激光同位素光谱法测量水中氢氧同位素组成的实验室间比对研究

蓝高勇; 吴夏; 杨会; 唐伟; 应启和; 王华

doi:10.15898/j.cnki.11-2131/td.201704060049

激光同位素光谱法测量水中氢氧同位素组成的实验室间比对研究

国土资源部广西岩溶动力学重点实验室, 中国地质科学院岩溶地质研究所, 广西桂林 541004

基金项目:
国土资源部公益性行业专项（21411075-03）；国家自然科学基金资助项目（41501222）；广西青年科学基金项目（2014GXNSFBA118227）；中国地质科学院岩溶地质研究所基本科研业务费项目（2016003）

详细信息

作者简介: 蓝高勇, 助理研究员, 从事同位素分析测试研究。E-mail:langaoyong@karst.ac.cn

通讯作者: 王华, 高级工程师, 从事同位素分析测试研究。E-mail:wanghua1@163.com

中图分类号: O657.38;O613.2;O613.3

收稿日期: 2017-04-06

修回日期: 2017-07-11

录用日期: 2017-07-20

Inter-Laboratory Comparison of Analysis for Hydrogen and Oxygen Stable Isotope Ratios in Water Samples by Laser Absorption Spectroscopy

Key Laboratory of Karst Dynamics, Ministry of Land and Resources & Guangxi, Institute of Karst Geology, Chinese Academy of Geological Sciences, Guilin 541004, China

More Information

Corresponding author: Hua WANG, wanghua1@163.com

Received Date: 06 April 2017

Revised Date: 11 July 2017

Accepted Date: 20 July 2017

摘要

摘要: 激光同位素光谱分析方法是近些年使用较广泛的一种便捷、快速的测试稳定同位素组成的技术，能同时分析出水中δD、δ¹⁸O同位素组成，因其操作简单，检测效率高，体积小，野外现场测试携带方便，迅速在环境、地质、生态和能源等领域得到广泛应用，但是该测试分析方法尚没有相应的国家标准，测试结果得不到有效的溯源，在使用过程中缺乏规范和统一。为此，本文通过在全国范围内12家实验室选取8个比对水样（δD值在-189.1‰~-0.4‰内，δ¹⁸O值在-24.52‰~0.32‰内），利用激光同位素光谱法测试比对D/H和¹⁸O/¹⁶O值，探讨激光同位素光谱仪分析水中δD、δ¹⁸O值的准确度和精密度。测试结果表明：各个协作实验室数据准确、稳定，方法的重复性和再现性良好；激光光谱法测定的δD精密度为0.4‰（1σ），δ¹⁸O精密度为0.05‰（1σ），与传统稳定同位素质谱的精度几乎一致，因此适用于常规水样中δD、δ¹⁸O测定，可以开展野外在线实时检测水中氢氧同位素组成。本研究为开展制定激光同位素光谱法测定环境液态水中δD、δ¹⁸O同位素组成标准方法的工作推广和应用提供了参考。
- 激光同位素光谱法 /
- 氢同位素 /
- 氧同位素 /
- 实验室比对 /
- 环境水样
Abstract: Laser Absorption Spectroscopy technology is a convenient and rapid method for the simultaneous determination of hydrogen and oxygen isotope ratios in environmental water samples. This method has been widely used in the environment, geology, ecology, and energy fields due to its simplicity, high detection efficiency, and portability. However, no national standards are available for this method and thus the analytical results are not traceable effectively. Moreover, the use of this method lacks norms and unity. In order to evaluate the accuracy and precision of the Laser Absorption Spectroscopy method for the determination of δD, δ¹⁸O, D/H and ¹⁸O/¹⁶O values of eight water samples (δD value of within -189.1‰-0.4‰, δ¹⁸O value of within -24.52‰-0.32‰), values were determined by 12 laboratories using optical cavity enhanced absorption spectroscopy. Data from each collaboration laboratory is accurate, stable, and reproducible. The precision value of δD is 0.4‰ (1σ) and δ¹⁸O is 0.05‰ (1σ), comparable to the traditional mass spectrometry method. Therefore, the method is suitable for the on-line and real-time determination of hydrogen and oxygen isotope ratio in the field. This study provides a reference for the development and application of the standard method for determination of δD and δ¹⁸O isotopes in environmental water.
- Laser Absorption Spectroscopy /
- hydrogen isotope /
- oxygen isotope /
- inter-laboratory comparison /
- environmental water sample

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图 1 A~L实验室δD和δ¹⁸O值测试准确度

Figure 1.

