Instrumentation thermal microscopy

Newly born, the scanning thermal microscopy derived from atomic force microscopy brings a revolution in the instrumentation for measuring thermophysical and thermomechanical properties of the matter, and the TA instrument was awarded at Pittsburg 1998. The instrument has been applied for the characterization of Ibuprofen compacts as model substance. ... 

The introduction and development of Micro-Thermal Analysis are described and discussed by Duncan Price in Chapter 3. The atomic force microscope (AFM) forms the basis of both scanning thermal microscopy (SThM) and instruments for performing localised thermal analysis. The principles and operation of these techniques, which exploit the abilities of a thermal probe to act both as a very small heater and as a thermometer, in the surface characterisation of materials are described in detail. The... 

Various sophisticated instrumental methods have been developed to characterize polymer blends and compatibility, including thermal, microscopy, spectroscopy and other processing techniques. Recently, ultrasound has also been applied extensively to the study of polymer blend properties in both solutions and solids. The ultrasonic velocity and attenuation by the interaction of the propagating wave were used to investigate the various physical properties of the polymer blends, including density, compatibility, molecular orientation, and phase inversion. 

A wide variety of instrumental techniques, including X-ray diffraction, thermal analysis, electron microscopy, MAS-NMR and infrared spectroscopy, have been employed at different levels of complexity to investigate the effects of mechanochemical treatment on kaolin. Unfortunately, vibrational spectroscopy has only been used at a superficial level in the study of milled kaolin despite the considerable contribution that it has made to the understanding of the structure and reactivity of kaolin itself. 

The solid fraction has been recovered by filtration, washed with deionized water up to pH 9 and dried at 70 C in air. The products have been characterized by powder X-ray diffraction, scanning electron microscopy (Cambridge SiOO instrument), atomic absorption spectroscopy and nitrogen adsorption. Characterization by and ai MAS-NMR spectroscopy and thermal gravimetry have been already reported (7). 

The optimal calcination method for zeolite beta was established by thermogravimetric analysis using a PL-Thermal Sciences STA 1500 apparatus. Chemical compositions of the zeolites were determined by atomic absorption spectroscopy on a Varian AAIO spectrometer after dissolution of the samples in hydrofluoric acid. The structure was confirmed by x-ray diffraction on a Siemens D-5000 diffractometer and with infrared spectroscopy on a Mattson Instruments Galaxy 2000 spectrometer. Total surface area, micropore area and micropore volume of the samples were determined by argon adsorption on a Micromeritics ASAP 200M volumetric analyzer using standard techniques. Crystal diameters were determined by scanning electron microscopy. 

For example, large compounds such as the can-nabinoids are not particularly thermally labile and benefit for derivatization, however, this has implications in drug profiling as derivatization results in altering the chemical structure. LC analysis of can-nabinoids will effect their identification but difficulties in resolution may hamper quantification and profiling. In practice many laboratories now identify cannabis on the basis of microscopy rather than instrumental techniques. 

Other uses of an IR microscope in forensic analysis include the examination of fibers, drugs, and traces of explosives. For example, oxidation of hair can occur chemically or by sunlight oxidation of cystine to cysteic acid can be seen in hair fibers by FTIR microscopy (Robotham and Izzia). Excellent examples in full color of FTIR imaging microscopy can be found on the websites of companies like PerkinElmer and Thermo Fisher Scientific. Our limitations in use of gray scale make many of the examples unsuited for reproduction in the text. A novel IR microscope combined with atomic force microscopy, the nanoIR platform from Anasys Instruments (www.anasysinstruments.com), permits nanoscale IR spectroscopy, AFM topography, nanoscale thermal analysis, and mechanical testing. 

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