FT‐IR and NIR Spectroscopic Imaging: Principles, Practical Aspects and Applications in Material and Pharmaceutical Sciences

Wessel, Elke; Vogel, Christian; Kolomiets, Olga; Hoffmann, Uwe; Siesler, Heinz W.

doi:10.1002/9783527628230.ch9

Cited by 10 publications

(7 citation statements)

References 69 publications

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“…The spatial resolution achieved with micro-ATR-FT-IR imaging using a Ge crystal is an improvement of approximately four times compared to the images obtained without the Ge crystal. [6][7][8] The measurement of spatial resolution was conducted using a vertically oriented sharp interface between two polymer laminates of similar refractive indices. The distance required for the step function to change from~95% tõ 5% of the maximum at the interface is defined as the spatial resolution achieved.…”

Section: Micro-attenuated Total Reflection Fourier Transform Infraredmentioning

confidence: 99%

Micro- and Macro-Attenuated Total Reflection Fourier Transform Infrared Spectroscopic Imaging

2010

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Fourier transform infrared (FT-IR) spectroscopic imaging has become a very powerful method in chemical analysis. In this review paper we describe a variety of opportunities for obtaining FT-IR images using the attenuated total reflection (ATR) approach and provide an overview of fundamental aspects, accessories, and applications in both micro- and macro-ATR imaging modes. The advantages and versatility of both ATR imaging modes are discussed and the spatial resolution of micro-ATR imaging is demonstrated. Micro-ATR imaging has opened up many new areas of study that were previously precluded by inadequate spatial resolution (polymer blends, pharmaceutical tablets, cross-sections of blood vessels or hair, surface of skin, single live cells, cancerous tissues). Recent applications of ATR imaging in polymer research, biomedical and forensic sciences, objects of cultural heritage, and other complex materials are outlined. The latest advances include obtaining spatially resolved chemical images from different depths within a sample, and surface-enhanced images for macro-ATR imaging have also been presented. Macro-ATR imaging is a valuable approach for high-throughput analysis of materials under controlled environments. Opportunities exist for chemical imaging of dynamic aqueous systems, such as dissolution, diffusion, microfluidics, or imaging of dynamic processes in live cells.

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Section: Micro-attenuated Total Reflection Fourier Transform Infraredmentioning

confidence: 99%

Micro- and Macro-Attenuated Total Reflection Fourier Transform Infrared Spectroscopic Imaging

2010

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“…Recently, IR imaging spectroscopy has attracted widespread interest in polymer science and technology and has frequently been used to investigate the phase separation, miscibility, and morphology of polymer blends. − With this technique, researchers can easily obtain information about the distributions of different components or different morphologies in blends. Additionally, it is possible to explore dynamic processes such as polymer dissolution and crystallization .…”

Section: Introductionmentioning

confidence: 99%

“…Additionally, it is possible to explore dynamic processes such as polymer dissolution and crystallization . For example, in previous studies, − FT-IR imaging spectroscopy has been applied to study the miscibility of PHB/PLLA blends as a function of the blend compositions. From these investigations, the concentration dependence of phase separation at room temperature was determined. , Also, Gupper and Kazarian examined solvent diffusion and solvent-induced crystallization in syndiotactic polystyrene using IR imaging spectroscopy.…”

Section: Introductionmentioning

confidence: 99%

Effects of Hydrogen Bond Intermolecular Interactions on the Crystal Spherulite of Poly(3-hydroxybutyrate) and Cellulose Acetate Butyrate Blends: Studied by FT-IR and FT-NIR Imaging Spectroscopy

et al. 2012

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The crystal melting behaviors of poly(3-hydroxybutyrate) (PHB) and cellulose acetate butyrate (CAB) blends were studied using infrared (IR) and near-infrared (NIR) imaging, which provided information about spherulite growth in dynamic blend systems. By analyzing the changes in the IR and NIR imaging spectra in the regions of the first and second overtones of the CO stretching vibrations of PHB and CAB, the evolution of heterogeneous spherulite during the time-resolved isothermal crystallization process was explored. Time-resolved IR and NIR imaging and polarized microscopic studies detected the PHB domains are able to separate from the PHB/CAB blends early in the process. Principal component analysis (PCA) was used to classify the distribution of the different morphologies of spherulite. The first principal component suggests that the discrimination of the imaging spectra relies largely upon the crystallinity, while the second principal component indicates the variations in the amorphous portion of PHB, the CAB contents, and the intermolecular hydrogen bonding of PHB and CAB. The PC1–PC2 scores of different parts of the spherulite suggest that the areas of low crystallinity in the blend spherulite contain both PHB and CAB.