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图 2 A~L实验室比对δD和δ¹⁸O曼德尔h-k统计图

Figure 2.

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表 1 测试样品的δD和δ¹⁸O参考值

Table 1. The reference hydrogen and oxygen isotope ratios of water sample

样品编号	名称	水样类型	δD_V-SMOW(‰)	δ¹⁸O_V-SMOW(‰)	备注
水平1	GBW04401	人工配置	-0.4±1.0	0.32±0.19	国家一级标准
水平2	YHS	人工配置	-12.0±1.0	-1.50±0.20	-
水平3	L4A	人工配置	-50.5±0.5	-7.69±0.10	-
水平4	GBW04402	地表水	-64.8±1.1	-8.79±0.14	国家一级标准
水平5	YYNS	地下水	-72.6±1.0	-10.23±0.10	-
水平6	L3A	人工配置	-96.4±0.5	-13.10±0.10	-
水平7	YXZS	天然水	-134.7±0.5	-17.68±0.10	-
水平8	GBW04403	人工配置	-189.1±1.1	-24.52±0.20	国家一级标准

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表 2 激光同位素光谱法协作实验测量的δD和δ¹⁸O精密度统计

Table 2. The precision statistics of δD and δ¹⁸O obtained from inter-laboratory by Laser Absorption Spectroscopy

统计参数	GBW04401	YHS	L4A	GBW04402	YYN	L3A	YXZS	GBW04403
δD、δ¹⁸O实验室数(p)	12	12	12	12	12	12	12	12
δD参考值(‰)	-0.4	-11.9	-50.5	-64.8	-72.6	-96.4	-134.7	-189.1
δD总平均值±1σ(‰)	-0.4±0.17	-11.2±0.26	-50.4±0.40	-64.9±0.32	-72.6±0.32	-96.2±0.40	-134.3±0.26	-189.1±0.10
δD实验室偏倚δ	0.030	0.746	0.638	-0.016	-0.066	0.230	0.373	0.033
δD偏倚区间[δ-AS_R, δ+AS_R]	-0.07~0.13	0.59~0.90	0.40~0.87	-0.20~0.17	-0.25~0.12	-0.01~0.47	0.22~0.53	-0.03~0.09
δ¹⁸O参考值(‰)	0.32	-1.50	-7.69	-8.79	-10.20	-13.10	-17.66	-24.52
δ¹⁸O总平均值±1σ(‰)	0.33±0.02	-1.47±0.03	-7.74±0.03	-8.78±0.05	-10.13±0.03	-13.15±0.05	-17.62±0.04	-24.52±0.01
δ¹⁸O方法偏倚δ	0.007	0.132	-0.051	0.010	0.069	-0.051	0.038	0.001
δ¹⁸O偏倚区间[δ-AS_R, δ+AS_R]	-0.01~0.02	0.11~0.15	-0.07~-0.03	-0.02~0.04	0.05~0.09	-0.08~-0.02	0.01~0.06	-0.01~0.01
注：表中重复性限r、再现性限R和测量方法偏倚AS_R基于95%的置信区间，n=60。

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表 3 不同实验室δD和δ¹⁸O的测试结果

Table 3. The measurement results of δD and δ¹⁸O obtained from different laboratories

