应用GasBench Ⅱ-IRMS优化碳氧同位素分析方法

朱园园; 邱海鸥; 杜永; 汤志勇; 帅琴; 宋虎跃

应用GasBench Ⅱ-IRMS优化碳氧同位素分析方法

1.
武汉地质矿产研究所, 湖北武汉 430205

2.
中国地质大学(武汉)材料与化学学院, 湖北武汉 430074

3.
十堰市环境保护监测站, 湖北十堰 442000

4.
中国地质大学(武汉)生物地质与环境地质国家重点实验室, 湖北武汉 430074

基金项目: 国家自然基金项目资助(41172312;41402302);生物地质与环境地质国家重点实验室自主课题资助(GKZ14Y663)

详细信息

作者简介: 宋虎跃, 讲师, 从事稳定同位素分析测试及古环境应用研究. E-mail: shycug@gmail.com

中图分类号: O657.63;O628.21

收稿日期: 2014-06-10

修回日期: 2014-10-25

录用日期: 2014-11-15

刊出日期: 2014-06-25

Evaluation and Optimization of Carbon and Oxygen Isotopes Experimental Conditions Determinated by GasBenchⅡ-IRMS Method

1.
Wuhan Institute of Geology and Mineral Resources, Wuhan 430205, China

2.
School of Material and Chemistry, China University of Geosciences (Wuhan), Wuhan 430074, China

3.
Environmental Protection Monitoring Station of Shiyan, Shiyan 442000, China

4.
State Key Laboratory of Biogeology and Environmental Geology, China University of Geosciences (Wuhan), Wuhan 430074, China

Received Date: 10 June 2014

Revised Date: 25 October 2014

Accepted Date: 15 November 2014

Publish Date: 25 June 2014

摘要

摘要:
GasBenchⅡ-连续流稳定同位素质谱仪(IRMS)联用在线分析已成为碳酸盐碳氧同位素分析测试的常用方法, 已有研究认为不同的实验条件直接影响δ¹³C和δ¹⁸O同位素测试结果的准确性。但这些报道未对该联用方法所涉及的实验条件进行综合分析。本文系统研究了GasBenchⅡ-IRMS法中各种实验条件(包括排空时间、反应温度、反应时间和色谱分离温度)对碳氧同位素测试结果的综合影响。结果表明:排空时间大于9 min可有效消除空气对测试结果的干扰, 不同的反应温度和时间对碳氧同位素分析结果均有一定影响, 经条件优化确定反应温度为72℃, 反应时间为60 min, 色谱分离温度为60℃。在优化的实验条件下, 碳氧同位素分析精度分别优于0.03‰和0.05‰, 达到了国际分析测试水平。同时, 选择合适的同位素数据归一化方法可以进一步保证碳氧同位素测试结果的准确性和可靠性。通过分析近4000件实际样品, 对比单一标准物质校准和双标准物质校准同位素归一化方法的计算结果, 发现双标准物质校准偏差小于单一标准物质校准偏差, 因此建议采用双标准物质校准法进行样品同位素标准化计算。本研究为GasBenchⅡ-IRMS联用技术中实验条件的选取提供了一定的参考, 保证碳氧同位素测试结果的可靠性和准确性。同时提出, 由于样品成分复杂且不均一, 在分析实际样品时需要根据样品的性质进一步对实验条件进行考察。
- GasBench Ⅱ-IRMS /
- 碳同位素 /
- 氧同位素 /
- 排空时间 /
- 反应温度 /
- 反应时间 /
- 色谱分离温度 /
- 同位素归一化方法
Abstract:
The continuous flow technique coupled with GasBenchⅡ-Isotope Ratio Mass Spectrometry (IRMS) became the routine method to analyse the stable carbon and oxygen isotope compositions of carbonate. Previous studies revealed that the isotope results were influenced by the varied experimental conditions. However, rare studies have assessed the influences of multiple experimental conditions on the isotope results. Here, all reaction conditions including flushing time, reaction temperature, reaction time and chromatographic separation temperature have been evaluated systematically. Flushing time longer than 9 minutes can eliminate the interference of air. Different reaction temperatures and time have distinct influences on the isotope values. 72℃, 60 minutes and 60℃ have been chosen for the reaction temperature, reaction time and chromatographic separation temperature respectively. The analytical precisions are better than 0.03‰ (for δ¹³C) and 0.05 (for δ¹⁸O) under the optimized conditions. In addition, different isotope normalization methods would affect the isotope results. Two isotope normalization methods have been compared, based on about 4000 samples of isotope data. The calculated results from two standard samples are much more precise and reliable than from single standard samples. The study provides a reference for experimental conditions in GasBench Ⅱ-IRMS technology, ensuring the accuracy and reliability for carbon and oxygen isotope analysis. At the same time, the experimental conditions should be further investigated in real samples analysis due to the inhomogeneous and complex sample compositions.
- GasBenchⅡ-IRMS /
- carbon isotope /
- oxygen isotope /
- flushing time, reaction temperature, reaction time /
- chromatographic separation temperature /
- isotope normalization method /
- /

