改进的两柱Cd色谱分离流程和高精度的Cd同位素分析

钟桥辉; 彭冰钰; 何炽凤; 郭家凯; 初高彬; 尹露; 李杰

doi:10.3799/dqkx.2025.122

改进的两柱Cd色谱分离流程和高精度的Cd同位素分析

doi: 10.3799/dqkx.2025.122

钟桥辉^{1, 4, ,},
彭冰钰^{1, 4},
何炽凤^{1, 4},
郭家凯^{1, 4},
初高彬²,
尹露³,
李杰^1, ,

1.
中国科学院广州地球化学研究所, 深部地球过程与资源国家重点实验室, 广东广州 510640
2.
广州市拓岩检测技术有限公司, 广东广州 510640
3.
河北地质大学, 河北省战略性关键矿产资源重点实验室, 河北石家庄 050031
4.
中国科学院大学地球与行星科学学院, 北京 100101

基金项目:

国家重点研发计划项目 2023YFF0803704

广东省自然科学基金项目 2024A1515010037

详细信息

作者简介:
钟桥辉（1993-），男，博士研究生，研究方向为金属稳定同位素分析方法研发. ORCID： 0000-0003-3825-8405. E-mail：1102058215@qq.com

通讯作者:
李杰, E-mail: jieli@gig.ac.cn

中图分类号: P597.2
计量
- 文章访问数: 32
- HTML全文浏览量: 13
- PDF下载量: 0
- 被引次数: 0
出版历程
- 收稿日期: 2025-06-05
- 网络出版日期: 2025-07-29
- 刊出日期: 2025-07-25

Improved Two⁃Column Cd Chromatographic Separation Procedure and High⁃Precision Cd Isotope Analysis

Zhong Qiaohui^{1, 4
,
,},
Peng Bingyu^{1, 4},
He Chifeng^{1, 4},
Guo Jiakai^{1, 4},
Chu Gaobin²,
Yin Lu³,
Li Jie^{1
, ,}

1.
State Key Laboratory of Deep Earth Processes and Resources, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China
2.
Guangzhou Tuoyan Analytical Technology Co. Ltd., Guangzhou 510640, China
3.
Hebei Key Laboratory of Strategic Critical Mineral Resources, Hebei GEO University, Shijiazhuang 050031, China
4.
College of Earth and Planetary Sciences, University of Chinese Academy of Sciences, Beijing 100101, China

