Analytical Sciences

Abstract − Analytical Sciences, 36(8), 947 (2020).

Influencing Factors for Determining the Crystallinity of Native Cellulose by X-ray Diffraction
Shihua YU,* Zhigang LIU,** Na XU,*** Jie CHEN,** and Yan GAO**
*College of Chemical and Pharmaceutical Engineering, Jilin Institute of Chemical Technology, Jilin 132022, China
**Center of Analysis and Measurement, Jilin Institute of Chemical Technology, Jilin 132022, China
***College of Materials Science and Engineering, Jilin Institute of Chemical Technology, Jilin 132022, China
Full width at half maximum (FWHM) of diffraction peaks of native cellulose is larger than 1°. The diffraction peaks of the crystalline phase largely coincide with those of the amorphous phase of cellulose, leading to the low resolution. Therefore, when calculating the crystallinity of natural cellulose by fitting the peaks, only relying on the single evaluation factor of Rwp (R-weighted Pattern) may lead to great randomicity of calculation results. Due to the special crystal structure of natural cellulose and the characteristics of crystallinity determination by peak separation method, the XRD Rietveld fitting method is adopted to determine the crystallinity of native cellulose. Through limiting the convergence conditions of fitting functions, we firstly discuss the effects of peak shape functions, scanning range, and the positions of amorphous peaks on crystallinity determination, which helps to reduce the randomness of XRD in solving crystallinity of cellulose and improve the precision of calculation. Then, three evaluation indexes (Rwp, FWHM, and RSD) are used to evaluate the rationality of crystallinity calculation results. Moreover, the reproducibility and precision of the crystallinity of three kinds of natural cellulose are tested under the optimized conditions. At the same time, the optimized fitting method is adopted to calculate the content of cellulose I and II, which can be used to guide the selection of alkali concentration and alkali treatment time in the spinning process of native cellulose.