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针式微萃取结合GC-IRMS测定水溶液中甲酸、乙酸的稳定碳同位素组成 被引量:1
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作者 李心清 黄代宽 +4 位作者 章炎麟 江伟 安宁 胡璐 徐刚 《地球化学》 CAS CSCD 北大核心 2008年第6期549-555,共7页
甲酸和乙酸稳定碳同位素组成(δ13C)的分析对环境、食品、制药和自然产品等的研究具有重要的应用价值。但目前尚缺乏有效的测定方法。本研究利用最近出现的针式固相微萃取技术(NeedlEX),以吹扫-捕集方式对水溶液中的有机酸进行了萃取,... 甲酸和乙酸稳定碳同位素组成(δ13C)的分析对环境、食品、制药和自然产品等的研究具有重要的应用价值。但目前尚缺乏有效的测定方法。本研究利用最近出现的针式固相微萃取技术(NeedlEX),以吹扫-捕集方式对水溶液中的有机酸进行了萃取,然后利用气相色谱-同位素比值质谱联用仪(GC-IRMS)对所萃取的有机酸分子进行了δ13C的测定。结果显示,质谱计的信号强度与水溶液中有机酸的浓度存在显著的线性相关关系(R2>0.99,P<0.05),表明NeedlEX对水溶液中有机酸具有稳定的萃取能力。在甲酸与乙酸含量分别不低于300μg/mL与200μg/mL的水溶液中,1000mL的吹扫体积可以使两者δ13C多次分析结果的相对误差分别保持在3%和1%左右,且整个实验流程没有造成可检测的碳同位素分馏作用。低于这两个浓度界线,则分析误差随浓度的降低迅速增加。本研究虽然是针对水溶液中有机酸δ13C的测定,其萃取方法对其他水溶性挥发和半挥发有机物δ13C的分析也同样具有应用价值。 展开更多
关键词 低分子有机酸 针式固相微萃取 吹扫-捕集 碳同位素组成 连续流质谱
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An online method to determine chlorine stable isotope composition by continuous flow isotope ratio mass spectrometry (CF-IRMS) coupled with a Gasbench Ⅱ 被引量:3
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作者 刘运德 周爱国 +3 位作者 甘义群 刘存富 余婷婷 李小倩 《Journal of Central South University》 SCIE EI CAS 2013年第1期193-198,共6页
An online method using continuous flow isotope ratio mass spectrometry (CF-IRMS) interfaced with a Gasbench Ⅱ was presented to determine chlorine stable isotope composition. Silver chloride (AgCl) was quantitativ... An online method using continuous flow isotope ratio mass spectrometry (CF-IRMS) interfaced with a Gasbench Ⅱ was presented to determine chlorine stable isotope composition. Silver chloride (AgCl) was quantitatively derived from chloride by using silver nitrate (AgNO3), and then was reacted with iodomethane (CH3Ⅰ) to produce methyl chloride (CH3Cl). A GasBench Ⅱ equipped with a PoraPlot Q column was used to separate CH3Cl from any other gas species. Finally, chlorine stable isotope analysis was carried out on CH3Cl introduced to the IRMS in a helium stream via an active open split. The minimum amount of Cl used in this method is of the order of 1.4 μmol. Inter-laboratory and inter-technique comparisons show that the total uncertainty incorporating both the precision and accuracy of this method is better than 0.007%. Furthermore, ten seawaters sampled from different locations have a narrow δ37Cl value range from -0.008% to 0.010%, with a mean value of (0.000±0.006)%. This supports the assumption that any seawater can be representative of standard mean ocean chloride (SMOC) and used as an international reference material. 展开更多
关键词 chlorine stable isotope continuous flow isotope ratio mass spectrometry CF-IRMS GasBench
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