Inter-Laboratory Comparison of Measuring Organic Carbon and Stable Nitrogen Isotopes in Marine Sediments by Elemental Analysis-Isotope Ratio Mass Spectrometry
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摘要: 海洋沉积物中有机碳、氮稳定同位素（δ13C、δ15N）作为一种有效指标，可对不同地质时期空气、温度、降水等参数的变化进行标记。元素分析-同位素比值质谱法是一种测量海洋沉积物有机碳、氮稳定同位素组成的合理、有效的方法。目前我国有诸多实验室使用元素分析仪（EA）与稳定同位素比值质谱仪（IRMS）联用的方法对沉积物中的有机碳、氮稳定同位素进行测试。各实验室之间测试技术及数据稳定性缺少比对依据，测试结果缺乏有效的溯源，使用过程中缺乏规范和统一。本文选取了我国2018年研制的三个国家一级海洋沉积物碳氮稳定同位素标准物质（GBW04701、GBW04702、GBW04703）及两个国际标准物质（EMA-B2152、EMA-B2151），在我国十家实验室对EA-IRMS在线技术测试方法进行实验室间的测量比对实验，以验证方法的稳定性、精密度和准确度。测试结果表明：各家协作实验室的数据准确、稳定，方法的重复性和再现性良好，测得的δ13C和δ15N精密度分别好于0.10‰、0.14‰。通过比对研究，同时证明了EA-IRMS在线技术适用于海洋沉积物中的有机碳、氮稳定同位素的测定，初步建立了一套适合海洋沉积物样品分析的方法。
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关键词:
- 元素分析-同位素比值质谱法 /
- 海洋沉积物 /
- 有机碳稳定同位素 /
- 氮稳定同位素 /
- 比对研究
Abstract:BACKGROUNDOrganic carbon and nitrogen stable isotopes (δ13C, δ15N) in marine sediments are used as effective indicators to trace the changes of air, temperature, precipitation and other parameters in different geological time. Elemental analysis-isotope ratio mass spectrometry is a reasonable and effective method to measure the composition of organic carbon and nitrogen stable isotopes in marine sediments. At present, many domestic laboratories use the method of element analyzer (EA) and stable isotope ratio mass spectrometer (IRMS) to analyze the stable isotopes of organic carbon and nitrogen. However, the comparison of analytical method and data stability between different laboratories is lacking. The analytical results lack effective traceability, and the process lacks standardization and unification. OBJECTIVESTo develop a method for determining organic carbon and nitrogen stable isotopes in marine sediments. METHODSThree newly developed national first-class standard materials (GBW04701, GBW04702, GBW04703) and two international standard materials (EMA-B2152, EMA-B2151) were sent to 10 domestic laboratories, in order to verify the stability, precision and accuracy of EA-IRMS online technology test method through the comparative measurement between laboratories. RESULTSThe data of each collaborative laboratory was accurate and stable, and the method had good repeatability and reproducibility. The results showed that precisions of 13C and 15N were better than 0.10‰ and 0.14‰, respectively. CONCLUSIONSThrough comparative study, it has been proved that EA-IRMS online technology is suitable for the determination of organic carbon and nitrogen stable isotopes in marine sediments. A suitable method for the determination of marine sediment samples has been preliminarily established. -
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表 1 协作实验样品类型和δ13C和δ15N值的范围
Table 1. Sample type of the collaboration experiment and the range of δ13C and δ15N values
