Determination of the substitution pattern in the polymer chain of cellulose acetates

Cellulose acetates have been investigated on different structural levels. Based on the determination of the acetate pattern of the monomers, a method has been developed to describe the distribution of the acetyl groups in the polymer chain. This approach comprises permethylation with methyl triflate, deacetylative deuteromethylation under alkaline conditions, random cleavage, remethylation with methyl-d3, FAB-MS analysis and comparison of the experimental data with those calculated for a random acetate pattern. Results are discussed with respect to the conditions of the acetylation reactions. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 3011–3016, 1999

[1]  R. Shapiro,et al.  Quantitative analysis by various g.l.c. response-factor theories for partially methylated and partially ethylated alditol acetates☆ , 1975 .

[2]  Petra Mischnick,et al.  Determination of the substitution pattern in the polymer chain of cellulose sulfates , 1998 .

[3]  B A Dmitriev,et al.  Structural characterization of the lipid A component of Pseudomonas aeruginosa wild-type and rough mutant lipopolysaccharides. , 1991, European journal of biochemistry.

[4]  H. Fink,et al.  66 – Wide angle X-ray and solid state 13C-NMR studies of cellulose alkalization , 1995 .

[5]  Shinichi Takahashi,et al.  Relationship between distribution of substituents and water solubility of O‐methyl cellulose , 1987 .

[6]  Jaap J. Boon,et al.  Substituent distribution along the cellulose backbone in O-methylcelluloses using GC and FAB-MS for monomer and oligomer analysis , 1995 .

[7]  P. Mischnick,et al.  Determination of the Substitution Pattern of Cationic Starch Ethers , 1997 .

[8]  Ionel Ciucanu,et al.  A simple and rapid method for the permethylation of carbohydrates , 1984 .

[9]  Petra Mischnick,et al.  Determination of the Substitution Pattern of Cellulose Acetates1 , 1991 .

[10]  M. G. Wirick A study of the enzymic degradation of CMC and other cellulose ethers , 1968 .

[11]  P. Mischnick,et al.  Rapid method for the determination of the substitution pattern of O-methylated 1,4-glucans by high-pH anion-exchange chromatography with pulsed amperometric detection , 1996 .

[12]  G. Kühn,et al.  Model studies on methyl amyloses: correlation between reaction conditions and primary structure , 1996 .

[13]  Gary R. Gray,et al.  ANALYSIS OF POSITIONS OF SUBSTITUTION OF O-ACETYL GROUPS IN PARTIALLY O-ACETYLATED CELLULOSE BY THE REDUCTIVE-CLEAVAGE METHOD , 1995 .

[14]  M. G. Wirick Study of the substitution pattern of hydroxyethylcellulose and its relationship to enzymic degradation , 1968 .

[15]  J. Kamerling,et al.  Composition analysis of carboxymethylcellulose by high- pH anion-exchange chromatography with pulsed amperometric detection , 1992 .

[16]  D. E. Willis,et al.  Calculation of Flame Ionization Detector Relative Response Factors Using the Effective Carbon Number Concept , 1985 .

[17]  J. Kennedy,et al.  Cellulose and cellulose derivatives : physico-chemical aspects and industrial applications , 1995 .

[18]  T. Iwata,et al.  Preparation and n.m.r. assignments of cellulose mixed esters regioselectively substituted by acetyl and propanoyl groups , 1992 .

[19]  Y. Tezuka 13C NMR determination of the distribution of two ester substituents in cellulose acetate butyrate , 1993 .

[20]  R. A. Gelman Characterization of carboxymethylcellulose: Distribution of substituent groups along the chain† , 1982 .

[21]  T. Fontaine,et al.  Analysis of pyruvic acid acetal containing polysaccharides by methanolysis and reductive cleavage methods. , 1991, Analytical biochemistry.

[22]  K. Uemura,et al.  Selective chemical modification of cyclomalto-oligosaccharides via tert-butyldimethylsilylation , 1989 .