样品编号	A		B		C		D		E		F		G		H		I		J		K		L
样品编号	δD	δ¹⁸O	δD	δ¹⁸O	δD	δ¹⁸O	δD	δ¹⁸O	δD	δ¹⁸O	δD	δ¹⁸O	δD	δ¹⁸O	δD	δ¹⁸O	δD	δ¹⁸O	δD	δ¹⁸O	δD	δ¹⁸O	δD	δ¹⁸O
GBW 04401	-0.2	0.32	-0.4	0.31	-0.3	0.32	-0.2	0.33	-0.3	0.31	-0.3	0.31	-0.4	0.32	-0.4	0.32	-0.4	0.28	-0.7	0.28	-0.8	0.29	-0.4	0.32
	-0.2	0.34	-0.4	0.33	-0.2	0.32	-0.3	0.33	-0.2	0.34	-0.2	0.31	-0.4	0.34	-0.4	0.37	-0.4	0.29	-0.7	0.30	-0.8	0.29	-0.4	0.32
	-0.1	0.36	-0.3	0.35	-0.2	0.33	-0.3	0.34	-0.3	0.33	-0.2	0.32	-0.3	0.34	-0.4	0.38	-0.3	0.30	-0.7	0.30	-0.8	0.30	-0.4	0.32
	-0.2	0.37	-0.3	0.36	-0.2	0.33	-0.3	0.35	-0.2	0.33	-0.2	0.32	-0.3	0.34	-0.4	0.36	-0.4	0.30	-0.7	0.31	-0.7	0.30	-0.4	0.32
	-0.3	0.39	-0.3	0.37	-0.3	0.34	-0.2	0.35	-0.2	0.32	-0.2	0.34	-0.3	0.36	-0.4	0.33	-0.4	0.32	-0.6	0.31	-0.7	0.30	-0.4	0.32
YHS	-11.0	-1.49	-11.1	-1.47	-11.5	-1.48	-11.5	-1.55	-11.3	-1.47	-11.1	-1.51	-11.6	-1.50	-11.5	-1.52	-11.5	-1.44	-11.3	-1.51	-10.8	-1.42	-11.2	-1.44
	-11.0	-1.49	-11.1	-1.48	-11.3	-1.47	-11.4	-1.54	-11.3	-1.46	-11.0	-1.49	-11.6	-1.49	-11.4	-1.50	-11.8	-1.44	-11.2	-1.51	-10.7	-1.42	-11.0	-1.46
	-10.9	-1.48	-11.0	-1.51	-11.4	-1.46	-11.3	-1.50	-11.3	-1.48	-11.0	-1.47	-11.3	-1.47	-11.4	-1.50	-11.6	-1.44	-11.1	-1.50	-10.6	-1.41	-11.0	-1.44
	-10.9	-1.47	-10.9	-1.47	-11.2	-1.46	-11.2	-1.49	-11.4	-1.46	-11.0	-1.47	-11.2	-1.45	-11.3	-1.49	-11.4	-1.42	-11.1	-1.48	-10.6	-1.41	-10.9	-1.44
	-10.7	-1.46	-10.9	-1.46	-11.2	-1.44	-11.2	-1.49	-11.4	-1.44	-10.9	-1.43	-11.2	-1.43	-11.1	-1.48	-11.3	-1.40	-11.0	-1.48	-10.6	-1.40	-11.1	-1.47
L4A	-50.7	-7.72	-50.6	-7.76	-50.7	-7.78	-50.6	-7.80	-50.8	-7.77	-50.5	-7.77	-50.6	-7.79	-50.6	-7.77	-50.8	-7.75	-49.8	-7.72	-49.7	-7.71	-50.4	-7.75
	-50.9	-7.80	-50.5	-7.74	-50.7	-7.78	-50.4	-7.78	-50.8	-7.75	-50.5	-7.76	-50.4	-7.76	-50.4	-7.76	-50.6	-7.70	-49.7	-7.71	-49.7	-7.69	-50.1	-7.75
	-50.7	-7.72	-50.5	-7.76	-50.6	-7.77	-50.4	-7.72	-50.8	-7.78	-50.5	-7.74	-50.3	-7.76	-50.3	-7.76	-50.7	-7.68	-49.6	-7.71	-49.6	-7.69	-50.0	-7.73
	-50.6	-7.70	-50.4	-7.74	-50.7	-7.75	-50.8	-7.72	-50.8	-7.78	-50.5	-7.73	-50.2	-7.75	-50.3	-7.75	-50.5	-7.76	-49.6	-7.68	-49.5	-7.68	-50.0	-7.70
