Cellulose crystalline structure and thermal properties under heat treatment: An investigation by 2D correlation of near infrared spectroscopy and differential scanning calorimetry

IF 17.7 1区化学 Q1 CHEMISTRY, MULTIDISCIPLINARY Accounts of Chemical Research Pub Date : 2024-06-15 DOI:10.1177/09670335241257649

Siti Hanifah Mahdiyanti, Masaki Asaoka, T. Inagaki, S. Tsuchikawa

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Abstract

This study investigated the thermal behavior and crystallinity of microcrystalline cellulose (MCC) under heat treatment using near infrared (NIR) spectroscopy and differential scanning calorimetry (DSC). The results showed that heat treatment reduced the crystallinity and thermal stability of MCC at a certain point, and that the changes in the chemical components and structure of MCC were correlated with the heat flow measured by DSC. The analysis was performed using two-dimensional correlation spectroscopy (2DCOS), which revealed the simultaneous changes in the NIR second-derivative spectra and the DSC thermograms of heat-treated MCC. Linear regression analysis showed a high r2 value of 0.90 between the DSC enthalpy change at 270 °C–400°C and the PC1 score of NIR second-derivative spectra at 7500–4100 cm−1. The 2DCOS synchronous map showed a positive correlation at 6656–6229 cm−1 with a r value of 0.70–0.98 for the endothermic reaction, and a negative correlation at 6229; 5620; 5401; 4844; 4535 cm−1 with a r value of −0.90 to −0.99 for the exothermic reaction. This study extended the knowledge on the thermal behavior and decomposition mechanisms of heat-treated MCC, and provided a useful method for cellulose characterization and identification.

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热处理下的纤维素结晶结构和热性能：近红外光谱和差示扫描量热仪的二维相关性研究

本研究利用近红外光谱法和差示扫描量热法研究了微晶纤维素（MCC）在热处理过程中的热行为和结晶度。结果表明，热处理在一定程度上降低了微晶纤维素的结晶度和热稳定性，微晶纤维素化学成分和结构的变化与 DSC 测得的热流相关。分析采用了二维相关光谱（2DCOS）技术，揭示了热处理后 MCC 的近红外二次衍射光谱和 DSC 热图的同步变化。线性回归分析表明，270°C-400°C 的 DSC 焓变与 7500-4100 cm-1 的近红外二次衍射光谱的 PC1 分数之间的 r2 值高达 0.90。二维COS同步图显示，内热反应在6656-6229 cm-1处呈正相关，r值为0.70-0.98；放热反应在6229；5620；5401；4844；4535 cm-1处呈负相关，r值为-0.90--0.99。这项研究扩展了人们对热处理 MCC 的热行为和分解机理的认识，为纤维素的表征和鉴定提供了一种有用的方法。

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来源期刊

Accounts of Chemical Research 化学-化学综合

CiteScore

31.40

自引率

1.10%

发文量

312

审稿时长

2 months

期刊介绍： Accounts of Chemical Research presents short, concise and critical articles offering easy-to-read overviews of basic research and applications in all areas of chemistry and biochemistry. These short reviews focus on research from the author’s own laboratory and are designed to teach the reader about a research project. In addition, Accounts of Chemical Research publishes commentaries that give an informed opinion on a current research problem. Special Issues online are devoted to a single topic of unusual activity and significance. Accounts of Chemical Research replaces the traditional article abstract with an article "Conspectus." These entries synopsize the research affording the reader a closer look at the content and significance of an article. Through this provision of a more detailed description of the article contents, the Conspectus enhances the article's discoverability by search engines and the exposure for the research.

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