首页|地质样品铊同位素分析预处理方法优化

地质样品铊同位素分析预处理方法优化

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铊同位素体系可以示踪天体演化、古环境变化、矿床成因及污染物迁移等地质过程.然而,目前用于铊同位素分析的样品消解和离子交换方法耗时较长,往往需要两周甚至更久;为了提高化学前处理效率,本文采用微波消解法分解样品,以AG1-X8阴离子交换树脂纯化铊,采用多接收器电感耦合等离子体质谱(MC-ICP-MS)测试,仪器的质量歧视用铅同位素标准溶液(NIST SRM981)校正.通过考察消解条件、淋洗曲线和基质效应,结果表明:采用微波消解法,在 2mL硝酸-2mL氢氟酸-0.5mL高氯酸的混合酸体系中选用适当的消解程序可以将 0.2g土壤标准物质GBW07406消解完全,总耗时不超过 2h;利用AG1-X8树脂,上样后,依次以 2mL 2mol/L硝酸-1%溴水淋洗 6次、2mL超纯水淋洗 1次和 2mL 0.1mol/L盐酸-6%二氧化硫淋洗 5次(收集铊),可有效地纯化铊;常见共存元素的干扰实验结果显示,树脂填充量为 2mL时,该淋洗流程所允许上样溶液中含有三价铁和三价铝离子的量分别不应超过 2.56mmol和 4.90mmol,否则会使铊的回收率降低.将此方法应用于 4个地质标准物质中铊同位素比值的测定,ε205TlGSB Tl的精密度(2SD,n=6)均优于 0.3;与文献的结果对比显示,标准物质 NOD-P-1、GBW07406和 GSP-2的 ε205Tl差值(ε205TlNIST 997-ε205TlGSB Tl)均为 0.8,NOD-A-1的ε205Tl差值为 0.7,说明方法具有较好的准确性;此外,可以估算标准物质GSB 04-1758-2004相对于NIST 997的ε205Tl值应约等于0.8.
Optimization of Pretreatment Method for Tl Isotope Analysis of Geological Samples
The thallium(Tl)isotope system can be utilized to track various geological processes,but the current sample digestion and ion exchange methods used for Tl isotope analysis take a long time.To improve the efficiency of chemical pretreatment of samples for Tl isotope analysis,the samples were decomposed by the microwave digestion method.In the mixed acid system of 2mL HNO3,2mL HF and 0.5mL HClO4,0.2g of GBW07406 could be completely dissolved by selecting the digestion procedure.The slurry was then loaded on AG1-X8 resin,followed by eluting with 2mL 2mol/L HNO3-1%Br2 for 6 times,2mL H2O for 1 time,and 2mL 0.1mol/L HCl-6%SO2 for 5 times(Tl collection).The amount of Fe3+ and Al3+ allowed in the sample solution should not exceed 2.56mmol and 4.90mmol respectively,otherwise the recovery rate of Tl will be reduced.Measurement ε205Tl values for four geological reference materials(NOD-P-1,NOD-A-1,GBW07406 and GSP-2)by multi-collector inductively coupled plasma-mass spectrometry(MC-ICP-MS)showed a good precision(2SD better than 0.3,n=6)and a fixed difference of 0.8 compared with the value in the literature,indicating that the ε205Tl value of GSB04-1758-2004 with respect to NIST 997 should be approximately equal to 0.8.The BRIEF REPORT is available for this paper at http://www.ykcs.ac.cn/en/article/doi/10.15898/j.ykcs.202311070174.

HNO3-HF-HClO4microwave digestionAG1-X8 anion exchange resinTl isotope compositionmulti-collector inductively coupled plasma-mass spectrometry

柒锦捷、余红霞、徐庆鸿、袁永海、杨锋、张惠评

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桂林理工大学地球科学学院,广西桂林 541006

桂林理工大学,广西隐伏金属矿产勘查重点实验室,广西桂林 541006

硝酸-氢氟酸-高氯酸 微波消解 AG1-X8阴离子交换树脂 铊同位素组成 多接收器电感耦合等离子体质谱法

国家重点研发计划广西壮族自治区研究生创新项目

2021YFC2900100YCBZ2022119

2024

岩矿测试
中国地质学会岩矿测试技术专业委员会 国家地质实验测试中心

岩矿测试

CSTPCD北大核心
影响因子:1.344
ISSN:0254-5357
年,卷(期):2024.43(2)
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