	-50.5	-7.78	-50.3	-7.79	-50.8	-7.75	-50.7	-7.70	-50.7	-7.75	-50.3	-7.73	-50.1	-7.74	-50.6	-7.74	-50.5	-7.74	-49.5	-7.68	-49.5	-7.68	-50.0	-7.73
GBW 04402	-65.1	-8.79	-64.9	-8.80	-65.0	-8.82	-65.1	-8.84	-65.2	-8.77	-65.1	-8.84	-65.0	-8.88	-65.1	-8.77	-64.9	-8.70	-64.5	-8.77	-64.3	-8.76	-64.5	-8.77
	-65.1	-8.87	-64.9	-8.77	-65.0	-8.82	-65.0	-8.83	-65.0	-8.81	-65.1	-8.81	-64.9	-8.88	-65.1	-8.75	-64.8	-8.69	-64.4	-8.77	-64.3	-8.75	-64.3	-8.77
	-65.2	-8.81	-64.8	-8.77	-65.1	-8.81	-65.0	-8.83	-65.3	-8.82	-65.1	-8.80	-64.9	-8.84	-65.1	-8.74	-64.8	-8.69	-64.4	-8.76	-64.3	-8.74	-64.3	-8.77
	-65.2	-8.81	-64.8	-8.75	-65.0	-8.79	-65.0	-8.82	-65.0	-8.79	-65.0	-8.80	-64.9	-8.83	-64.9	-8.73	-64.8	-8.67	-64.4	-8.75	-64.2	-8.74	-64.2	-8.76
	-65.0	-8.79	-64.7	-8.74	-65.0	-8.78	-65.0	-8.81	-65.2	-8.82	-65.0	-8.77	-64.7	-8.81	-64.9	-8.73	-64.7	-8.66	-64.4	-8.73	-64.2	-8.74	-64.3	-8.77
YYN	-72.8	-10.18	-72.7	-10.17	-73.1	-10.15	-73.1	-10.11	-72.8	-10.13	-72.8	-10.16	-72.8	-10.21	-72.7	-10.16	-72.3	-10.10	-72.3	-10.13	-72.1	-10.09	-72.6	-10.13
	-72.9	-10.19	-72.7	-10.15	-72.9	-10.14	-73.1	-10.18	-73.0	-10.15	-72.8	-10.14	-72.6	-10.20	-72.6	-10.16	-72.5	-10.10	-72.2	-10.13	-72.0	-10.09	-72.3	-10.11
	-72.9	-10.14	-72.6	-10.14	-72.9	-10.14	-72.9	-10.14	-72.7	-10.14	-72.8	-10.13	-72.6	-10.19	-72.3	-10.12	-72.7	-10.10	-72.1	-10.12	-72.0	-10.08	-72.2	-10.11
	-72.8	-10.13	-72.4	-10.11	-72.8	-10.13	-72.9	-10.13	-72.9	-10.14	-72.8	-10.12	-72.4	-10.18	-72.5	-10.12	-72.6	-10.09	-72.1	-10.12	-72.0	-10.07	-72.3	-10.10
	-72.7	-10.13	-72.4	-10.10	-72.9	-10.13	-72.9	-10.12	-72.5	-10.13	-72.8	-10.11	-72.4	-10.18	-72.4	-10.12	-72.8	-10.07	-72.1	-10.11	-72.0	-10.06	-72.2	-10.12
L3A	-96.4	-13.25	-96.3	-13.20	-96.4	-13.18	-96.3	-13.21	-96.4	-13.17	-95.9	-13.15	-96.4	-13.13	-96.8	-13.08	-96.1	-13.07	-95.5	-13.12	-95.9	-13.17	-96.1	-13.21
	-96.3	-13.23	-96.3	-13.18	-96.4	-13.17	-96.1	-13.20	-96.8	-13.18	-95.9	-13.15	-96.4	-13.12	-96.7	-13.18	-96.3	-13.12	-95.4	-13.12	-95.8	-13.16	-95.9	-13.22
	-96.4	-13.19	-96.3	-13.18	-96.5	-13.15	-96.5	-13.18	-96.8	-13.13	-95.8	-13.12	-96.3	-13.11	-96.5	-13.12	-96.2	-13.21	-95.3	-13.10	-95.8	-13.13	-95.8	-13.21
