Nishida Kozue, Ishimura Toyoho
Department of Chemistry and Material Engineering, National Institute of Technology, Ibaraki College, 866 Nakane, Hitachinaka, Ibaraki, 312-8508, Japan.
Rapid Commun Mass Spectrom. 2017 Nov 30;31(22):1875-1880. doi: 10.1002/rcm.7966.
The new international reference material IAEA-603 (calcite) for stable carbon and oxygen isotopes (δ C and δ O values) was released in 2016 to replace the previous reference material, NBS19 (exhausted). We examined the grain-scale isotopic variations in IAEA-603 for application to microscale isotopic analysis of carbonate samples.
Individual grains of IAEA-603 were analyzed with an IsoPrime100 isotope ratio mass spectrometer with a customized continuous-flow gas preparation system (MICAL3c). The individual grains of IAEA-603 were observed by optical and scanning electron microscopy, and their observational characteristics (grain color and size) were compared with their stable isotope compositions.
Translucent grains (main component of IAEA-603; grain weight, 4-132 μg) had homogeneous isotopic ratios, comparable with the grain-scale isotopic homogeneity of NBS 19. Their average δ C and δ O values were the same as the recommended values determined by the IAEA. Opaque (whitish) grains (1-2 per 100 grains; grain weight, 8-63 μg) were significantly more depleted in C and O than the translucent grains.
Low-abundance opaque grains (1-2 grains out of 100 grains) have lower δ C and δ O values, suggesting that these grains should be eliminated when using IAEA-603 for single-grain (microscale) isotope analysis.
用于稳定碳和氧同位素(δC和δO值)的新型国际参考物质IAEA - 603(方解石)于2016年发布,以取代先前的参考物质NBS19(已耗尽)。我们研究了IAEA - 603中颗粒尺度的同位素变化,以便应用于碳酸盐样品的微观尺度同位素分析。
使用配备定制连续流气体制备系统(MICAL3c)的IsoPrime100同位素比率质谱仪分析IAEA - 603的单个颗粒。通过光学显微镜和扫描电子显微镜观察IAEA - 603的单个颗粒,并将其观察特征(颗粒颜色和大小)与其稳定同位素组成进行比较。
半透明颗粒(IAEA - 603的主要成分;颗粒重量为4 - 132μg)具有均匀的同位素比率,与NBS 19的颗粒尺度同位素均匀性相当。它们的平均δC和δO值与国际原子能机构确定的推荐值相同。不透明(白色)颗粒(每100个颗粒中有1 - 2个;颗粒重量为8 - 63μg)的13C和18O明显比半透明颗粒贫化。
低丰度的不透明颗粒(100个颗粒中有1 - 2个)具有较低的δC和δO值,这表明在使用IAEA - 603进行单颗粒(微观尺度)同位素分析时应去除这些颗粒。