样品编号 样品类型 标准物质编号 δ13C (‰) δ15N (‰) 水平1 沉积物 GBW04701 -20.9~-20.7 3.7~4.0 水平2 沉积物 GBW04702 -23.8~-23.6 6.3~6.7 水平3 沉积物 GBW04703 -22.8~-22.4 4.5~5.0 水平4 土壤 EMA-B2152 -27.4~-27.2 7.0~7.3 水平5 沉积物 EMA-B2151 -26.4~-26.2 4.1~4.5 
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表 2 协作试验δ13C和δ15N测定准确度数据
Table 2. Accuracy data of δ13C and δ15N in the cooperative experiment
实验室编号 GBW04701 GBW04702 GBW04703 EMA-B2152 EMA-B2151 δ13C (‰) δ15N (‰) δ13C (‰) δ15N (‰) δ13C (‰) δ15N (‰) δ13C (‰) δ15N (‰) δ13C (‰) δ15N (‰) A 0.16 0.07 -0.10 0.07 -0.02 0.22 0.05 0.03 0.01 0.12 0.15 0.12 -0.03 0.11 -0.02 0.15 0.03 -0.02 0.01 0.13 0.21 0.12 -0.03 0.00 0.01 0.28 0.08 - 0.03 0.18 0.19 0.16 -0.07 0.17 -0.03 0.16 0.04 - 0.05 0.18 0.15 0.09 -0.05 0.15 -0.05 0.12 0.06 0.28 0.04 0.10 0.18 -0.01 -0.06 0.01 -0.04 0.29 0.04 0.14 0.05 0.12 标准偏差(‰) 0.02 0.05 0.02 0.06 0.02 0.06 0.02 0.12 0.02 0.03 B 0.15 0.06 -0.08 0.09 -0.23 -0.02 0.02 0.05 -0.08 0.04 0.10 -0.04 0.00 0.07 -0.32 0.01 0.12 0.11 -0.06 0.09 0.09 -0.06 0.05 0.06 -0.15 0.09 0.08 0.15 -0.07 -0.08 0.12 0.10 -0.19 -0.04 -0.14 0.03 0.11 0.14 -0.09 -0.08 - 0.06 - 0.06 - -0.15 - - - - - 0.06 - -0.03 - 0.01 - - - - 标准偏差(‰) 0.02 0.06 0.09 0.05 0.07 0.07 0.04 0.04 0.01 0.07 C 0.37 -0.09 0.01 -0.03 0.21 0.19 -0.01 0.08 0.01 0.03 0.28 -0.10 0.12 -0.11 0.13 0.11 -0.18 0.09 -0.04 0.06 0.26 -0.03 0.12 0.20 0.18 0.21 -0.13 0.14 0.03 0.12 0.34 0.10 -0.08 0.12 0.18 0.21 -0.07 0.03 0.02 0.17 0.36 -0.13 0.14 0.04 0.10 0.27 - - - - 0.32 -0.15 0.12 0.17 0.20 0.22 - - - - 标准偏差(‰) 0.04 0.08 0.08 0.11 0.04 0.05 0.06 0.04 0.03 0.05 D 0.20 0.06 -0.07 -0.19 -0.07 -0.03 -0.10 -0.01 -0.14 - 0.13 0.15 -0.10 -0.22 0.04 -0.09 -0.15 0.19 -0.11 -0.01 0.19 0.12 -0.20 -0.09 -0.02 -0.08 -0.09 -0.02 -0.05 -0.17 0.21 -0.04 -0.26 -0.01 -0.19 -0.11 -0.22 -0.03 -0.08 - 0.19 - -0.19 -0.03 -0.11 -0.07 -0.10 0.06 - - 0.20 - -0.04 -0.13 -0.17 -0.09 -0.15 0.21 - - 标准偏差(‰) 0.03 0.07 0.08 0.08 0.08 0.02 0.05 0.10 0.03 0.08 E 0.24 -0.01 0.09 -0.15 0.03 0.01 -0.04 - -0.01 0.06 0.10 0.04 0.02 0.06 0.09 0.27 0.03 - 0.05 0.10 0.20 0.01 -0.04 -0.02 0.08 0.17 -0.11 - 0.11 0.07 0.22 0.17 -0.08 -0.15 0.04 -0.04 0.10 0.13 0.04 0.24 0.15 0.05 0.05 -0.05 0.05 0.04 0.01 0.14 - - 0.08 0.11 0.07 -0.12 0.06 0.28 -0.03 - - - 标准偏差(‰) 0.06 0.06 0.06 0.08 0.02 0.13 0.06 0.00 0.04 0.07 F 0.12 -0.17 -0.03 -0.12 -0.12 -0.35 0.07 0.12 -0.08 0.09 0.13 -0.11 -0.09 -0.13 -0.11 -0.26 0.12 0.11 -0.07 0.15 0.06 -0.04 -0.11 -0.12 -0.26 -0.28 0.10 0.23 -0.12 -0.02 0.06 -0.25 -0.05 -0.03 -0.28 -0.31 0.08 0.09 -0.09 0.10 0.10 -0.11 -0.16 0.00 -0.22 - 0.05 0.11 - - -0.03 -0.11 -0.18 -0.24 -0.15 - - - - - 标准偏差(‰) 0.05 0.06 0.05 0.08 0.07 0.03 0.02 0.05 0.02 0.06 G 0.33 0.26 0.06 -0.03 -0.01 0.10 -0.28 0.15 0.02 -0.03 0.30 0.13 -0.04 -0.02 0.13 0.11 -0.10 0.01 0.14 0.05 0.27 0.14 0.02 -0.02 0.06 0.10 -0.14 -0.02 0.06 0.07 0.12 0.22 0.16 -0.04 -0.04 0.14 -0.03 -0.05 0.04 0.26 0.27 