摘要

摘要:
地质和环境样品中Cd同位素组成的准确、高精度分析对于研究海洋初级生产力、古环境变化、重金属Cd污染的溯源、硫化物矿床的成因和海洋Cd循环等领域具有重要意义.然而，环境和地质样品的低Cd含量和复杂基体给高精度Cd同位素分析带来挑战.针对地质和环境样品，开发了一种高效可靠的两柱Cd色谱分离流程和高精度的Cd同位素测定方法.在第一柱AG-MP-1M阴离子交换树脂中，主要基体元素（包括≥99%的Sn）被优先去除，随后Cd及少量残余的Sn用4 mL 1 M HNO₃溶液快速洗脱.与传统第二柱分离Cd常用的TRU.Spec、UTEVA和BPHA萃取树脂不同，除了Mo、Sn、Zr等元素，TOPO树脂还能有效去除其他潜在残余基体元素（如Mg、Fe、Pb、Ti、V、Ag、Cu、Zn等），且避免了树脂来源有机质引入的问题.Cd同位素比值在Neptune Plus MC-CP-MS上测定，仪器的质量分馏采用Cd的双稀释剂法（¹¹¹Cd-¹¹³Cd）校正.两个标准溶液（NIST SRM 3108和Spex Cd）长期测量值的外部精度优于0.05‰.采用优化的两柱Cd色谱分离流程处理地质和环境标准样品，其测定的Cd同位素值在误差范围内与文献报道值一致，证实了该方法准确可靠且高效实用.此外，首次报道了国内的地质标样GSR-2、GSR-3及土壤标样GSS-6a的Cd同位素组成，这些参考数据为不同实验室间Cd同位素分析能力的评估和数据质量控制提供了依据.综上，本研究为地质和环境样品的高精度Cd同位素分析建立了一种高效实用的可靠分析方法.
- Cd同位素 /
- TOPO树脂 /
- 色谱分离 /
- 双稀释剂法 /
- 地球化学
Abstract:
Accurate and high-precision analysis of Cd isotope composition in geological and environmental samples is of great significance for the study of marine primary productivity, paleoenvironmental changes, traceability of heavy metal Cd pollution, genesis of sulfide deposits, and marine Cd cycles. However, the low Cd content and complex matrix of environmental and geological samples pose challenges to high-precision Cd isotope analysis. For geological and environmental samples, this study developed an efficient and reliable two-column Cd chromatographic separation procedure and a high-precision Cd isotope determination method. In the first column of AG-MP-1M anion exchange resin, a large amount of the matrix, including ≥99% ratio of Sn, was removed first, then Cd and a small amount of Sn were rapidly eluted using 4 mL of 1M HNO₃ solution. Unlike the traditional second-column separation of Cd using TRU, Spec, UTVEA and BPHA extraction resins, in addition to Mo, Sn and Zr elements, TOPO resin can further separate other potential residual matrix elements such as Mg, Fe, Pb, Ti, V, Ag, Cu and Zn, etc., without causing problems with resin-derived organic matter. Cadmium isotope ratio was conducted on Neptune Plus MC-CP-MS, using double spike method (¹¹¹Cd-¹¹³Cd) for instrumental mass discrimination correction. The long-term external reproducibility for two standard solutions (NIST SRM 3108 and Spex Cd) was better than ±0.05‰ (2SD).Geological and environmental standard samples processed by the presented two-column Cd chromatographic separation procedure and then determined the δ^114/110Cd_{NIST 3108} values are consistent with the values reported in the literature within uncertainty, confirming the accuracy, reliability and efficiency of this method. Furthermore, the Cd isotope compositions of the domestic geological standard samples GSR-2 and GSR-3, and soil standard sample GSS-6a are reported for the first time, which are beneficially for evaluating the analytical capabilities between different laboratories and data quality control. Overall, this study will provide efficient and convenient new technique for the accurate and high-precision Cd isotope analysis of geological and environmental samples.
- Cd isotope /
- TOPO resin /
- chromatographic separation /
- double spike method /
- geochemistry

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图 1 不同酸介质下，Cd、Zn、Sn和Mo在TOPO树脂的分配系数

Fig. 1. Distribution coefficients of Cd, Zn, Sn and Mo in TOPO resin under different acid media

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图 2 不同酸介质下Cd的化学分离曲线

a. 0.5 mL TOPO树脂，GSR-3；b. 0.2 mL TOPO树脂，单元素的混合标准溶液

Fig. 2. Chemical separation curves of Cd under different acid media

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图 3 阴离子交换树脂的Cd化学分离曲线

Fig. 3. Chemical separation curve of Cd using anion exchange resin AG-MP-1M

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图 4 Cd色谱分离流程分离基体的效率

基体元素与Cd的浓度比表示为［X］/［Cd］，其中X表示基体元素

Fig. 4. The efficiency of the Cd chromatographic separation protocols in separating the matrix

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图 5 （a） NIST SRM 3108和（b）Spec-Cd的δ^114/110Cd_{NIST 3108}值的长期重现性

误差棒代表每次测量的两倍标准误差；浅色区域分别代表NIST SRM 3108和Spec-Cd的δ^114/110Cd_{NIST 3108}值的两倍标准偏差

Fig. 5. The long-term reproducibility of δ^114/110Cd_{NIST 3108} values for (a) NIST SRM 3108 and (b) Spec-Cd

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图 6 参考物质的Cd同位素组成包括本研究和以前的数据

橙色正方形代表本研究数据，其他符号代表文献数据.误差棒代表两倍标准偏差（2SD）.浅红色的区域表示δ^114/110Cd_BSE（-0.06‰±0.03‰；Pickard et al.， 2022）

Fig. 6. δ^114/110Cd values of reference materials including the data from this study and previous studies

