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Related Concept Videos

¹³C NMR: ¹H–¹³C Decoupling01:04

¹³C NMR: ¹H–¹³C Decoupling

The probability of having two carbon-13 atoms next to each other is negligible because of the low natural abundance of carbon-13. Consequently, peak splitting due to carbon-carbon spin-spin coupling is not observed in spectra. However, protons up to three sigma bonds away split the carbon signal according to the n+1 rule, resulting in complicated spectra.
A broadband decoupling technique is used to simplify these complex, sometimes overlapping, signals. Broadband decoupling relies on a...
Carbon-13 (¹³C) NMR: Overview01:10

Carbon-13 (¹³C) NMR: Overview

Carbon-13 is a naturally occurring NMR-active isotope of carbon with a low natural abundance of 1.1%. In contrast, carbon-12 is the most abundant isotope of carbon with zero nuclear spin. Therefore, it is NMR inactive. The gyromagnetic ratio of carbon-13 is smaller than that of protons. As a result, carbon-13 resonance is about 6000 times weaker than proton resonance. For a given magnetic field strength, the resonance frequency of carbon-13 is about one-fourth of the resonance frequency for...
¹H NMR: Complex Splitting01:13

¹H NMR: Complex Splitting

A proton M that is coupled to a proton X results in doublet signals for M. However, NMR-active nuclei can be simultaneously coupled to more than one nonequivalent nucleus. When M is coupled to a second proton A, such as in styrene oxide, each peak in the doublet is split into another doublet.
Splitting diagrams or splitting tree diagrams are routinely used to depict such complex couplings. While drawing splitting diagrams, the splitting with the larger coupling constant is usually applied first.
NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

The spin state of an NMR-active nucleus can have a slight effect on its immediate electronic environment. This effect propagates through the intervening bonds and affects the electronic environments of NMR-active nuclei up to three bonds away; occasionally, even farther. This phenomenon is called spin–spin coupling or J-coupling. Coupling interactions are mutual and result in small changes in the absorption frequencies of both nuclei involved. While nuclei of the same element are involved in...
Cellulose and Pectic Polysaccharides01:15

Cellulose and Pectic Polysaccharides

Every plant cell has a cell wall that protects the cell, provides structural support, and gives the cell shape. Cellulose, the main structural component of the plant cell wall, makes up over 30% of plant matter. It is the most abundant organic compound on earth.  Cellulose is an unbranched polysaccharide composed of linear chains of glucose molecules linked by β (1→4) glycosidic bonds.
As a cell matures, its cell wall specializes according to its type. For example, the parenchyma cells of...
NMR and Mass Spectroscopy of Carboxylic Acids01:30

NMR and Mass Spectroscopy of Carboxylic Acids

In ¹H NMR spectroscopy, acidic protons (–COOH) of carboxylic acids are highly deshielded and absorb far downfield, at around 9–12 ppm. The chemical shift value depends on the concentration and solvent used.
While α protons of carboxylic acids absorb at 2–2.5 ppm, β protons absorb further upfield.
Carboxylic acids are easily identified by dissolving them in deuterium oxide, which results in a rapid exchange of the acidic protons with deuterium. This leads to the disappearance of the acidic...

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Updated: Jul 13, 2026

Highly Stable, Functional Hairy Nanoparticles and Biopolymers from Wood Fibers: Towards Sustainable Nanotechnology
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Highly Stable, Functional Hairy Nanoparticles and Biopolymers from Wood Fibers: Towards Sustainable Nanotechnology

Published on: July 20, 2016

Solid-state 13C NMR study of na-cellulose complexes.

Fabrizio Porro1, Olivier Bédué, Henri Chanzy

  • 1Centre de Recherches sur les Macromolécules Végétales (CERMAV-CNRS), BP 53, F-38041, Grenoble cedex 9, France.

Biomacromolecules
|July 31, 2007
PubMed
Summary

Investigating cellulose and sodium hydroxide interactions using 13C NMR solid-state spectroscopy revealed distinct structural phases (Na-cellulose I, II, and Q). Lower temperatures enhance sodium hydroxide interaction with cellulose, influencing structural conformations and solubility.

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Area of Science:

  • Solid-state chemistry
  • Materials science
  • Polymer science

Background:

  • Microcrystalline cellulose (MCC) and wood pulp exhibit complex interactions with aqueous sodium hydroxide (NaOH).
  • Understanding these interactions is crucial for cellulose processing and material modification.

Purpose of the Study:

  • To investigate the structural changes of cellulose upon interaction with aqueous NaOH using 13C NMR solid-state spectroscopy.
  • To elucidate the phase behavior of the cellulose/NaOH system as a function of temperature and NaOH concentration.

Main Methods:

  • 13C NMR solid-state spectroscopy was employed to analyze microcrystalline cellulose and wood pulp treated with varying concentrations of aqueous NaOH at different temperatures.
  • Spectroscopic data were analyzed to identify structural changes, conformations, and phase transitions.

Main Results:

  • Distinct spectra corresponding to Na-cellulose I, Na-cellulose II, and a novel Q phase were identified, correlating with NaOH concentration and temperature.
  • Na-cellulose I exhibited a single glucosyl moiety as the independent magnetic residue with a gt conformation for the C6 hydroxymethyl group.
  • Na-cellulose II showed a cellotriosyl moiety as the independent magnetic residue with a gg conformation for the C6 hydroxymethyl groups.
  • The Q phase, observed in wood pulp, resulted from topological constraints not present in MCC.
  • Lower temperatures (268 K) intensified NaOH-cellulose interactions.

Conclusions:

  • A simplified phase diagram for the cellulose/NaOH system was proposed based on temperature and NaOH concentration.
  • The study provides insights into the structural basis of different cellulose-alkali phases and their formation conditions.