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首页> 外文期刊>Applied Spectroscopy >Variable-Temperature Fourier Transform Infrared Spectroscopic Investigations of Poly(3-Hydroxyalkanoates) and Perturbation-Correlation Moving-Window Two-Dimensional Correlation Analysis. Part I: Study of Non-Annealed and Annealed Poly(3-Hydroxybutyrate) Homopolymer
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Variable-Temperature Fourier Transform Infrared Spectroscopic Investigations of Poly(3-Hydroxyalkanoates) and Perturbation-Correlation Moving-Window Two-Dimensional Correlation Analysis. Part I: Study of Non-Annealed and Annealed Poly(3-Hydroxybutyrate) Homopolymer

机译：聚（3-羟基链烷酸酯）的变温傅里叶变换红外光谱研究和微扰相关移动窗口二维相关分析。第一部分：未退火和退火的聚（3-羟基丁酸）均聚物的研究

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Generalized two-dimensional correlation spectroscopy (2DCOS) and perturbation-correlation moving-window two-dimensional (PCMW2D) correlation spectroscopy were applied to explore the melting behavior of non-annealed and annealed poly(3-hydroxybutyrate) (PHB) homopolymer as studied by variable-temperature Fourier transform infrared (FT-IR) spectroscopy. The absorption band of the C=O stretching vibration was employed to investigate the structural changes during the heating process (30–200 °C). Non-annealed PHB showed a recrystallization process in the temperature range 30–120 °C. In the asynchronous 2D correlation spectrum we clearly captured the existence of two components in the crystallinity-sensitive wing of the C=O stretching mode: a well-ordered crystalline state at lower wavenumbers (1718 cm−1) and a less ordered crystalline state at higher wavenumbers (1724 cm−1). These crystallinity-sensitive bands at 1718 and 1724 cm−1, which are not readily detectable in the one-dimensional (1D) FT-IR spectra, share asynchronous cross-peaks with bands at around 1737 and 1747 cm−1 assignable to the C=O stretching absorptions due to the amorphous components. In the case of the melting process of non-annealed PHB in the temperature range 120–200 °C, it is helpful to use the PCMW2D correlation analysis, which indicates the recrystallization between 40 and 110 °C by the shift of the C=O stretching band from 1726 cm−1 to 1722 cm−1 and the sharp change to the broad amorphous C=O stretching absorption at 1747 cm−1 at the melting temperature of PHB around 190 °C. For an annealed sample of PHB only the melting behavior was observed in the PCMW2D correlation analysis by the sharp transition from the crystalline to the amorphous C=O stretching band.
机译：通过广义二维相关光谱（2DCOS）和摄动相关移动窗口二维（PCMW2D）相关光谱，研究了非退火和退火的聚（3-羟基丁酸酯）（PHB）均聚物的熔融行为。可变温度傅立叶变换红外（FT-IR）光谱。利用C = O拉伸振动的吸收带来研究加热过程（30–200°C）中的结构变化。未退火的PHB在30–120°C的温度范围内显示出重结晶过程。在异步2D相关光谱中，我们清楚地捕获了C = O拉伸模式的对结晶度敏感的机翼中存在的两个成分：在较低波数（1718 cm -1 ）上有序的晶体状态在较高的波数（1724 cm -1 ）处晶序较少。这些在1718和1724 cm -1 上对结晶度敏感的谱带在一维（1D）FT-IR光谱中不易检测到，它们与1737和1747左右的谱带共享异步交叉峰。 cm -1 可以归因于无定形成分的C = O拉伸吸收。对于未退火的PHB在120–200°C的温度范围内的熔化过程，使用PCMW2D相关分析是有帮助的，它通过C = O的变化指示40至110°C之间的重结晶。从1726 cm -1 到1722 cm -1 的拉伸带，在1747 cm -1 在PHB的熔化温度190°C附近。对于退火的PHB样品，在PCMW2D相关性分析中，仅观察到了熔融行为，即从晶体到无定形C = O拉伸带的急剧转变。

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    《Applied Spectroscopy》 |2009年第9期|1027-1033|共7页
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