	-96.4	-13.17	-96.2	-13.16	-96.7	-13.13	-96.4	-13.17	-96.7	-13.15	-95.8	-13.12	-96.2	-13.08	-96.5	-13.11	-96.2	-13.11	-95.3	-13.19	-95.7	-13.13	-95.7	-13.21
	-96.3	-13.14	-96.2	-13.15	-96.6	-13.11	-96.4	-13.16	-96.5	-13.11	-95.8	-13.11	-96.2	-13.06	-96.4	-13.10	-96.7	-13.20	-95.3	-13.15	-95.3	-13.02	-95.9	-13.21
YXZS	-134.5	-17.70	-134.6	-17.72	-134.5	-17.62	-134.7	-17.66	-134.4	-17.63	-134.6	-17.63	-134.5	-17.71	-134.0	-17.69	-134.3	-17.59	-134.5	-17.65	-134.4	-17.62	-134.2	-17.59
	-134.6	-17.65	-134.5	-17.70	-134.5	-17.60	-134.6	-17.65	-134.7	-17.68	-134.6	-17.62	-134.4	-17.68	-133.8	-17.65	-134.3	-17.57	-134.3	-17.64	-134.4	-17.60	-134.0	-17.59
	-134.5	-17.65	-134.5	-17.66	-134.7	-17.60	-134.5	-17.63	-134.2	-17.65	-134.6	-17.61	-134.3	-17.68	-133.8	-17.65	-134.4	-17.57	-134.3	-17.64	-134.4	-17.60	-133.9	-17.58
	-134.4	-17.62	-134.4	-17.60	-134.6	-17.58	-134.5	-17.59	-134.6	-17.65	-134.3	-17.61	-134.2	-17.65	-133.8	-17.62	-134.0	-17.56	-134.3	-17.63	-134.4	-17.60	-133.9	-17.57
	-134.4	-17.61	-134.4	-17.60	-134.6	-17.55	-134.1	-17.56	-134.5	-17.64	-134.3	-17.56	-134.1	-17.58	-133.7	-17.58	-133.9	-17.56	-134.3	-17.63	-134.3	-17.59	-133.9	-17.59
GBW 04403	-189.0	-24.52	-189.1	-24.52	-189.1	-24.52	-189.0	-24.51	-188.9	-24.52	-189.0	-24.53	-189.1	-24.52	-189.1	-24.50	-189.1	-24.55	-189.3	-24.54	-189.3	-24.55	-189.1	-24.52
	-189.0	-24.53	-189.1	-24.52	-189.0	-24.52	-189.0	-24.51	-189.0	-24.52	-189.0	-24.52	-189.1	-24.52	-189.0	-24.53	-189.1	-24.54	-189.3	-24.53	-189.3	-24.54	-189.0	-24.52
	-189.0	-24.51	-189.1	-24.52	-189.0	-24.52	-189.0	-24.51	-189.0	-24.51	-189.0	-24.51	-189.1	-24.51	-188.9	-24.52	-189.1	-24.54	-189.2	-24.53	-189.3	-24.54	-189.0	-24.52
	-189.0	-24.50	-189.1	-24.50	-189.0	-24.52	-189.0	-24.51	-189.0	-24.52	-189.0	-24.51	-189.0	-24.50	-188.9	-24.51	-189.1	-24.54	-189.2	-24.53	-189.3	-24.53	-189.0	-24.51
	-189.0	-24.50	-189.1	-24.50	-189.0	-24.51	-189.0	-24.50	-189.0	-24.52	-189.0	-24.51	-189.0	-24.50	-188.9	-24.50	-189.2	-24.53	-189.2	-24.53	-189.2	-24.53	-189.0	-24.51
注：测试结果单位均为‰，所报数据均为相对于国际标准V-SMOW的比值。

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参考文献(23)

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