0.23 0.10 0.03 0.01 0.05 -0.05 -0.17 - - - - - - - -0.08 - - - - 标准偏差(‰) 0.07 0.05 0.07 0.02 0.06 0.07 0.09 0.10 0.05 0.11 H 0.21 0.00 -0.03 -0.23 0.07 -0.32 0.00 -0.19 -0.07 -0.07 0.27 -0.07 0.05 -0.27 0.04 -0.07 0.09 -0.07 -0.11 0.03 0.19 -0.12 0.04 -0.25 0.06 -0.11 0.09 -0.09 -0.05 -0.05 0.22 -0.01 0.07 -0.08 0.06 -0.22 0.11 -0.05 0.03 0.02 0.24 -0.07 0.06 -0.16 0.05 -0.31 0.15 -0.11 -0.01 -0.04 0.31 -0.20 - - - - - - - - 标准偏差(‰) 0.04 0.07 0.04 0.07 0.01 0.10 0.05 0.05 0.05 0.04 I 0.04 -0.14 0.11 0.18 0.12 0.18 0.12 -0.10 -0.11 0.14 0.09 -0.05 0.15 0.22 0.03 0.02 0.13 -0.11 -0.10 0.08 0.07 -0.06 0.05 0.14 0.22 0.18 0.25 -0.20 -0.05 0.13 0.09 -0.11 -0.07 0.14 0.18 0.08 -0.03 -0.25 -0.13 0.14 0.14 -0.10 0.04 - 0.16 0.25 0.11 -0.08 -0.09 0.28 0.16 -0.17 0.09 - 0.09 0.06 0.13 0.05 - - 标准偏差(‰) 0.04 0.04 0.07 0.03 0.06 0.08 0.08 0.09 0.03 0.07 J 0.19 - -0.06 - -0.06 - 0.05 - - - 0.09 - -0.19 - -0.25 - 0.09 - - - 0.11 - -0.10 - -0.16 - 0.00 - - - 0.09 - -0.16 - -0.03 - -0.14 - - - 0.09 - -0.06 - -0.13 - 0.06 - - - 标准偏差(‰) 0.04 - 0.05 - 0.08 - 0.08 - - - 注：“-”表示未得到测试结果，不参与统计计算。
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表 3 δ13C和δ15N测定的重复性与再现性统计结果
Table 3. Statistical results of repeatability and reliability of δ13C and δ15N
参数 统计参数 GBW04701 GBW04702 GBW04703 EMA-B2152 EMA-B2151 δ13C(‰) 有效实验室数目(p) 10 10 10 10 9 总平均值(m) -20.79 -23.65 -22.58 -27.29 -26.33 重复性标准差(Sr) 0.049 0.070 0.062 0.067 0.037 再现性标准差(SR) 0.091 0.104 0.141 0.112 0.072 重复性限(r) 0.139 0.199 0.175 0.190 0.104 再现性限(R) 0.258 0.295 0.399 0.317 0.205 r/R与m的关系 重复性限r与测试值m的关系：r=0.0066m；再现性限r与测试值m的关系：R=0.012m δ15N(‰) 有效实验室数目(p) 9 9 9 9 9 总平均值(m) 3.80 6.46 4.81 7.18 4.37 重复性标准差(Sr) 0.069 0.078 0.084 0.089 0.075 再现性标准差(SR) 0.125 0.131 0.184 0.128 0.100 重复性限(r) 0.195 0.221 0.237 0.253 0.213 再现性限(R) 0.352 0.371 0.520 0.363 0.284 r/R与m的关系 重复性限r与测试值m的关系：r=0.0694m；再现性限r与测试值m的关系：R=0.1068m
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表 4 δ13C和δ15N测量方法偏倚的估计
Table 4. Estimation of measurement method bias of δ13C and δ15N
统计参数 δ13C (‰) δ15N (‰) GBW04701 GBW04702 GBW04703 EMA-B2152 EMA-B2151 GBW04701 GBW04702 GBW04703 EMA-B2152 EMA-B2151 γ(SR/Sr) 1.861 1.481 2.277 1.672 1.975 1.807 1.677 2.191 1.435 1.334 A 0.635 0.643 0.630 0.638 0.633 0.635 0.638 0.630 0.644 0.648 A×SR 0.058 0.067 0.089 0.072 0.046 0.079 0.084 0.116 0.083 0.065 总平均值(m) -20.79 -23.65 -22.58 -27.29 -26.33 3.80 6.46 4.81 7.18 4.37 标准值(μ) -20.79 -23.63 -22.57 -27.29 -26.27 3.80 6.48 4.78 7.18 4.42 测量方法偏倚(δ) -0.004 -0.022 -0.013 -0.002 -0.057 0.002 -0.020 0.032 0.001 -0.046 δ-A×SR -0.062 -0.089 -0.101 -0.073 -0.103 -0.078 -0.104 -0.084 -0.082 -0.111 δ+A×SR 0.054 0.045 0.076 0.070 -0.011 0.081 0.063 0.148 0.084 0.019 注：A为标准物质认定值的估计值不确定度的系数；A×SR为测量方法的偏倚的95%的置信区间；GBW04701、GBW04702、GBW04703的标准值(μ)为该标准物质的认定值，EMA-B2152的标准值(μ)为各比对实验室测量获得的平均值。
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