Abstract
In cellulose materials, the cellulose II polymorph is often present either exclusively or inconjunction with cellulose I, the natural cellulose. Moreover, in regenerated andmercerized fibers (e,g., viscose and lyocell), natural cellulose adopts to the crystalstructure cellulose II Therefore, its detection and quantitation are important for acomplete assessment of such materials investigations. In the Raman spectra of suchmaterials, a band at 577 cm -1 is typically observed indicating the presence of thispolymorph. In the present study, to quantify the content of cellulose II, a calibrationmethod was developed based on the intensity of the 577 cm -1 peak relative to the1096 cm -1 band of cellulose. For this purpose, in addition to pure cellulose I andcellulose II samples (respectively, Avicel PH-101 and mercerized Avicel PH-101; hencereferred to as Avicel I and Avicel II), a set of five samples were produced by mixingthem in known quantities of Avicel I and Avicel II. The crystalline cellulose II contents ofthe samples were calculated based on the X-ray crystallinity of mercerized Avicel I.These seven samples were included in the calibration set and their Raman spectrawere obtained. Subsequently, Raman intensity ratios I 577 /I 1096 were calculatedby taking ratios of peak intensities at 577 and 1096 cm -1 . These ratios were plottedagainst the % of crystalline cellulose II present in the calibration set samples and thetwo were found to be linearly correlated (R 2 = 0.9944). The set-samples were alsoanalyzed using XRD which were then compared with the Raman method developedhere. Compared to XRD, the Raman method was found to be more sensitive atdetecting and quantifying cellulose II. Additionally, several cellulose II containingmaterials were analyzed by the new Raman method.
Detection and quantitation of cellulose II by Raman spectroscopy
