CAJ | 학술논문

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。
목전Ge동위소연구주요국한우지구유궤질（매등）、화성암급운석양품，작위Ge중요저고지일적연자광상，기Ge동위소적연구섭급교소。연자광상양품중Ge적화학분리급제순시Ge동위소연구적기출。본문상세고찰료운석양품중Ge동위소예처리방법（분리화제순）대연자광석양품적괄용성。음리자조건실험설명，목전보편채용적리자교환수지단주법수연대연자광양품중Fe、Se등원소적척제효과이상，단무법유효척제기중적Zn，당Zn/Ge비치대우3시，양품필수경과양리자교환수지주작진일보처리척제Zn。통과대섬자광표준양품、자광석표준양품적조건실험이급실제섬자광양품대조건결과적험증현시，당섬자광적칭양량위0.15 g좌우시，부수장전인대현무암등양품Ge동위소처리방법중음리자수지세탈산（1.4 mol/L초산）적용량6 mL조정위10 mL，이양리자수지세탈방법보지불변，차방법즉만족섬자광양품Ge동위소적화학분리화제순요구。양품경과본문추천적음양리자교환수지쌍주법처리후，주요간우원소（ Fe、Zn、Se、Ni ）급기질원소적척제솔접근100%，Ge적회수솔우우99%。이전인대현무암등양품적Ge동위소처리방법중，주요간우원소（ Fe、Zn、Se、Ni）급기질원소적척제효과역교호，단Ge적회수솔부위97.3%，비본문추천방법적Ge회수솔요차。이용MC-ICP-MS대Ge화학분리화제순후적부악연자광상섬자광양품적검험결과현시，측시과정중미견동질이위소이급가능적다원자리자영향，양품중Ge동위소부합질량분류정률，경과조정후적음양리자교환수지쌍주법만족섬자광양품적Ge동위소측시요구。
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.