Low Temperature Catalytic Combustion Reactors for High Precision Carbon Isotope Measurements in Gas Chromatography Combustion Isotope Ratio Mass Spectrometry.

ANALYTICAL CHEMISTRY(2019)

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摘要
Metal oxide-filled reactors constructed with ceramic tubes or fused silica capillary are widely used for combustion in gas chromatography combustion isotope ratio mass spectrometry (GCC-IRMS). However, they tend to be easily cracked or broken and prone to leaks at operating temperatures of similar to 950 degrees C. Here we introduce a modified commercially available catalytic combustion/reduction methanizer to quantitatively convert organics to CO2 for delta C-13 analysis while retaining chromatographic resolution. These modified "ARC" reactors operate with a transition-metal catalyst that requires a flowing O-2 gas to enable complete conversion to CO2 at lower temperature (620 degrees C) with acceptable reactor life, reduced complexity, and improved robustness. Performance of two versions of the ARC reactors with different combustion volumes was characterized by analysis of steroid and alkane isotopic standard materials. Linearity of steroid isotopic standards ranged from 0.02 to 0.60 parts per thousand/V in the range of 25 to 200 ng of each steroid injected. Precisions and accuracies of measurements for steroids and alkanes had average standard deviations of SD(delta C-13) less than +/- 0.18 parts per thousand and average accuracy of better than 0.19 parts per thousand delta C-13(VPDB). Peak width expansion within both devices were similar to that in traditionally used metal oxide reactors. These data demonstrate for the first time that novel combustion schemes enable operation at lower temperatures as an alternative approach comparable to high temperature techniques to yield high precision delta C-13 data with GCC-IRMS.
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关键词
chromatography,carbon,reactors
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