On the Interpretation of X‐Ray Diffraction Powder Patterns in Terms of the Nanostructure of Cellulose I Fibres

Garvey, Christopher J.; Parker, Ian H; Simon, George P.

doi:10.1002/macp.200500008

Cited by 246 publications

(186 citation statements)

References 42 publications

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“…This will result in lower crystallinity values because a higher contribution of the amorphous component would be subtracted. The suggestion is supported by both the diffractrogram deconvolution method which suggests a value of 21.5° (Garvey et al 2005) and the authors' current WAXS data where for amorphous Whatman CC31 sample a value of 21°was observed (Fig. 3j).…”

Section: Ball Milled Samplessupporting

confidence: 57%

Cellulose I crystallinity determination using FT–Raman spectroscopy: univariate and multivariate methods

2010

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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 cellulose I samples was determined based on univariate regression that was first developed using the Raman band intensity ratio of the 380 and 1,096 cm -1 bands. For calibration purposes, 80.5% crystalline and 120-min milled (0% crystalline) Whatman CC31 and six cellulose mixtures produced with crystallinities in the range 10.9-64% were used. When intensity ratios were plotted against crystallinities of the calibration set samples, the plot showed a linear correlation (coefficient of determination R 2 = 0.992). Average standard error calculated from replicate Raman acquisitions indicated that the cellulose Raman crystallinity model was reliable. Crystallinities of the cellulose mixtures samples were also calculated from X-ray diffractograms using the amorphous contribution subtraction (Segal) method and it was found that the Raman model was better. 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 the second approach, successful Raman PLS regression models for crystallinity, covering the 0-80.5% range, were generated from the ten calibration set Raman spectra. Both univariateRaman and WAXS determined crystallinities were used as references. The calibration models had strong relationships between determined and predicted crystallinity values (R 2 = 0.998 and 0.984, for univariateRaman and WAXS referenced models, respectively). Compared to WAXS, univariate-Raman referenced model was found to be better (root mean square error of calibration (RMSEC) and root mean square error of prediction (RMSEP) values of 6.1 and 7.9% vs. 1.8 and 3.3%, respectively). It was concluded that either of the two Raman methods could be used for cellulose I crystallinity determination in cellulose samples.

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Section: Ball Milled Samplessupporting

confidence: 57%

Cellulose I crystallinity determination using FT–Raman spectroscopy: univariate and multivariate methods

2010

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“…Individual crystalline peaks were first extracted by a curve-fitting process from the diffraction intensity profiles [20,21,22]. The CI was calculated by dividing the diffractogram area of crystalline cellulose by the total area of the original diffractogram.…”

Section: The Crystallinity Indexmentioning

confidence: 99%

Suitability of Date Palm Leaflets for Sulphated Cellulose Nanocrystals Synthesis

Hindi¹

2017

NNR

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Cellulose nanocrystals (SCNCs) were synthesized from macerated fibers isolated from leaflets of date palm (Phoenix dactylifera L.). The resultant SCNCs were characterized by optical, scanning and transmission electron microscopy, X-ray diffraction (XRD), Fourier transform infrared (FTIR) and thermogravimetric analysis (TGA). H 2 SO 4 -hydrolysis helped isolation of SCNCs with high crystallinity by removing the amorphous regions of the cellulosic microfibril. The SCNCs in an acidic solution were aggregated to form bigger architectures. The SCNCs exhibited a principle sharp peak around 2θ = 21.25° related to the cellulose-I structure. The crystallinity index of the SCNCs was found to be high (85.5%). The average crystallite size of the SCNCs was 2.7 nm. The FTIR results confirmed high purity of the SCNCs conforming to cellulose I. The TGA showed that about 59.13% of the SCNCs mass was lost up to 500°C. Based on the results, the leaflets are suitable precursor for SCNCs synthesis.

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“…The crystalline domain size of the Iβ cellulose was calculated via the Scherrer (1918) equation from the (002) reflection, to provide commonly quoted results (Garvey et al 2005). The alternative whole powder pattern modelling (WPPM) (Scardi and Leoni 2002), which gives a more physical quantitative result, was also tentatively employed.…”

Section: X-ray Diffraction Analysismentioning

confidence: 99%

Exploring Ulex europaeus to Produce Nontoxic Binderless Fibreboard

Pesenti¹,

Torres²,

Oliveira³

et al. 2017

BioResources

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Ulex europaeus is one of the most abundant and aggressively invasive plants on the world. Its fibres, which can be isolated using an alkaline pulping process, have been successfully thermo-pressed into high-density fibreboards without any type of binder. The influence of the bioorganic and crystalline components on the product was investigated using crystallographic, thermo-analytical, and mechanical techniques. Cellulose was predominantly an Iβ polymorph, more common in hardwood, but the composition of the material was typical of softwood. Both the crystallinity in the fibres and the average domain size of cellulose increased during thermo-pressing. Notwithstanding that the residual lignin was present in a small amount, this promoted the cohesion of fibres by improving hydrolysis and adhesion properties. The best overall properties were observed in the pressed products of 1030 ± 38 kg/m 3 , showing an elastic modulus of 4.31 ± 0.26 GPa, with a modulus of rupture of 26.5 ± 1.3 MPa. These results serve as the basis to transform the invasive species into a fully non-toxic added-value resource.

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On the Interpretation of X‐Ray Diffraction Powder Patterns in Terms of the Nanostructure of Cellulose I Fibres

Cited by 246 publications

References 42 publications

Cellulose I crystallinity determination using FT–Raman spectroscopy: univariate and multivariate methods

Cellulose I crystallinity determination using FT–Raman spectroscopy: univariate and multivariate methods

Suitability of Date Palm Leaflets for Sulphated Cellulose Nanocrystals Synthesis

Exploring Ulex europaeus to Produce Nontoxic Binderless Fibreboard

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