Journal
ANALYTICAL CHEMISTRY
Volume 87, Issue 18, Pages 9443-9450Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.analchem.5b02475
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Funding
- Helmholtz Centre for Environmental Research (UFZ-Leipzig)
- Deutsche Forschungsgemeinschaft (Research Unit FOR 1530) [NI 1329/1-1]
- European Union's Seventh Framework Program (CSI: ENVIRONMENT) [PITN-GA-2010-264329]
- U.S. National Science Foundation [EAR-1052927]
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The traditional high-temperature conversion (HTC) approach toward compound-specific stable isotope analysis (CSIA) of hydrogen for heteroatom-bearing (i.e., N, Cl, S) compounds has been afflicted by fractionation bias due to formation of byproducts HCN, HCI, and H2S. This study presents a chromium-based high-temperature conversion (Cr/HTC) approach for organic compounds containing nitrogen, chlorine, and sulfur. Following peak separation along a gas chromatographic (GC) column, the use of thermally stable ceramic Cr/HTC reactors at 1100-1500 degrees C and chemical sequestration of N, Cl, and S by chromium result in quantitative conversion of compound-specific organic hydrogen to H-2 analyte gas. The overall hydrogen isotope analysis via GC-Cr/HTC-isotope ratio mass spectrometry (IRMS) achieved a precision of better than +/- 5 mUr along the VSMOW-SLAP scale. The accuracy of GC-Cr/HTC-IRMS was validated with organic reference materials (RM) in comparison with online EA-Cr/HTC-IRMS and offline dual-inlet IRMS. The utility and reliability of the GC-Cr/HTC-IRMS system were documented during the routine measurement of more than 500 heteroatom-bearing organic samples spanning a delta H-2 range of -181 mUr to 629 mUr.
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