Differential thermogravimetry analysis

Thermal analysis iavolves techniques ia which a physical property of a material is measured agaiast temperature at the same time the material is exposed to a coatroUed temperature program. A wide range of thermal analysis techniques have been developed siace the commercial development of automated thermal equipment as Hsted ia Table 1. Of these the best known and most often used for polymers are thermogravimetry (tg), differential thermal analysis (dta), differential scanning calorimetry (dsc), and dynamic mechanical analysis (dma). 

The procedures of measuring changes in some physical or mechanical property as a sample is heated, or alternatively as it is held at constant temperature, constitute the family of thermoanalytical methods of characterisation. A partial list of these procedures is differential thermal analysis, differential scanning calorimetry, dilatometry, thermogravimetry. A detailed overview of these and several related techniques is by Gallagher (1992). 

Thermal analysis helps in measuring the various physical properties of the polymers. In this technique, a polymer sample is subjected to a controlled temperature program in a specific atmosphere and properties are measured as a function of temperature. The controlled temperature program may involve either isothermal or linear rise or fall of temperature. The most common thermoanalytical techniques are (1) differential scanning analysis (DSC), (2) thermomechanical analysis (TMA), and (3) thermogravimetry (TG). 

The techniques referred to above (Sects. 1—3) may be operated for a sample heated in a constant temperature environment or under conditions of programmed temperature change. Very similar equipment can often be used differences normally reside in the temperature control of the reactant cell. Non-isothermal measurements of mass loss are termed thermogravimetry (TG), absorption or evolution of heat is differential scanning calorimetry (DSC), and measurement of the temperature difference between the sample and an inert reference substance is termed differential thermal analysis (DTA). These techniques can be used singly [33,76,174] or in combination and may include provision for EGA. Applications of non-isothermal measurements have ranged from the rapid qualitative estimation of reaction temperature to the quantitative determination of kinetic parameters [175—177]. The evaluation of kinetic parameters from non-isothermal data is dealt with in detail in Chap. 3.6. 

Recently we investigated ferromagnetic properties of CoPt bimetallic nanoparticles [232,233]. CoPt3 nanoparticles can be prepared by a two-step reduction using NaBH4 as a reductant. The bimetallic nanoparticles were characterized by thermogravimetry (TG) and differential thermal analysis (DTA), FT-IR, TEM) and XRD. Structural and spectroscopic studies showed that the bimetallic nanoparticles adopt an fee crystalline structure with an average particle size of 2.6 nm. SQUID studies revealed... 

Shurygina EA, Larina NK, Chubarova MA, Kononova MM. Differential thermal analysis (DTA) and thermogravimetry (TG) of soil humus substances. Geoderma 1971 6 169-177. 

Leinweber P, Schulten HR. Differential thermal analysis, thermogravimetry and in-source pyrolysis-mass spectrometry studies on the formation of soil organic matter. Thermochim. Acta 1992 200 151-167. 

Thermal analytical techniques such as thermogravimetry (TG), differential thermal analysis (DTA) and differential scanning calorimetry (DSC) have all been successfully employed in studying the pyrotechnic reactions of energetic materials such as black powder, as well as of binary mixtures of the constituents. 

TGA/DTA combined thermogravimetry / differential thermal analysis WDX wavelength-dispersive X-ray diffraction... 

Differential thermal analysis (DTA) was performed in air with an OD-102 Derivatograph (MOM, Hungary) using 100 mg samples at a heating rate of 10°C/min. Differential thermogravimetry (DTG) and thermogravimetry... 

The research papers which originated in the last couple of years in different countries in this field indicate that ED and Er are not generally reported and there is an emphasis on the study of comprehensive thermal behavior of explosives as a function of temperature or time by means of different thermal analytical techniques. Most commonly used methods of thermal analysis are differential thermal analysis (DTA), thermogravimetric analysis (TGA) or thermogravimetry and differential scanning calorimetry (DSC). 

C. Campbell, "Differential Thermal Analysis and Thermogravimetry Applied to Potassium Perchlorate-Aluminum-Barium Nitrate Mixtures , AnalChem 29, 306-10(1957) (See also PATR 2373 (Feb 1957) 4) W.J. Smothers 8r Y. 

Figure 9. Thermal analysis of levoglucosenone samples (a) neat, (b) +5% zinc chloride, (c) +5% diammonium phosphate, and (d) +5% diphenyl phosphate (D.t.a., differential thermal analysis T.g., thermo gravimetry D.t.g., derivative of thermogravimetry)...

In addition to routinely used methods, such as elemental analysis, IR and UV-vis-NIR spectra, thermogravimetry-differential thermal analysis (TG-DTA), single-crystal X-ray diffraction, and gas adsorption, there are some important characterization methods for coordination polymers. 

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. 

Thermogravimetry - Differential Thermal Analysis - Mass Spectrometry... 

All methods in which the sample to be analyzed is gradually heated and its calorimetric behavior studied. The method includes thermogravimetry (TG) and differential thermal analysis (DTA). 

The synthesis of the complex is followed by the most important step of characterization of the complex. The composition and the structural features of both the ligand and complex have to be established before embarking on further studies. There exist many methods by which the composition and structural features of the complexes are studied. Some of the methods are (i) elemental analysis, (ii) X-ray crystallography, (iii) UV-Vis absorption spectra, (iv) infrared spectroscopy, (v) Raman spectroscopy, (vi) thermal methods of analysis such as thermogravimetry, differential thermal analysis, (vii) nuclear magnetic resonance spectroscopy (proton, multinuclear), (viii) electrospray mass spectrometry. Depending upon the complexity of the system, some or all the methods are used in the studies of complexes. 

Thermal decomposition kinetics of complexes have been studied by thermogravimetry and differential thermal analysis in order to understand the thermal stability and the mechanism... 

The addition of various salts to potato starch on its compression up to 1.2 X 109 Pa had only a small effect on the thermal properties of starch, as measured by thermogravimetry/differential thermogravimetry/differential thermal analysis (TG/DTG/DTA). Only FeCl3, CoCl2, and I2 caused significant effects.62... 

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