Raman spectroscopic investigation of acetylation of raw cotton

Raman spectroscopy has been used to investigate raw cotton acetylation using acetic anhydride/4-dimethylaminopyridine (DMAP) catalyst blend without solvent. The Raman data further confirm successful acetylation as shown by FTIR that was demonstrated previously to be highly sensitive for determining the level of acetylation. However, the Raman peaks are much weaker than the FTIR bands. Nevertheless, the variations of the extent of acetylation estimated from both Raman and FTIR spectra with weight percent gain due to acetylation (WPG) were observed to follow the same pattern. The degrees of acetylation calculated from Raman data were also found to increase linearly with that calculated from the more sensitive FTIR technique. Raman technique is thus suitable for further development as an analytical tool for determining the acetylation level of natural cellulose fibres. Raman data have also shown that the acetylation reaction reduces the crystallinity of cotton. (c) 2005 Elsevier B.V. All rights reserved

X-ray diffraction and Raman spectroscopic studies of Zn-substituted carrboydite-like compounds

Hydrotalcite-like compounds of the formula NixZn6-xAl2(OH)(16)(SO4)(.)4H(2)O where x varies from 0 to 6, equivalent to a zinc-substituted carrboydite have been synthesised and characterised by X-ray diffraction, electron microscopy and vibrational spectroscopy. Both the d (003) spacing and the crystallite size are a function of the amount of zinc replacement for nickel in the carrboydite-like compounds. Transmission electron microscopy (TEM) shows the clay-like crystal structure for these hydrotalcite compounds. These compounds were characterised by vibrational spectroscopic techniques and a comparison made with the naturally occurring minerals. Additional bands in the sulphate antisymmetric stretching and bending region leads to the conclusion that the symmetry of the sulphate anion is reduced inferring the bonding of the sulphate anion to the hydrotalcite hydroxyl surface. (c) 2005 Elsevier B.V. All rights reserved