【引用本文】 李科, 张琳, 刘福亮, 等. 有机化学物质碳氮稳定同位素系列标准物质研制[J]. 岩矿测试, 2020, 39(5): 753-761. doi: 10.15898/j.cnki.11-2131/td.201905290074
LI Ke, ZHANG Lin, LIU Fu-liang, et al. Preparation of Reference Materials for Carbon and Nitrogen Isotopes of Organic Materials[J]. Rock and Mineral Analysis, 2020, 39(5): 753-761. doi: 10.15898/j.cnki.11-2131/td.201905290074

有机化学物质碳氮稳定同位素系列标准物质研制

自然资源部地下水科学与工程重点实验室, 中国地质科学院水文地质环境地质研究所, 河北 正定 050803

收稿日期: 2019-05-29  修回日期: 2019-12-16  接受日期: 2020-06-03

基金项目: 中国地质科学院基本科研业务费项目(SK201908)

作者简介: 李科, 硕士, 工程师, 水质分析专业。E-mail:77906583@qq.com

通信作者: 张琳, 硕士, 研究员, 从事地下水同位素分析研究。E-mail:zhl5369@163.com

Preparation of Reference Materials for Carbon and Nitrogen Isotopes of Organic Materials

Key Laboratory of Groundwater Sciences and Engineering, Ministry of Natural Resources; Institute of Hydrogeology and Environmental Geology, Chinese Academy of Geological Science, Zhengding 050803, China

Corresponding author: ZHANG Lin, zhl5369@163.com

Received Date: 2019-05-29
Revised Date: 2019-12-16
Accepted Date: 2020-06-03

摘要:实验室和研究人员所使用的碳、氮同位素标准物质一般由国际原子能机构(IAEA)获得,然而近年来,随着碳氮同位素在实验室质量监控、方法评价、仪器校准等方面的广泛应用,市场需求量不断增加,IAEA研制的碳、氮同位素标准物质的种类与数量逐渐不能满足科学研究快速发展的需求。我国急需研制适应当今分析技术水平的有机质碳氮同位素国家标准物质用以进行质量监控、方法评价、仪器校准。为保证量值传递精度,本文研制了4个有机化学物质的碳氮稳定同位素标准物质,其中3个为尿素样品,1个为L-谷氨酸。经检验4种标准物质的均匀性通过F值检验,标准物质的δ13C和δ15N值经过一年的稳定性检验,特征量值变化在测量方法允许的不确定度范围内,由此判定δ13C和δ15N值稳定性良好。由包括研制单位实验室在内的12家实验室协同定值,采用高温燃烧-气体同位素质谱法测定了δ13C和δ15N值,系列标准物质δ13C和δ15N认定值区间呈梯度分布,δ13C值为-40‰~0‰,δ15N值为-10‰~30‰,涵盖了我国天然样品中有机质碳氮稳定同位素组成范围;研制的系列标准物质δ13C的定值扩展不确定度不大于0.08‰,δ15N的定值扩展不确定度不大于0.09‰,定值水平与国际标准物质相当。该系列标准物质已被国家质检总局批准为国家一级标准物质,批准号为GBW04494~GBW04497。可被用于地质、生态、环境等多种样品δ13C和δ15N比值测定时的分析监控、仪器校准、方法评价、质量保证和质量监控。

关键词: 尿素, L-谷氨酸, 标准物质, 碳氮稳定同位素, 特征量值, 定值, 不确定度

要点

(1) 研制完成一组梯度范围大的有机质碳氮同位素国家一级标准物质GBW04494 ~ GBW04497。

(2)联合国内外12家实验室使用同位素质谱仪,采用国际标准物质作为溯源标准联合定值。

(3)扩展不确定度分别由测量不确定度、不均匀性不确定度、不稳定性不确定度合成计算得到。

Preparation of Reference Materials for Carbon and Nitrogen Isotopes of Organic Materials

ABSTRACT

OBJECTIVES:

To prepare carbon and nitrogen isotope reference materials for organic matter.

METHODS:

In order to ensure the accuracy of the transmission of the value, 4 stable carbon and nitrogen isotope reference materials of organic chemical materials were developed, of which 3 were urea samples and 1 was L-glutamic acid.

RESULTS:

According to the homogeneity test results, no statistically significant heterogeneity was found based on F test. The verified results by variance analysis for four samples showed very good homogeneity for the series. Nearly one-year stability analysis of δ13C and δ15N values confirmed that no statistically significant instability was found. The certified values of the reference materials were determined by an interlaboratory comparison of 12 participating laboratories. Carbon and nitrogen stable isotope ratios were measured using an elemental analyzer coupled with an isotope ratio mass spectrometer. The δ13C and δ15N values of the series of reference materials had a gradient distribution. The δ13C values ranged from -40‰ to 0‰, and the δ15N value from -10‰ to 30‰, covering the range of organic carbon and nitrogen stable isotope composition in natural samples in China. The extended uncertainty of the series of standard materials was not greater than 0.08‰ for δ13C and not greater than 0.09‰ for δ15N, and the fixed value level was equivalent to that of the international standard materials. This series of reference materials had been approved by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China as the national first-level reference materials (GBW04494-GBW04497).

Conclusion:

The series of reference materials can be used for analysis and monitoring, instrument calibration, method evaluation, quality assurance and quality monitoring in the determination of δ13C and δ15N ratios of various samples in geology, ecology and environment.

KEY WORDS: urea, L-glutamic acid, reference materials, carbon and nitrogen stable isotopes, characteristic values, certified values, uncertainty

HIGHLIGHTS

(1) A series of national first-level standard materials from GB W04494 to GB W04497 were prepared for carbon and nitrogen 1sotope analysis in organic materials.

(2) The certified values of reference materials were determined by 12 participating laboratories, using isotope ratio mass spectrometry and national reference material as the traceability standard.

(3) Expanded uncertainties were a combination of uncertainties in analysis,inhomogeneity and instability.

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有机化学物质碳氮稳定同位素系列标准物质研制

李科, 张琳, 刘福亮, 贾艳琨