Routine hydrogen isotope measurement of cellulose nitrate by high-temperature pyrolysis - reference materials and precision

The determination of isotope ratios of non‐exchangeable hydrogen in tree‐ring cellulose is commonly based on the nitration of wood cellulose followed by online high‐temperature pyrolysis and isotope ratio mass spectrometry measurement of cellulose nitrate samples. The application of this method requ...

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Bibliographic Details
Published in:Rapid communications in mass spectrometry 2007-09, Vol.21 (18), p.3085-3092
Main Authors: Knöller, Kay, Boettger, Tatjana, Haupt, Marika, Weise, Stephan M.
Format: Article
Language:English
Subjects:
Collodion - analysis
Collodion - chemistry
Germany
Hot Temperature
Isotope Labeling - methods
Isotope Labeling - standards
Mass Spectrometry - methods
Mass Spectrometry - standards
Reference Values
Reproducibility of Results
Sensitivity and Specificity
Water - chemistry
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Summary:The determination of isotope ratios of non‐exchangeable hydrogen in tree‐ring cellulose is commonly based on the nitration of wood cellulose followed by online high‐temperature pyrolysis and isotope ratio mass spectrometry measurement of cellulose nitrate samples. The application of this method requires a proper calibration using appropriate reference materials whose δ2H values have been reliably normalized to the V‐SMOW/SLAP scale. In our study, we achieve this normalization by a direct alternating measurement of reference waters (V‐SMOW and SLAP) and three cellulose nitrates chosen as reference materials. For that purpose, both water and solid organic samples are introduced into the pyrolysis reactor by silver capsule injection. The analytical precision of the water measurement using the capsule method is ±1.5‰. The hydrogen isotopic composition of three cellulose nitrate standards measured ranges from −106.7 to −53.9‰. The standard deviation of the calculated means from five measurement periods of those standards is better than 1‰. Twenty‐four different measurements of the hydrogen isotope composition of cellulose nitrate were evaluated in order to assess the precision of the described method. We obtained an analytical precision of ±3.0‰ as representative for the 95% confidence interval applicable for routine measurements of cellulose nitrate samples. Evidence was found for significant differences in the behavior of cellulose nitrate and PE foil during the pyrolitic conversion that emphasizes the need for a proper calibration of the routine measurements. This calibration can only be successful if the reference materials used have a very similar chemical composition and undergo the same preparation procedure as the samples. Copyright © 2007 John Wiley & Sons, Ltd.
ISSN:0951-4198
1097-0231
DOI:10.1002/rcm.3183