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Discrimination of Cellulose I, II, III I and III II Polymorphs in Cellulosic Fibers by NIR Hyperspectral Imaging Supported by XRD and XPS.

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Title: Discrimination of Cellulose I, II, III I and III II Polymorphs in Cellulosic Fibers by NIR Hyperspectral Imaging Supported by XRD and XPS.
Authors: Reyes-González, Isidora1,2 (AUTHOR), Carrillo-Varela, Isabel2,3 (AUTHOR), Rosales Charlín, Natacha1,3 (AUTHOR), Reyes-Contreras, Pablo2,4 (AUTHOR), Romero-Albornoz, Lucas2,5 (AUTHOR), Castillo, Rosario del P.2,4,6 (AUTHOR), King, Alistair W. T.1,5 (AUTHOR), Valdebenito, Fabiola2,6 (AUTHOR), Teixeira Mendonҫa, Regis1,2,3 (AUTHOR) rteixeira@udec.cl
Source: Polymers (20734360). May2026, Vol. 18 Issue 9, p1047. 17p.
Subjects: Cellulose fibers, Infrared imaging, Chemical processes, X-ray photoelectron spectroscopy, Crystal structure, X-ray powder diffraction, Cellulose
Abstract: Native cellulose I can be converted into crystalline polymorphs II and IIII, while cellulose II can be further converted into IIIII through chemical treatments that induce significant structural, physical, and chemical changes. Accurate identification and differentiation of these polymorphs is essential for predicting fiber reactivity and processing behavior, but current methods are time-consuming. This study demonstrates the potential of near-infrared hyperspectral imaging (HSI-NIR) combined with linear discriminant analysis as a rapid, non-destructive tool for polymorph discrimination. Cellulose I, II, IIII, and IIIII were produced from bleached kraft pulps of eucalyptus and pine and from cotton linters using NaOH (20% w/v) and ethylenediamine treatments. HSI-NIR successfully differentiated polymorphs based on spectral signatures in the 1480–1600 nm range, regardless of botanical source. Complementary characterization by XRD confirmed polymorph conversions, showing crystallinity reductions of 10–15% for cellulose I→II and I→IIII conversions, with crystallite size decreasing from 7.2 nm (cotton CI) to 3.2–3.4 nm in all CIIIII samples. XPS analysis revealed increased C-O surface accessibility in cellulose II and III, with complete disappearance of COOH groups in cellulose III samples. These results establish HSI as a promising screening tool for cellulose polymorph identification (>95% classification accuracy) and provide comprehensive baseline data on structural and chemical transformations that govern fiber reactivity in chemical and enzymatic processes. [ABSTRACT FROM AUTHOR]
Copyright of Polymers (20734360) is the property of MDPI and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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  Data: Discrimination of Cellulose I, II, III I and III II Polymorphs in Cellulosic Fibers by NIR Hyperspectral Imaging Supported by XRD and XPS.
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  Data: <searchLink fieldCode="DE" term="%22Cellulose+fibers%22">Cellulose fibers</searchLink><br /><searchLink fieldCode="DE" term="%22Infrared+imaging%22">Infrared imaging</searchLink><br /><searchLink fieldCode="DE" term="%22Chemical+processes%22">Chemical processes</searchLink><br /><searchLink fieldCode="DE" term="%22X-ray+photoelectron+spectroscopy%22">X-ray photoelectron spectroscopy</searchLink><br /><searchLink fieldCode="DE" term="%22Crystal+structure%22">Crystal structure</searchLink><br /><searchLink fieldCode="DE" term="%22X-ray+powder+diffraction%22">X-ray powder diffraction</searchLink><br /><searchLink fieldCode="DE" term="%22Cellulose%22">Cellulose</searchLink>
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  Data: Native cellulose I can be converted into crystalline polymorphs II and IIII, while cellulose II can be further converted into IIIII through chemical treatments that induce significant structural, physical, and chemical changes. Accurate identification and differentiation of these polymorphs is essential for predicting fiber reactivity and processing behavior, but current methods are time-consuming. This study demonstrates the potential of near-infrared hyperspectral imaging (HSI-NIR) combined with linear discriminant analysis as a rapid, non-destructive tool for polymorph discrimination. Cellulose I, II, IIII, and IIIII were produced from bleached kraft pulps of eucalyptus and pine and from cotton linters using NaOH (20% w/v) and ethylenediamine treatments. HSI-NIR successfully differentiated polymorphs based on spectral signatures in the 1480–1600 nm range, regardless of botanical source. Complementary characterization by XRD confirmed polymorph conversions, showing crystallinity reductions of 10–15% for cellulose I→II and I→IIII conversions, with crystallite size decreasing from 7.2 nm (cotton CI) to 3.2–3.4 nm in all CIIIII samples. XPS analysis revealed increased C-O surface accessibility in cellulose II and III, with complete disappearance of COOH groups in cellulose III samples. These results establish HSI as a promising screening tool for cellulose polymorph identification (>95% classification accuracy) and provide comprehensive baseline data on structural and chemical transformations that govern fiber reactivity in chemical and enzymatic processes. [ABSTRACT FROM AUTHOR]
– Name: AbstractSuppliedCopyright
  Label:
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  Data: <i>Copyright of Polymers (20734360) is the property of MDPI and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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        Value: 10.3390/polym18091047
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      – Code: eng
        Text: English
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      Pagination:
        PageCount: 17
        StartPage: 1047
    Subjects:
      – SubjectFull: Cellulose fibers
        Type: general
      – SubjectFull: Infrared imaging
        Type: general
      – SubjectFull: Chemical processes
        Type: general
      – SubjectFull: X-ray photoelectron spectroscopy
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      – SubjectFull: Crystal structure
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      – SubjectFull: X-ray powder diffraction
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      – SubjectFull: Cellulose
        Type: general
    Titles:
      – TitleFull: Discrimination of Cellulose I, II, III I and III II Polymorphs in Cellulosic Fibers by NIR Hyperspectral Imaging Supported by XRD and XPS.
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              M: 05
              Text: May2026
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              Y: 2026
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