摘要
目前Ge同位素研究主要局限于地球有机质(煤等)、火成岩及陨石样品,作为Ge重要储库之一的铅锌矿床,其Ge同位素的研究涉及较少。铅锌矿床样品中Ge的化学分离及提纯是Ge同位素研究的基础。本文详细考察了陨石样品中Ge同位素预处理方法(分离和提纯)对铅锌矿石样品的适用性。阴离子条件实验说明,目前普遍采用的离子交换树脂单柱法虽然对铅锌矿样品中Fe、Se等元素的剔除效果理想,但无法有效剔除其中的Zn,当Zn/Ge比值大于3时,样品必须经过阳离子交换树脂柱作进一步处理剔除Zn。通过对闪锌矿标准样品、锌矿石标准样品的条件实验以及实际闪锌矿样品对条件结果的验证显示,当闪锌矿的称样量为0.15 g左右时,仅需将前人对玄武岩等样品Ge同位素处理方法中阴离子树脂洗脱酸(1.4 mol/L硝酸)的用量6 mL调整为10 mL,而阳离子树脂洗脱方法保持不变,此方法即满足闪锌矿样品Ge同位素的化学分离和提纯要求。样品经过本文推荐的阴阳离子交换树脂双柱法处理后,主要干扰元素(Fe、Zn、Se、Ni)及基质元素的剔除率接近100%,Ge的回收率优于99%。而前人对玄武岩等样品的Ge同位素处理方法中,主要干扰元素(Fe、Zn、Se、Ni)及基质元素的剔除效果亦较好,但Ge的回收率仅为97.3%,比本文推荐方法的Ge回收率要差。利用MC-ICP-MS对Ge化学分离和提纯后的富乐铅锌矿床闪锌矿样品的检验结果显示,测试过程中未见同质异位素以及可能的多原子离子影响,样品中Ge同位素符合质量分馏定律,经过调整后的阴阳离子交换树脂双柱法满足闪锌矿样品的Ge同位素测试要求。
Up to the present,main research of Ge isotopes has been carried out on organic,magmatic and meteoritic samples. Pb-Zn deposits are one of the most important reservoirs of Ge;however,there are few studies on Ge isotopes for these samples. Ge separation and purification for samples collected from Pb-Zn deposits are the basis of Ge isotope research. Therefore,the suitability for Pb-Zn ores of the Ge isotopic purification method established for meteoritic samples in details has been investigated. The results demonstrate that anion exchange resins single-column method for Pb-Zn ores can eliminate the potential interferences efficiently（ including Fe,Se and other interfering matrix elements）,but does not work for Zn as Zn/Ge﹥3,indicating that further separation and purification by ion-exchange column are needed to eliminate Zn. Conditional experiments of standard samples （ ores and sphalerite）and three sphalerite samples from the Fule deposits showed that adjusting the volume of anion exchange resin elution acid（1. 4 mol/L,HNO3 ）from 6 mL to 10 mL and maintaining the method of cation exchange resin is suitable for Ge isotope purification. The results of anion/cation exchange resin two-column procedure indicate that the recovery of Ge was better than 99%,and the potential interferences on Ge isotopes （ including Fe,Se,Zn and other interfering matrix elements）were almost 100% eliminated. Although the previous method has a good recovery of Ge（97. 3%）and the potential interferences on Ge isotopes（including Fe,Se,Zn and other interfering matrix elements ） were reduced to the negligible levels,the recovery is lower than the recommended method in this paper. Furthermore,the Ge isotopic composition of three sphalerite samples from the Fule deposit show that there are no signals coming from interfering elements and matrix elements,and the mass fractionation of Ge isotope followed the rule of mass-dependent fractionation. Overall,this modified method for Ge isotope measurement is suitable for sphalerite samples.
出处
《岩矿测试》
CAS
CSCD
北大核心
2014年第3期305-311,共7页
Rock and Mineral Analysis
基金
中国科学院矿床地球化学国家重点实验室"十二五"项目群(SKLODG-ZY125-070)
中国科学院国家外国专家局创新团队国际合作伙伴计划"陆内成矿作用研究团队"(KZZD-EW-TZ-20)
国家自然科学基金(40930425
41173026
41173029)
关键词
Ge同位素
闪锌矿
分离提纯
预处理方法
Ge isotopes
sphalerite
separation and purification
pre-treatment method
