連続フロー型質量分析計による固体試料の炭素・硫黄同位体比分析 : 高精度分析のための改善点
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Continuous flow isotope ratio mass spectrometry (CF-IRMS) has significant advantages over the classic off-line methods in terms of high sensitivity and short analytical time. These advantages play an important role in expansion of its application to many scientific fields. However, the precision for isotope analysis by CF-IRMS has been believed to be lower than that of the off-line methods. In this study, a detailed evaluation of the performance of CF-IRMS for carbon and sulfur isotope analysis for solid materials is reported. High-precision, similar to the offline methods (within ±0.1 ‰), was achieved for carbon isotope analyses after the following improvements: (1) stabilization of room temperature (within ±0.1℃ in 10 minutes). (2) minimization of the non-linearity effect (i.e., pressure effect for instrumental isotopic fracionation) by the adjustment to a proper ion-repeller voltage. (3) reduction of background gas by using pre-heated tin capsules and high-grade helium and oxygen. In addition to the improvements mentioned above, high-precision isotope analyses (within ±0.1 ‰) of sulfur in solid materials require the following improvements: (1) stabilization of reference gas pressure by installing a centrifuge fan to properly exhaust the reference gas. (2) equilibrium of oxygen isotopes using a tube filled with quartz wool. (3) minimization of a memory effect by using polytetrafluoroethylene (PTFE) tubes and a PTFE gas-chromatography column. (4) use of V_2O_5 with a low sulfur content.
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- 連続フロー型質量分析計による固体試料の炭素・硫黄同位体比分析 : 高精度分析のための改善点