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Hubík Pavel - Thermal Physics and Thermal Analysis: From Macro to Micro, Highlighting Thermodynamics, Kinetics and Nanomaterials

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Hubík Pavel Thermal Physics and Thermal Analysis: From Macro to Micro, Highlighting Thermodynamics, Kinetics and Nanomaterials
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Thermal Physics and Thermal Analysis: From Macro to Micro, Highlighting Thermodynamics, Kinetics and Nanomaterials: summary, description and annotation

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From the Contents: Calorimetry on time scales from days to microseconds -- The use of digital image processing for local thermal analysis and other techniques -- Glass behavior at nanostate, glass transition and fictive temperatures -- Quantum aspects of nanomaterials characterization -- Kinetic phase diagrams as a consequence of radical changing temperature or particle size -- Material properties and thermal analysis of non-stoichiometric solids -- Ehrenfest equations for calorimetry and dilatometry.;Features twenty-five chapter contributions from an international array of distinguished academics based in Asia, Eastern and Western Europe, Russia, and the USA. This multi-author contributed volume provides an up-to-date and authoritative overview of cutting-edge themes involving the thermal analysis, applied solid-state physics, micro- and nano-crystallinity of selected solids and their macro- and microscopic thermal properties. Distinctive chapters featured in the book include, among others, calorimetry time scales from days to microseconds, glass transition phenomena, kinetics of non-isothermal processes, thermal inertia and temperature gradients, thermodynamics of nanomaterials, self-organization, significance of temperature and entropy. Advanced undergraduates, postgraduates and researchers working in the field of thermal analysis, thermophysical measurements and calorimetry will find this contributed volume invaluable. This is the third volume of the triptych volumes on thermal behaviour of materials; the previous two receiving thousand of downloads guaranteeing their worldwide impact.

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Hubík Pavel - Thermal Physics and Thermal Analysis: From Macro to Micro, Highlighting Thermodynamics, Kinetics and Nanomaterials
Thermal Physics and Thermal Analysis: From Macro to Micro, Highlighting Thermodynamics, Kinetics and Nanomaterials
Hubík Pavel
Thermal Physics and Thermal Analysis: From Macro to Micro, Highlighting Thermodynamics, Kinetics and Nanomaterials