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表 1 干扰Cd同位素测试的多原子团和同质异位素元素（Wombacher et al., 2003)

Table 1. Isobars and molecular interfering ions for Cd isotopic measurements (Wombacher et al., 2003)

质量数/丰度	多原子团	同质异位素
¹⁰⁶Cd(1.25%)	⁶⁶Zn⁴⁰Ar⁺, ⁹⁰Zr¹⁶O⁺,
¹⁰⁸Cd(0.89%)	⁶⁸Zn⁴⁰Ar⁺, ⁹²Zr¹⁶O⁺, ⁹²Mo¹⁶O⁺	¹⁰⁸Pd
¹¹⁰Cd(12.5%)	⁷⁰Zn⁴⁰Ar⁺, ⁷⁰Ge⁴⁰Ar⁺, ⁹⁴Zr¹⁶O⁺, ⁹⁴Mo¹⁶O⁺, ⁹²Mo¹⁸O⁺, ¹⁰⁹Ag¹H⁺, ⁹³Nb¹⁷O⁺	¹¹⁰Pd
¹¹¹Cd(12.8%)	⁷¹Ga⁴⁰Ar⁺, ⁹⁵Mo¹⁶O⁺, ⁹⁷Mo¹⁴N⁺, ⁹³Nb¹⁸O⁺
¹¹²Cd(24.1%)	⁷²Ge⁴⁰Ar⁺, ⁹⁶Zr¹⁶O⁺, ⁹⁶Mo¹⁶O⁺, ⁹⁶Ru¹⁶O⁺, ⁹⁸Mo¹⁴N⁺, ⁷⁶Se³⁶Ar⁺	¹¹²Sn
¹¹³Cd(12.2%)	⁷³Ge⁴⁰Ar⁺, ⁹⁷Mo¹⁶O⁺, ⁹⁹Ru¹⁴N⁺, ⁷⁷Se³⁶Ar⁺	¹¹³In
¹¹⁴Cd(28.7%)	⁷⁴Ge⁴⁰Ar⁺, ⁹⁸Mo¹⁶O⁺, ⁹⁸Ru¹⁶O⁺, ¹⁰⁰Ru¹⁴N⁺, ¹⁰⁰Mo¹⁴N⁺, ⁷⁷Se³⁶Ar⁺, ⁷⁴Se⁴⁰Ar⁺	¹¹⁴Sn
¹¹⁶Cd(7.49%)	⁷⁶Ge⁴⁰Ar⁺, ¹⁰⁰Mo¹⁶O⁺, ¹⁰⁰Ru¹⁶O⁺, ⁷⁶Se⁴⁰Ar⁺, ⁸⁰Se³⁶Ar⁺	¹¹⁶Sn

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表 2 两柱的Cd色谱分离流程

Table 2. The two-column chromatographic separation procedure of Cd

柱流程	试剂	体积(mL)
第一柱: AG-MP-1M树脂(2 mL)
平衡	2 M HCl_‘	10
上样	2 M HCl_‘	2~3
基体(Mg, Ca, Ni, Fe, Ga, Ge, Ag, Zr, etc.)	2 M HCl_‘	6
基体(Mo, In, Pb)	2 M HCl+3 M HF	16
基体(Zn, Sn, In)	0.05 M HCl	16
基体(Sn, In) 残余基体	0.015 M HCl 1 M HNO₃	8 2
接收Cd	1 M HNO₃	3
第二柱: TOPO树脂(0.2 mL)
平衡	1 M HCl	2
上样残余基体	1 M HCl 1 M HCl+0.1 M HNO₃	0.5 3
接收Cd	1 M HCl+0.5 M HNO₃	0.8

