2-Chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane, a Reagent for the Accurate Determination of the Uncondensed and Condensed Phenolic Moieties in Lignins

The use of 2-chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane as a phosphitylation reagent in quantitative 31P NMR analysis of the hydroxyl groups in lignins has been thoroughly examined, and an experimental protocol recommended for spectra acquisition has been developed. Quantitative analysis of s...

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Bibliographic Details
Published in:Journal of agricultural and food chemistry 1995-06, Vol.43 (6), p.1538-1544
Main Authors: Granata, Alessandro, Argyropoulos, Dimitris S
Format: Article
Language:English
Subjects:
Analytical biochemistry: general aspects, technics, instrumentation
ANALYTICAL METHODS
Analytical, structural and metabolic biochemistry
Biological and medical sciences
CHEMICAL COMPOSITION
CHEMICAL REACTIONS
CHEMICAL STRUCTURE
COMPOSE ORGANOCHLORE
COMPOSICION QUIMICA
COMPOSITION CHIMIQUE
COMPUESTO ORGANICO DEL CLORO
ELABORACION DE PULPA
ESPECTROSCOPIA RMN
ESTRUCTURA QUIMICA
FOSFORO
Fundamental and applied biological sciences. Psychology
ISOTOPE RADIOACTIF
KRAFT LIGNINS
LIGNINAS
LIGNINE
LIGNINS
MILLED WOOD LIGNINS
NMR SPECTROSCOPY
ORGANOCHLORINE COMPOUNDS
PHOSPHORE
PHOSPHORUS
PHOSPHOTYLATION
PULPING
RADIOISOTOPES
RADIOISOTOPOS
REACCIONES QUIMICAS
REACTION CHIMIQUE
REDUCTION EN PATE
SPECTROSCOPIE RMN
STABLE ISOTOPES
STANDARD LIGNINS
STEAM EXPLOSION LIGNINS
STRUCTURE CHIMIQUE
SULFATE
SULFATOS
SULPHATES
TECHNIQUE ANALYTIQUE
TECNICAS ANALITICAS
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Description
Summary:The use of 2-chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane as a phosphitylation reagent in quantitative 31P NMR analysis of the hydroxyl groups in lignins has been thoroughly examined, and an experimental protocol recommended for spectra acquisition has been developed. Quantitative analysis of six "standard lignins" gave results comparable to those obtained by other methods of analysis. Excellent resolution of the various phenolic hydroxyl environments including those present in condensed moieties was observed. However, this was at the expense of resolution in the aliphatic hydroxyl region, where no distinction between primary, secondary, and the erythro and threo forms of the secondary hydroxyls of the beta-O-4 bonds can be made
ISSN:0021-8561
1520-5118
DOI:10.1021/jf00054a023