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Springer International Publishing Switzerland 2017
Jaroslav estk , Pavel Hubk and Ji J. Mare (eds.) Thermal Physics and Thermal Analysis Hot Topics in Thermal Analysis and Calorimetry 10.1007/978-3-319-45899-1_1
1. Local Thermal Analysis by Structural Characterization (TASC)
Mike Reading 1 and Muqdad Alhijjaj 2
(1)
Department of Chemical Sciences, University of Huddersfield, Queensgate, Huddersfield, NR4 7TJ, UK
(2)
School of Pharmacy, University of East Anglia, Norwich, Norfolk, NR4 7TJ, UK
Mike Reading (Corresponding author)
Email:
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Sheng Qi
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Abstract
Thermal analysis by structural characterization (TASC) is a new thermal technique that is based on image analysis combined with hot-stage microscopy (HSM, also called thermomicroscopy). The image analysis algorithm is sensitive to any change in structure as seen by digital optical microscopy. A key feature of the algorithm is that it accounts for any sample movement. Due to thermal expansion of the sample or the sample chamber, there is, at high magnification, usually some sample displacement and this needs to be removed, so the measurement is purely one of structural change. HSM has a variety of uses but struggles with opaque samples (such as filled samples) and cannot routinely detect glass transitions. TASC, when used with an imposed structure such as an indentation, can routinely measure glass transition temperatures because, when the sample softens, the indentation disappears. This is true even when analyzing opaque samples. TASC can also be used to measure melting temperatures, transitions in small (microgram) samples, dissolution behavior, and heterogeneity.
1.1 The Development of Methods for Local Thermal Analysis
The first approach to local thermal analysis (LTA) was proposed by Hammiche et al. [], i.e., an order of magnitude worse than conventional thermal techniques . Furthermore, conventional temperature calibrants, such as indium, cannot be used because their high thermal conductivity gives rise to temperature gradients that they are so far removed from those experienced with organic samples that calibration curves obtained with these materials cannot be relied on when analyzing polymers, pharmaceuticals, etc. To overcome this difficulty, polymer calibrants are used and these are not primary standards.
A solution to the problems encountered by micro-/nano-TA has recently been proposed in the form of thermal analysis by structural characterization or TASC [.
Fig 11 An illustration of a TASC experiment with a DSC measurement for - photo 1
Fig. 1.1
An illustration of a TASC experiment with a DSC measurement for comparison. The image a size 1 mm 1 mm is an indentation in a filled polystyrene sample prior to heating. Image b is the same area after heating to 160 C. The dashed line is the TASC curve and the solid line is a DSC experiment for the same sample (normalized to final value)
The TASC value is calculated by subtracting a selected area within the first image from the corresponding areas in each subsequent image; thus, any change in appearance will result in a change in the TASC curve. The algorithm is able to compensate for any movement by the sample; this is essential because heating a sample under high magnification is almost certain to result in shifts in its position due to thermal expansion by the sample and the sample chamber. These are not of interest so eliminating them is a requirement for the analysis to work. Clearly, the absolute values of the TASC calculations are dependent on the size of the area that is chosen so TASC curves are normalized to the highest value. Details of the algorithm can be found in []. The areas of application can be categorized as follows:
  • A general tool of measuring transition temperatures,
  • Local thermal analysis including surface analysis,
  • Measuring heterogeneity
These are considered below.
1.2 Measuring Transition Temperatures and Local Thermal Analysis
Figure .
Fig 12 Above left is a micrograph of sugar crystals right are the TASC - photo 2
Fig. 1.2
Above left is a micrograph of sugar crystals; right are the TASC results for the crystals indicated by the colored circles . There is excellent agreement for the onset of the principle event. For the crystal highlighted by the blue circle, there is a suggestion of a preliminary process (further work would be needed to confirm this). This is illustrative of how TASC provides discrete information rather than the global data obtained by conventional methods
Particles made of amorphous materials also change shape upon being heated above their glass transition . This type of experiment complements traditional thermal measurements. Analyzing a mixture of particles of the order of tens of microns using, for example, DSC can provide information on the constituents and their relative amounts. However, it is only by making measurements on individual components that it can be established whether these material are within each particle or each particle is a different material. The components might only be a few micrograms and could not, therefore, be analyzed by conventional means. TASC provides an easy and convenient means of analyzing a large number of such small samples in a single experiment.
Another aspect of this type of localized measurement is that, in most cases, it is a form of surface analysis. Figure is a measurement made on the surface of a foodstuff coated in carnauba wax.
Fig 13 This is an example of a TASC measurement on the surface of a piece of - photo 3
Fig. 1.3
This is an example of a TASC measurement on the surface of a piece of candy. The surface is coated in carnauba wax, and its melting temperature can be determined as being 80 C
It might be argued that this measurement could be made using thermomechanical analysis in penetration mode, but it would usually not be possible to be sure whether the transition arose from the surface or somewhere deeper.
For complex systems, TASC has demonstrated the ability to detect hidden transitions that are often difficult to measure by conventional thermal methods such as DSC. Two examples of such cases are detection of the dissolution of crystalline material into matrices upon heating and the development of metastable polymorphs with rapid kinetic transformation during the thermal ramp. Alhijjaj and coworkers reported the use of TASC to study a series of complex pharmaceutical formulations containing three semicrystalline excipients (poly(ethylene glycol), poly(ethylene oxide), and d --tocopheryl polyethylene glycol succinate) with low melting points (3770 C) and a model drug (felodipine) with a melting point of 145 C [d, a clear plateau can be obtained implying the complete dissolution and melting of crystalline drug in the molten excipient matrices. This can be used as an evidence of the presence of crystalline drug in the original formulation which could not be detected by DSC.
Fig 14 An illustration of the detection of the thermal dissolution of - photo 4
Fig. 1.4
An illustration of the detection of the thermal dissolution of crystalline drug (with melting point at 145 C) in complex polymeric matrices by TASC a DSC results of the formulations show no indication of melting of the crystalline drug due to thermal dissolution; b TASC results of placebo formulations demonstrate the clear detection of thermal melting of excipients and a plateau region indicating the complete melting of all materials in the formulations; c TASC results of formulations containing crystalline drug show onset of thermal dissolution of the crystalline drug which is not detectable by DSC, but without the plateau due to the incomplete melting/thermal dissolution of the drug at 90 C; d The clear detection of the plateau indicating the complete melting of drug at 150 C which is above the melting point of the crystalline drug. (Reproduced from Ref. [] with permission)
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