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表 3 MC⁃ICP⁃MS测试过程的典型仪器参数

Table 3. Typical instrumental setup during Neptune Plus MC-ICP-MS analysis

	仪器参数	Neptune Plus
	RF功率	1 056 W （每天优化）
	辅助气	0.88 L·min^‒1（每天优化）
	样品气	1.04 L·min^‒1（每天优化）
	冷却气	16.00 L·min^‒1
	连接锥	H样品锥+X截取锥
	放大器	10¹¹ Ω
	积分时间	4.19 s
	膜去溶	Aridus Ⅱ
	吹扫气	2.74 L·min^‒1
	辅助气（氮气）	2.6 L·min^‒1
	雾室温度	104 ℃
	脱溶温度	140 ℃
	Cd灵敏度	1 200~1 521 V·ppm^‒1
	雾化器	MicoFlow PFA-100; 流速: 100 μL·min^‒1
杯结构	L4
	L3	¹¹⁰Cd
	L2	¹¹¹Cd
	L1	¹¹²Cd
	C	¹¹³Cd
	H1	¹¹⁴Cd
	H2
	H3	¹¹⁶Cd
	H4	¹¹⁷Sn

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表 4 参考标样的Cd同位素组成

Table 4. Cd isotopic composition of reference materials

样品/类型	Cd(10^‒6)	δ^114/110Cd_{NIST 3108}	2SD	n	数据来源
GSR-2(GBW07104)/安山岩	0.056	0.088	0.046	2	本研究
		0.065	0.024	2	本研究
		0.079	0.017	2	本研究
		0.080	0.037	6	平均值(M=3)
GSR-3(GBW07105)/玄武岩	0.070	0.106	0.029	2	本研究
		0.173	0.017	2	本研究
		0.165	0.025	2	本研究
		0.155	0.066	6	平均值(M=3)
GSD-3a(GBW07303a)/沉积物	0.509	-0.091	0.033	2	本研究
		-0.054	0.032	2	本研究
		-0.111	0.052	2	本研究
		-0.085	0.061	6	平均值(M=3)
		-0.08	0.04		Peng et al. (2021)
		-0.095	0.055		Zhong et al. (2023b)
GSD-5a(GBW07305a)/沉积物	1.52	0.039	0.015	2	本研究
		0.042	0.042	2	本研究
		0.076	0.065	3	本研究
		0.056	0.047	7	平均值(M=3)
		0.036	0.064		Tan et al. (2020)
		0.01	0.02		Peng et al. (2021)
		0.062	0.046		Zhong et al. (2023b)
GSS-1a(GBW07401a)/土壤	2.98	-0.079	0.048	2	本研究
		-0.062	0.040	2	本研究
		-0.040	0.057	2	本研究
		-0.060	0.058	6	平均值(M=3)
		-0.078	0.050		Zhong et al. (2023b)
GSS-6a(GBW07406a)/土壤	0.340	-0.284	0.064	3	本研究
		-0.316	0.036	3	本研究
		-0.311	0.017	2	本研究
		-0.303	0.052	8	平均值(M=3)
注：本文和文献的Cd同位素数据都是以NIST SRM 3108标样为基准；n代表测量次数；M代表标样独立消解次数；2SD是两倍标准偏差.

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改进的两柱Cd色谱分离流程和高精度的Cd同位素分析

doi: 10.3799/dqkx.2025.122

作者简介:
钟桥辉（1993-），男，博士研究生，研究方向为金属稳定同位素分析方法研发. ORCID： 0000-0003-3825-8405. E-mail：1102058215@qq.com

通讯作者:
李杰, E-mail: jieli@gig.ac.cn

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Improved Two⁃Column Cd Chromatographic Separation Procedure and High⁃Precision Cd Isotope Analysis

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留言板

改进的两柱Cd色谱分离流程和高精度的Cd同位素分析

doi: 10.3799/dqkx.2025.122

作者简介: 钟桥辉（1993-），男，博士研究生，研究方向为金属稳定同位素分析方法研发. ORCID： 0000-0003-3825-8405. E-mail：1102058215@qq.com

通讯作者: 李杰, E-mail: jieli@gig.ac.cn

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Improved Two⁃Column Cd Chromatographic Separation Procedure and High⁃Precision Cd Isotope Analysis

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出版历程

目录

作者简介:
钟桥辉（1993-），男，博士研究生，研究方向为金属稳定同位素分析方法研发. ORCID： 0000-0003-3825-8405. E-mail：1102058215@qq.com

通讯作者:
李杰, E-mail: jieli@gig.ac.cn