Centre for Stable Isotope Research and Analysis, Büsgen Institute, Georg-August-University Göttingen, Büsgenweg 2, 37077, Göttingen, Germany.
Rapid Commun Mass Spectrom. 2014 May 15;28(9):1019-22. doi: 10.1002/rcm.6878.
A high sensitivity elemental analyzer/isotope ratio mass spectrometer setup was developed to allow analysis of (13)C and (15)N isotopic composition on microgram amounts of C and N, respectively.
Increased sensitivity of a conventional elemental analyzer equipped with a low blank autosampler was obtained by decreased carrier gas flow of 35 mL/min. The diameters of the oxidation and reduction reactors and water trap were reduced to 7.8, 7.8 and 4 mm i.d., respectively, to obtain sharp sample peaks in the mass spectrometer. To increase the lifetime of the reduction reactor, a 1:1 He/O2 mixture was used as oxidizing agent in the elemental analyzer.
Sample amounts of 0.6 µg N and 1 µg C were sufficient for accurate isotopic analysis with <1 ‰ standard error after blank correction. One major advantage of the setup is the easy switching between conventional EA and μEA as only consumable parts need to be exchanged.
The proposed setup proved to be suitable to analyze minute amounts of C and N in one analytical run simultaneously.
开发了一种高灵敏度元素分析仪/同位素比质谱仪装置,可分别分析微克级的 C 和 N 的 (13)C 和 (15)N 同位素组成。
通过将载气流速降低至 35 mL/min,提高了配备低空白自动进样器的常规元素分析仪的灵敏度。氧化和还原反应器以及水阱的直径分别减小到 7.8、7.8 和 4 mm i.d.,以在质谱仪中获得尖锐的样品峰。为了延长还原反应器的使用寿命,在元素分析仪中使用 1:1 的 He/O2 混合物作为氧化剂。
经过空白校正后,样品量为 0.6 µg N 和 1 µg C 即可进行准确的同位素分析,标准误差<1 ‰。该装置的一个主要优点是可以轻松在传统 EA 和 μEA 之间切换,只需更换消耗品即可。
该装置可用于在一次分析运行中同时分析微量的 C 和 N。