Publication Details

Category Text Publication
Reference Category Journals
DOI 10.1002/rcm.2743
Title (Primary) Rapid online equilibration method to determine the D/H ratios of non-exchangeable hydrogen in cellulose
Author Filot, M.S.; Leuenberger, M.; Pazdur, A.; Böttger, T.
Source Titel Rapid Communications in Mass Spectrometry
Year 2006
Department ISOHYD
Volume 20
Issue 22
Page From 3337
Page To 3344
Language englisch
Abstract An improved method for the determination of deuterium-to-hydrogen (D/H) ratios of non-exchangeable hydrogen in cellulose is presented. The method is based on the equilibration reaction of the hydroxyl hydrogen of cellulose and water vapour of known isotopic composition. The equilibrated cellulose is pyrolysed and the total D/H ratio determined by subsequent online isotope ratio mass spectrometry (IRMS). With a mass balance system the D/H ratio of non-exchangeable hydrogen is recalculated after an empirical calibration has been performed, yielding a mean exchangeability of 0.239 and an equilibrium fractionation factor of 1.082 between the hydroxyl hydrogen of cellulose and water hydrogen at 110 degrees C. Equilibration takes 10 min per sample. Results obtained by this online equilibration method agree very well with values obtained by the nitration technique (R-2 = 0.941). The uncertainty of the equilibration method is +/- 4 parts per thousand resulting from a single standard deviation of +/- 2.8 parts per thousand for the equilibration determined by standard cellulose and 2.8 parts per thousand from the variable exchangeability of the hydroxyl hydrogen in cellulose due to crystalline areas. The latter uncertainty may be lowered by minimising the crystallinity of the cellulose. Advantages of this new technique are (i) the considerably reduced sample amount required (as low as 0.2 mg, ideally 0.5 mg compared with 20 mg for the conventional nitration technique); (ii) an approximately 100-fold reduced process time; and (iii) no need for the hazardous chemicals used in the nitration technique.
Persistent UFZ Identifier https://www.ufz.de/index.php?en=20939&ufzPublicationIdentifier=2608
Filot, M.S., Leuenberger, M., Pazdur, A., Böttger, T. (2006):
Rapid online equilibration method to determine the D/H ratios of non-exchangeable hydrogen in cellulose
Rapid Commun. Mass Spectrom. 20 (22), 3337 - 3344 10.1002/rcm.2743