Thermogravimetry, thermal analysis

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. 

Mara. Kamei and Osada [109 described a detailed study of the thermal decomposition of TNT. They examined the decomposition by differential thermal analysis, thermogravimetry, infra-red spectroscopy. HSR and mass spectrometry. One of their most important findings was that TNT produced free radicals already in the vicinity of the melting point, that is SO C. The substances which promote the decomposition of TNT are free radicals which are stable at room temperature. They are insoluble in benzene or chloroform and are partly oxidized polymeric substances. 

The differential calorimetric curves (DSC) of the various crystalline forms of triamterene grown from organic solutions containing water and from absolute organic solutions, and the DSC curves of triamterene crystals dried under reduced pressure have been described. The differential thermal analysis-thermogravimetry analysis (DTA-TG) thermograms are also given. 

Paulik F, Paulik J, Erdey L (1958) The Derivatograph. I. An Automatic Recording Apparatus for Simultaneously Conducting Differential Thermal Analysis, Thermogravimetry, and Derivative Thermogravimetry. Z anal Chem 160 241-252. For standardization, quasi-isothermal and isobaric analyses and some example research with the Derivatograph see also (1966) Anal Chim Acta 34 419-426 Paulik F, Paulik J (1973) J Thermal Anal 5 253-270 (1975) 8 557-576. 

The thermal transition of the 5 form was also studied by de Candia et al. [77] by using different techniques such as thermal analysis, thermogravimetry X-ray diffraction, and infrared spectroscopy. Experimental evidence showed that the solvent included in the crystal lattice was partially released on heating the sample within the range of stability of the 5 form. The solvent release depends on the time and temperature of annealing. Furthermore, the transition 5 to y occurs through an intermediate form characterized by conformational order, without crystalline order. This mesomorphic form was found to be impermeable to the vapor of dichloromethane at low activity, and it was possible to calculate its fraction. 

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. 

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. 

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