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表 1 不同排空时间下石笋标准的碳氧同位素组成

Table 1. δ¹³C>and δ¹⁸Ocompositions of the stalagmite standard on varied flushing times

排空时间 (min)	δ¹³C_VPDB (‰)	SD (1σ, n=4)	δ¹⁸O_VPDB (‰)	SD (1σ, n=4)
1~7	存在空气次级峰		存在空气次级峰
9	-10.740	0.038	-8.567	0.010
11	-10.784	0.026	-8.480	0.010
12	-10.774	0.012	-8.563	0.004
13	-10.798	0.003	-8.574	0.010

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表 2 不同反应温度下石笋标准的碳氧同位素组成

Table 2. δ¹³C and δ¹⁸O compositions of the stalagmite standard on varied temperatures

反应温度 (℃)	δ¹³C_VPDB (‰)	SD (1σ, n=4)	δ¹⁸O_VPDB (‰)	SD (1σ, n=4)
50	-10.785	0.031	-8.588	0.024
60	-10.726	0.050	-8.629	0.013
72	-10.758	0.039	-8.550	0.027
80	-10.811	0.065	-8.577	0.022

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表 3 不同反应时间下石笋标准的碳氧同位素组成

Table 3. δ¹³C and δ¹⁸O compositions of the stalagmite standard on varied reaction times

反应时间 (min)	δ¹³C_VPDB (‰)	SD (1σ, n=4)	δ¹⁸O_VPDB (‰)	SD (1σ, n=4)
30	-10.776	0.009	-8.562	0.036
45	-10.749	0.046	-8.512	0.006
60	-10.765	0.036	-8.524	0.009
75	-10.760	0.011	-8.533	0.044
90	-10.944	0.036	-8.522	0.027

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表 4 不同色谱分离温度下石笋标准的碳氧同位素组成

Table 4. δ¹³Cand δ¹⁸Ocompositions of the stalagmite standard on varied chromatographic separation temperatures

色谱温度 (℃)	δ¹³C_VPDB (‰)	SD (1σ, n=4)	δ¹⁸O_VPDB (‰)	SD (1σ, n=4)
45	-10.823	0.050	-8.488	0.053
60	-10.811	0.024	-8.485	0.036
70	-10.760	0.024	-8.584	0.047

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应用GasBench Ⅱ-IRMS优化碳氧同位素分析方法

1. 武汉地质矿产研究所, 湖北 武汉 430205 2. 中国地质大学(武汉)材料与化学学院, 湖北 武汉 430074 3. 十堰市环境保护监测站, 湖北 十堰 442000 4. 中国地质大学(武汉)生物地质与环境地质国家重点实验室, 湖北 武汉 430074

作者简介: 宋虎跃, 讲师, 从事稳定同位素分析测试及古环境应用研究. E-mail: shycug@gmail.com

Evaluation and Optimization of Carbon and Oxygen Isotopes Experimental Conditions Determinated by GasBenchⅡ-IRMS Method

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目录

1.
武汉地质矿产研究所, 湖北武汉 430205

2.
中国地质大学(武汉)材料与化学学院, 湖北武汉 430074

3.
十堰市环境保护监测站, 湖北十堰 442000

4.
中国地质大学(武汉)生物地质与环境地质国家重点实验室, 湖北武汉 430074