Thermogravimetric analysis Infrared spectroscopy

Rao and co-workers [82] used an inverted emulsion process for the synthesis of the emeraldine salt of PAM using a novel oxidising agent, benzoyl peroxide. The polymerisation was carried out in a non-polar solvent in the presence of four different protonic acids as dopants and an emulsifier (sodium lauryl sulfate). The polymer salts were characterised spectroscopically by ultraviolet-visible, Fourier-transform infrared, Fourier-transform Raman and electron paramagnetic resonance spectroscopy. Thermogravimetric analysis, was used to determine the stability of the salts and the activation energy for the degradation. The conductivity of the salts was found to be in the order of 10 S/cm. 

The characterization includes infrared, ultraviolet-visible, electron spin resonance and x-ray diffraction spectroscopies, thermogravimetric analysis and differential scanning calorimetry. 

In this study, we extend the range of inorganic materials produced from polymeric precursors to include copper composites. Soluble complexes between poly(2-vinylpyridine) (P2VPy) and cupric chloride were prepared in a mixed solvent of 95% methanol 5% water. Pyrolysis of the isolated complexes results in the formation of carbonaceous composites of copper. The decomposition mechanism of the complexes was studied by optical, infrared, x-ray photoelectron and pyrolysis mass spectroscopy as well as thermogravimetric analysis and magnetic susceptibility measurements. 

First-order phase transitions can be detected by various thermoanalytical techniques, such as DSC, thermogravimetric analysis (TGA), and thermomechanical analysis (TMA) [31]. Phase transitions leading to visual changes can be detected by optical methods such as microscopy [3], Solid-solid transitions involving a change in the crystal structure can be detected by X-ray diffraction [32] or infrared spectroscopy [33], A combination of these techniques is usually employed to study the phase transitions in organic solids such as drugs. 

The thermal characterisation of elastomers has recently been reviewed by Sircar [28] from which it appears that DSC followed by TG/DTG are the most popular thermal analysis techniques for elastomer applications. The TG/differential thermal gravimetry (DTG) method remains the method of choice for compositional analysis of uncured and cured elastomer compounds. Sircar s comprehensive review [28] was based on single thermal methods (TG, DSC, differential thermal analysis (DTA), thermomechanical analysis (TMA), DMA) and excluded combined (TG-DSC, TG-DTA) and simultaneous (TG-fourier transform infrared (TG-FTIR), TG-mass spectroscopy (TG-MS)) techniques. In this chapter the emphasis is on those multiple and hyphenated thermogravimetric analysis techniques which have had an impact on the characterisation of elastomers. The review is based mainly on Chemical Abstracts records corresponding to the keywords elastomers, thermogravimetry, differential scanning calorimetry, differential thermal analysis, infrared and mass spectrometry over the period 1979-1999. Table 1.1 contains the references to the various combined techniques. 

Osmium tetroxide reacts with CsF or RbF in water forming M2[0s04F2] H20 (M = Cs, Rb) which were characterized by elemental analysis, X-ray powder diffraction, infrared spectroscopy and thermogravimetric analysis [353]. Based on vibrational spectroscopy, the 0s04F22 anion is considered to possess a m-difluoro arrangement. Osmium Lm EXAFS data have been obtained for Cs2[0s04F2] giving values for the 0s=0 and Os—F bond distances [354]. 

Comparison of several techniques (namely Fourier transform infrared spectroscopy (FTIR), simultaneous thermogravimetric analysis-differential scanning calorimetry (TGA-DSC) and ultrasonic spectroscopy) for assessing the residual physical and mechanical characteristics of polymer matrix composites (PMCs) exposed to excessive thermal loads showed the measured power spectra of ultrasonic energy to correlate with performance of graphite fibre epoxy matrix composites exposed to thermal degradation, and also that analyses with the three techniques all pointed to the same critical temperature at which thermally induced damage increased sharply [58],... 

Analytical techniques commonly used to check for solid-state characteristics include melting point (including hot-stage microscopy), solid-state infrared spectroscopy, x-ray powder diffraction, thermal analysis (e.g., differential scanning calorimetry, thermogravimetric analysis, and differential thermal analysis), Raman spectroscopy, scanning electron microscopy, and solid-state nuclear magnetic resonance (NMR). 

The catalysts were characterized by N2 adsorption-desorption isotherms, thermogravimetric analysis (TGA), temperature-programmed desorption of ammonia (NH3-TPD), X-ray diffraction (XRD), Raman spectroscopy, in-situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), and X-ray photoelectron spectroscopy (XPS). The procedures and experimental conditions have been detailed elsewhere [9]. 

Effect of thermostabilizers on the polymer properties was studied by different physicochemical methods. For example, in the work [260] method of DSS (differential spectroscopy) was used to define the effect of polyester-imide on thermo-physical properties of PETP. By this method it was found out that polyester-imide reduces PETP ability to crystallization. Methods of thermogravimetric analysis (TGA) and infrared spectroscopy in the nitrogen atmosphere were used in the work [261] to define thermal stability of the mixture of PETP and polyamide with the additive - modifier - polyethylene. It has been found that introduction of the additive decreases activation energy which positively tells on the ability of PETP to thermal destruction. 

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