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“…8,9 Nevertheless, vibrational spectroscopic imaging provides a powerful method for obtaining molecular information on the miscibility and morphology of polymer blends. 10,11 Thus, Raman microspectroscopy and FT-IR spectroscopic imaging have been used to investigate the dissolution process of polymers. 12,15 There are reports on the combination of FT-IR or Raman imaging for the characterization of heterogeneity in polymer blends 16,21 and on the application to explore dynamic processes such as crystallization 22,23 or the diffusion of solvents into a polymer film.…”

Section: Introductionmentioning

confidence: 99%

“…In a previous research, 11,19 FT-IR imaging spectroscopy was applied to study the miscibility of polymer blends of PHB and PLA as a function of the blend composition. From these investigations, the concentration dependence of phase separation at room temperature was determined.…”

Section: Introductionmentioning

confidence: 99%

Temperature-Dependent Fourier Transform Infrared Spectroscopy and Raman Mapping Spectroscopy of Phase-Separation in a Poly(3-hydroxybutyrate)–Poly(l-Lactic Acid) Blend

et al. 2013

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Variable-temperature Fourier transform infrared spectroscopy (FT-IR) and Raman spectroscopic mapping measurements were applied to study the phase separation of a poly(3-hydroxybutyrate) (PHB)-poly(L-lactic acid) (PLA) (50 : 50 wt.%) polymer-blend film as a function of temperature between 25 and 175 °C. Because of the better band separation compared with the fundamental absorptions, the first overtones of the ν(C=O) bands of PHB and PLA were used to evaluate the temperature-dependent FT-IR images as PLA-PHB and PHB-PLA band-ratio contour plots, respectively. From the visualization of the band-ratio FT-IR images, it could be derived that even beyond the melting point of PLA (145 °C), the lateral position and the geometry of the PHB-rich and PLA-rich phases were retained up to 165 °C. Furthermore, the FT-IR images derived during and after the melting of PHB (174 °C) provided an interesting insight into the homogenization process of the polymer melt. By exploiting its higher lateral resolution, valuable additional information became available from the Raman mapping measurements. Based on the Raman data, the scenario of phase-separated PHB-rich and PLA-rich domains of about 50 μm size, based on the FT-IR imaging measurements, had to be revised. Instead, the originally interpreted PHB-rich and PLA-rich domains are actually clusters of much smaller grains. Additionally, the Raman images measured in the same temperature interval revealed that the clusters of small PHB-rich grain structures aggregated as a function of temperature increase. These investigations prove that FT-IR and Raman imaging in combination with variable-temperature measurements can provide new (and so far unavailable) insights into structural phenomena of phase-separated polymer blends.

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FT‐IR and NIR Spectroscopic Imaging: Principles, Practical Aspects and Applications in Material and Pharmaceutical Sciences

Cited by 10 publications

References 69 publications

Micro- and Macro-Attenuated Total Reflection Fourier Transform Infrared Spectroscopic Imaging

Micro- and Macro-Attenuated Total Reflection Fourier Transform Infrared Spectroscopic Imaging

Effects of Hydrogen Bond Intermolecular Interactions on the Crystal Spherulite of Poly(3-hydroxybutyrate) and Cellulose Acetate Butyrate Blends: Studied by FT-IR and FT-NIR Imaging Spectroscopy

Temperature-Dependent Fourier Transform Infrared Spectroscopy and Raman Mapping Spectroscopy of Phase-Separation in a Poly(3-hydroxybutyrate)–Poly(l-Lactic Acid) Blend

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