 金贵善, 刘汉彬, 韩娟, 等. 镀镍碳为还原剂在线高温裂解法测定硫酸钡中氧同位素组成[J]. 岩矿测试, 2019, 38(4): 365-372. doi: 10.15898/j.cnki.11-2131/td.201809090103
JIN Gui-shan , LIU Han-bin , HAN Juan , et al. Determination of Oxygen Isotopic Composition in Barium Sulfate by Online Pyrolysis Method with Nickel-plated Carbon as Reductant[J]. Rock and Mineral Analysis, 2019, 38(4): 365-372. doi: 10.15898/j.cnki.11-2131/td.201809090103

镀镍碳为还原剂在线高温裂解法测定硫酸钡中氧同位素组成

核工业北京地质研究院, 北京 100029

收稿日期: 2018-09-09  修回日期: 2019-03-11 

基金项目: 国家重点研发计划项目“华南热液型铀矿基地深部探测技术示范”(2017YFC0602600)

作者简介: 金贵善,高级工程师,主要从事同位素地球化学研究。E-mail:16626162@qq.com。。

通信作者:

Determination of Oxygen Isotopic Composition in Barium Sulfate by Online Pyrolysis Method with Nickel-plated Carbon as Reductant

Beijing Research Institute of Uranium Geology, Beijing 100029, China

Corresponding author: LIU Han-bin , 主要从事同位素地球化学研究。hanbinliu@sina.com。

Received Date: 2018-09-09
Revised Date: 2019-03-11

摘要:测定矿物或水中硫酸根的氧同位素组成(δ18O)能够识别物质来源及转化过程,常用的方法是将硫酸根转化为硫酸钡再用离线或在线法测试其δ18O值。目前普遍采用在1420℃在线测试硫酸钡的氧同位素组成,该方法极易缩短反应炉的寿命,通过添加还原剂碳可以降低反应温度,但是已有报道对于添加还原剂后的反应温度讨论较少。本文选择镀镍碳(Ni-C)作为还原剂,将样品经Ni-C高温处理后进行一系列条件实验,确认了采用元素分析仪-稳定同位素质谱仪(EA-IRMS)测定硫酸钡中氧同位素组成的分析方法的关键技术参数:硫酸钡在线反应温度为1350℃;Ni-C与硫酸钡样品量的质量比范围选择0.73~2.15;为了获得更加精确的数据,硫酸钡与Ni-C用量都控制在700±100μg。在以上实验条件下,EA/HT-IRMS测定硫酸钡δ18O值的精密度为±0.12‰~±0.26‰,优于在线法已报道的精密度±0.20‰~±0.50‰。本方法在满足测试精密度的前提下,通过添加Ni-C降低了硫酸钡在线反应温度,延长了反应炉使用寿命。

关键词: 硫酸钡, 元素分析-稳定同位素质谱法, 氧同位素, 镀镍碳, 在线高温裂解

Determination of Oxygen Isotopic Composition in Barium Sulfate by Online Pyrolysis Method with Nickel-plated Carbon as Reductant

KEY WORDS: barium sulfate, Elemental Analysis-Isotope Ratio Mass Spectrometry, oxygen isotope, nickel-plated carbon, online pyrolysis method

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镀镍碳为还原剂在线高温裂解法测定硫酸钡中氧同位素组成

金贵善, 刘汉彬, 韩娟, 李军杰, 张建锋, 张佳, 石晓