Reference Material Preparation of 143Nd/144Nd Isotope Ratio
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摘要: 钕同位素比值(143Nd/144Nd)是Sm-Nd同位素方法的关键量值,由于被测样品的143Nd/144Nd比值变化范围很小,所以对143Nd/144Nd比值测试的精准度要求很高(精度优于0.005%)。为了获得高精度和高准确度的测试数据,分析过程中所用Nd同位素标准物质起着重要作用。以往的Nd同位素标准物质都是氧化钕,经过近三十年有的已消耗殆尽。本文阐述了钕同位素比值143Nd/144Nd标准溶液的研制,经检验标准溶液的均匀性和稳定性良好,由11家实验室协同定值,采用MC-TIMS和MC-ICP-MS方法测定143Nd/144Nd,确定了Nd同位素标准溶液的特性值143Nd/144Nd=0.512438,不确定度为5×10-6。此标准溶液于2015年5月获得国家标准样品证书(批号为GSB 04-3258—2015),可被用于地质、资源、海洋、环境、考古等多种样品143Nd/144Nd比值测定时的仪器校准和分析过程的质量监控。
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关键词:
- 标准溶液 /
- 钕同位素比值143Nd/144Nd /
- 特性值 /
- 多接收热电离质谱法 /
- 多接收电感耦合等离子体质谱法
Abstract: 143Nd/144Nd isotope ratio is the key for Sm-Nd isotope method. The 143Nd/144Nd isotope ratio of geological samples varies within a small range, and thus the 143Nd/144Nd isotope ratio analysis must be precise. In order to obtain high precision and high accuracy of the analytical data, the analysis process involving Nd isotope reference material plays an important role. The previous Nd isotope reference material is neodymium oxide, which have been exhausted in recent three decades. A national reference material of 143Nd/144Nd isotope ratio was introduced in this paper, which shows sufficient homogeneity and stability. The certified value of this reference material was determined by eleven participating laboratories using MC-TIMS and MC-ICP-MS. The 143Nd/144Nd isotope ratio value for the reference material is 0.512438, with a combined expanded uncertainty (k=2) of 5×10-6. The standard solution gets certification in May, 2015 and the Serial number is GSB 04-3258—2015. The standard solution can be used for quality monitoring of the equipment calibration and analysis process during the 143Nd/144Nd ratio determination for geology, resources, ocean, environment, archaeological and other type samples. -
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表 1 均匀性检验方差分析结果
Table 1. Variance analysis for homogeneity inspection of reference sample
项目 方差
SS自由度
df均方
MS统计量
F临界值
Fα(ν1, ν2)不确定度
ubb标准偏差
Sr2组间 3.2×10-10 14 2. 3×10-11 0.67 2.04 1.7×10-6 5.8×10-6 组内 1.1×10-9 30 3.4 ×10-11 表 2 标准溶液143Nd/144Nd定值实验室及定值使用方法
Table 2. Summary of participating laboratories, methods and equipment used for measurements of the 143Nd/144Nd ratio
实验室编号 实验室名称 定值方法 仪器型号 (生产国) Lab 1 中国地质科学院地质研究所同位素实验室 MC-ICP-MS Nu Plasam HR
(英国Nu Instuements公司)Lab 2 中国科学院广州地球化学研究所同位素地球化学国家重点实验室 MC-ICP-MS ISOPROBE
(英国GV公司)Lab 3 国土资源部武汉地质矿产研究所同位素地球化学实验室 TIMS MAT 261
(德国Finnigan公司)Lab 4 国土资源部天津地质矿产研究所实验测试室 TIMS TRITON
(美国Thermo公司)Lab 5 南京大学地球科学系同位素地球化学实验室 MC-ICP-MS NEPTUNE-plus
(美国Thermo公司)Lab 6 中国科学院地质与地球物理研究所固体同位素实验室 TIMS MAT 262
(德国Finnigan公司)Lab 7 中国科学院地质与地球物理研究所多接收器电感耦合等离子体质谱实验室 MC-ICP-MS NEPTUNE
(美国Thermo公司)Lab 8 中国科学院地质与地球物理研究所固体同位素实验室 TIMS ISOPROBE-T
(英国GV公司)Lab 9 国家海洋局第一海洋研究所海洋环境测试中心 MC-ICP-MS Nu Plasam HR
(英国Nu Instuements公司)Lab 10 中国地质科学院矿产资源研究所同位素实验室 MC-ICP-MS NEPTUNE
(美国Thermo公司)Lab 11 核工业北京地质研究院核工业地质分析测试中心 TIMS ISOPROBE-T
(英国GV公司)表 3 标准溶液143Nd/144Nd定值分析结果
Table 3. The analytical data of 143Nd/144Nd for reference samples
实验室
编号143Nd/144Nd测量值 S-1 S-2 S-3 S-4 S-5 S-6 平均值 Lab 1 0.512431 0.512433 0.512441 0.512450 0.512446 0.512447 0.512441 Lab 2 0.512433 0.512430 0.512435 0.512432 0.512426 0.513434 0.512432 Lab 3 0.512438 0.512448 0.512432 0.512435 0.512443 0.512439 0.512439 Lab 4 0.512440 0.512450 0.512439 0.512437 0.512448 0.512437 0.512442 Lab 5 0.512445 0.512440 0.512446 0.512440 0.512448 0.512432 0.512442 Lab 6 0.512440 0.512448 0.512421 0.512452 0.512427 0.512432 0.512437 Lab 7 0.512429 0.512439 0.512435 0.512437 0.512430 0.512437 0.512434 Lab 8 0.512431 0.512441 0.512433 0.512448 0.512452 0.512437 0.512440 Lab 9 0.512434 0.512440 0.512454 0.512445 0.512431 0.512428 0.512439 Lab 10 0.512450 0.512432 0.512435 0.512435 0.512443 0.512450 0.512441 Lab 11 0.512413 0.512416 0.512434 0.512435 0.512438 0.512424 0.512427 表 4 常用Nd同位素比值分析标准物质分析结果
Table 4. Measurement results of certified reference materials
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