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Title: Determination of Cellulose I Crystallinity by FT-Raman Spectroscopy

Source: In: Proceedings of the 15th International Symposium on Wood, Fiber and Pulping Chemistry, Oslo, Norway (June 15-18, 2009). Paper number: P-053_ISWFPC_Cellulose_Crystallinity. Oslo, Norway : Congress-Conference AS, 2009. 1 flash drive.

Author(s)Agarwal, U.P.; Reiner, R.S.; Ralph, S.A.

Publication Year: 2009  View PDF »

Category: Conference Proceedings
Associated Research Project(s):   FPL-4709-2A

Abstract: Two new methods based on FT-Raman spectroscopy, one simple, based on band intensity ratio, and the other, using a partial least-squares (PLS) regression model, are proposed to determine cellulose I crystallinity. In the simple method, crystallinity in semicrystalline cellulose I samples was determined based on univariate regression that was first developed using the Raman band intensity ratio of the 380 and 1096 cm-1 bands. For calibration purposes, 90% crystalline Whatman CC31 and cellulose mixtures with crystallinities in the range 12-72% were used. When the intensity ratios were plotted against the theoretical crystallinities of the mixtures the plot showed a linear correlation (correlation coefficient R2 = 0.995). Standard error calculated from five replicate Raman acquisitions indicated that the cellulose I Raman crystallinity model was reliable. Crystallinities of these cellulose mixtures were also calculated from x-ray diffractograms but these generated a correlation that was inferior compared to the one based on the Raman model. Additionally, using both Raman and x-ray techniques, sample crystallinities were determined from partially crystalline cellulose samples that were generated by grinding Whatman CC31 in a vibratory mill. The two techniques showed significant differences. In contrast to x-ray diffractograms, evidence of significant differences was present between the Raman spectra of low crystallinity celluloses and indicated that Raman spectroscopy was better suited to investigate differences between such samples.

Keywords: Correlation, statistics, analytic chemistry, cellulose, chemistry, wood chemistry, X-rays, Raman spectroscopy, Fourier transform spectroscopy, spectrum analysis, regression analysis, standard error, partial least squares, band intensity ratio, cellulose I, crystallinity

File size: 116 kb(s)

Date posted: 08/19/2009

This publication is also viewable on Treesearch:  view
RITS Product ID: 30797

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