CAJ | 학술논문

随着Os同位素在地质学领域定年与示踪的广泛应用，对分析测试精度和检出限提出了更高的要求。本文利用热表面电离质谱负离子模式（ HTIMS）对OsO3-进行测定，通过试剂纯化、器皿清洗等前处理步骤的优化保证了超低的化学流程空白和获得灵敏而稳定的仪器测量信号，建立了高精度pg-ng级Os同位素分析测试方法。采用逐级剥谱法扣除氧同位素干扰，采用内标迭代法按照指数规律对仪器的质量歧视效应进行校正，全流程Os空白为0.41 pg，1 pg的190 Os计数约85000 cps，质量分馏系数在0.1%以内。pg级Os采用离子计数器动态跳峰扫描模式进行测量，187 Os/188 Os值测量精度小于在0.2%以内；ng级Os采用法拉第杯静态接收模式采集信号，187 Os/188 Os值测量精度在0.005%以内。经国际上Os同位素标准溶液H2、JMC以及国家一级Re-Os同位素标准物质JCBY的验证，分析精度达到了国际同类实验室先进水平。本方法具有低空白、高灵敏度、高精度的特点，可为地质学研究提供高精度Os同位素数据。
수착Os동위소재지질학영역정년여시종적엄범응용，대분석측시정도화검출한제출료경고적요구。본문이용열표면전리질보부리자모식（ HTIMS）대OsO3-진행측정，통과시제순화、기명청세등전처리보취적우화보증료초저적화학류정공백화획득령민이은정적의기측량신호，건립료고정도pg-ng급Os동위소분석측시방법。채용축급박보법구제양동위소간우，채용내표질대법안조지수규률대의기적질량기시효응진행교정，전류정Os공백위0.41 pg，1 pg적190 Os계수약85000 cps，질량분류계수재0.1%이내。pg급Os채용리자계수기동태도봉소묘모식진행측량，187 Os/188 Os치측량정도소우재0.2%이내；ng급Os채용법랍제배정태접수모식채집신호，187 Os/188 Os치측량정도재0.005%이내。경국제상Os동위소표준용액H2、JMC이급국가일급Re-Os동위소표준물질JCBY적험증，분석정도체도료국제동류실험실선진수평。본방법구유저공백、고령민도、고정도적특점，가위지질학연구제공고정도Os동위소수거。
Higher analytical precision and lower detection limit are required in geological dating and tracing,due to the wide application of Os. In this study,high-precision determination of pg-ng Os by Hegative Ion Thermal Ionization Mass Spectrometry( HTIMS ) was established by reagent purification,vessel cleaning and chemical preparation to ensure the ultra-low blank and obtain sensitive and stable signals. Isobaric oxygen interferences are corrected by stepwise spectrum stripping,and mass discrimination effect is corrected by internal standard iteration. The total procedural blank of Os is 0. 41 pg,the signal of 1 pg 190 Os is about 85000 cps,and the mass fractionation factor is less than 0 . 1%. Pg level of Os is measured by ion counter dynamic jumping scan mode and the measurement precision of 187 Os/ 188 Os is less than 0 . 2%. ng level of Os using Faraday cup static mode yielded the measurement precision of 187Os/ 188Os less than 0. 005%. The measured value,187Os/ 188Os=0. 3361 ± 7(2RSD, n=9),for national reference material JCBY is identical with the certified value within uncertainty. The analysis precision meets the advanced international laboratory level. This method has the merits of low blank,high sensitivity and high accuracy,and can provide high-precision Os isotope data of geological samples.