Abstract
The alditol acetate method is a common procedure for sugar analysis, also applied to determine the substituent distribution in monomer units of polysaccharide ethers like methyl cellulose by gas liquid chromatography. Consisting of several preparation and work-up steps this procedure is both time consuming and prone to side reactions that promote discrimination of single constituents, especially when no peralkylation step is performed prior to hydrolysis. As a consequence results scatter in dependence on individual treatment and conditions. In the context of this work these critical points were overcome by strict but simplified work-up procedures and using acid instead of alkaline catalyzed acetylation. Under the acidic conditions the tedious removal of borate is no longer necessary and a reduced time requirement was achieved as well as good reproducibility. Comparison with independent reference methods excluded a systematic error of the method and confirmed the results obtained. Without peralkylation, i.e. in the presence of free hydroxyl groups, another fast modification of the method using DMSO as solvent, no removal of borate, and 1-methylimidazole as catalyst for acetylation was found to produce a systematic error.
Abbreviations
- AAM:
-
Alditol acetate method
- AGU:
-
Anhydro glucose unit
- ATR-IR:
-
Attenuated total reflection infra red
- BSTFA:
-
N,O–bis(trimethylsilyl)-trifluoroacetamide
- c i :
-
i-fold substituted monomer units
- DMSO:
-
Dimethyl sulfoxide
- DS:
-
Degree of substitution
- ECR:
-
Effective carbon response
- ESI:
-
Electrospray ionization
- FID:
-
Flame ionization detector
- GLC:
-
Gas liquid chromatography
- HMF:
-
Hydroxymethylfurfural
- MC:
-
Methyl cellulose
- MEC:
-
Methyl ethyl cellulose
- MS:
-
Mass spectrometry
- MWCO:
-
Molecular weight cut off
- n:
-
Number of experiments
- r. t.:
-
Room temperature
- s i :
-
Molar fraction of monomers substituted at O-i
- TES:
-
Triethylsilyl/triethylsilane
- TFA:
-
Trifluoroacetic acid
- TMS:
-
Trimethylsilyl/trimethylsilane
- x i :
-
Partial degree of substitution in position i
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Acknowledgments
Financial support of the WoodWisdom-Net and the Bundesministerium für Bildung und Forschung (BMBF FKZ 0330837A) and of Dow Wolff Cellulosics GmbH (Dow), Germany, is gratefully acknowledged.
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Voiges, K., Adden, R., Rinken, M. et al. Critical re-investigation of the alditol acetate method for analysis of substituent distribution in methyl cellulose. Cellulose 19, 993–1004 (2012). https://doi.org/10.1007/s10570-012-9663-y
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DOI: https://doi.org/10.1007/s10570-012-9663-y