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Abstract  

This paper reports the synthesis, characterisation and thermolysis studies of a series of azotetrazolate salts, viz., ammonium/guanidinium/triaminoguanidinium [azotetrazolate]. TG-DTA and DSC results of these compounds exhibited their thermal stability up to 180°C. DSC indicated the highest heat release (2804 J g-1) for guanidinium azotetrazolate salt during exothermic decomposition. FTIR of the decomposition products of azotetrazolate salts showed bands at 3264 and 2358 cm-1 which may be attributed to gaseous species such as NH3 and HCN or NH2CN. The sensitivity data suggests low vulnerability of ammonium and guanidinium salts. In cyclic voltammetric studies all the salts showed similar response in reduction reactions. Triamino guanidinium azotetrazolate (TAGAZ) was incorporated into solid propellant formulations in order to establish the compatibility of this class of compounds. DSC results revealed that it does not have adverse effect on thermal stability of double base matrix. The burning rate data obtained indicated that TAGAZ acts as an efficient energetic additive in composite modified double base (CMDB) propellant formulations in high-pressure region.

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Abstract  

Combustion profiles of coal-limestone-paper blends were studied using thermogravimetric/ Fourier transform infrared spectroscopy (TG/FTIR). The role of limestone in promoting the initial combustion of coal-paper blends and its ability to absorb sulphur oxides were examined.

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Abstract  

Thermal analysis combined with evolved gas analysis has been used for some time. Thermogravimetry (TG) coupled with Fourier transform infrared (FTIR) spectroscopy(TG/FTIR), Thermogravimetry (TG) coupled with mass spectrometry (TG/MS), and Thermogravimetry (TG) coupled with GC/MS offers structural identification of compounds evolving during thermal processes. These evolved gas analysis (EGA) techniques allow to evaluate the chemical pathway of the degradation reaction by determining the decomposition products. In this paper the TG/FTIR, TG/MS, and Pyrolysis/GC-MS systems will be described and their applications in the study of several materials will be discussed, including the analysis of the degradation mechanisms of organically modified clays, polymers, and coal blends.

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Abstract  

Thermal decomposition of compounds consisting of tetrahalogenocuprate(II), [CuBrnCl4−n]2− (n=0–4) anions and a tetraethylammonium cation has been studied using TG-FTIR, TG-MS, DTA and DTG techniques. The measurements were carried out in an argon and air atmospheres over the temperature range 293-1073 K. The products of the thermal decomposition were identified by IR and Far Infrared (FIR) spectroscopy as well as X-ray powder diffractometry.

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Journal of Thermal Analysis and Calorimetry
Authors:
V. Sydorchuk
,
W. Janusz
,
S. Khalameida
,
E. Skwarek
,
J. Skubiszewska-Zięba
,
R. Leboda
, and
V. Zazhigalov

Abstract

Deposited zirconium phosphate samples on the base of silica and titania have been prepared using the sol–gel and mechanochemical methods. Porous structure, phase composition, and electrokinetic parameters have been studied by means of nitrogen adsorption–desorption, XRD, DTA-TG, FTIR, electrophoresis, and potentiometric titration. The compositions possess varied parameters of porous structure, structure of deposited phase, and electrokinetic properties depending on support nature and synthesis conditions.

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Abstract  

Embedding of barium titanate into porous oxide matrices via sol–gel synthesis and introduction in structured slurry based on fumed oxides has been carried out. Prepared compositions have been studied using XRD, DTA-TG, FTIR, TEM, and adsorption of nitrogen. It has been established that simultaneous formation both barium titanate crystal structure and porous structure of matrices occurs. Crystallites of barium titanate, which arise in pores, possess lesser size in comparison with that for bulk BaTiO3.

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Abstract  

Thermal analysis is a useful tool for investigating the properties of polymer/clay nanocomposites and mechanisms of improvement of thermal properties. This review work presents examples of applications of differential scanning calorimetry (DSC), modulated temperature differential scanning calorimetry (MT-DSC), dynamic mechanical thermal analysis (DMA), thermal mechanical analysis (TMA), thermogravimeric analysis (TG) and thermoanalytical methods i.e. TG coupled with Fourier transformation infrared spectroscopy (TG-FTIR) and mass spectroscopy (TG-MS) in characterization of nanocomposite materials. Complex behavior of different polymeric matrices upon modification with montmorillonite is briefly discussed.

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Journal of Thermal Analysis and Calorimetry
Authors:
Yu. Trach
,
V. Sydorchuk
,
O. Makota
,
S. Khalameida
,
R. Leboda
,
J. Skubiszewska-Zięba
, and
V. Zazhigalov

Abstract

Deposited catalysts composition H3PMo12O40/SiO2 and Ag/H3PMo12O40/SiO2 have been synthesized on the basis of fumed silica, including milling technique. Physical–chemical characteristics of prepared catalysts have been studied by means of XRD, DTA-TG, FTIR, UV–Vis spectroscopy, and adsorption of nitrogen. Catalysts possess meso- or meso-macroporous structure and contain deposited Keggin heteropolycompounds. Deposition of heteropolycompounds on support with high specific surface area results in increase of selectivity to epoxide in epoxidation reactions. The use of milling during catalyst synthesis leads to further growth of selectivity of epoxides formation.

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Journal of Thermal Analysis and Calorimetry
Authors:
Thangamani Rajkumar
,
Chinnaswamy Vijayakumar
,
Palanichamy Sivasamy
,
Bojja Sreedhar
, and
Charles Wilkie

Abstract  

Imparting thermal stability to polymethyl methacrylate (PMMA) without affecting its optical clarity is attempted by incorporating HET acid based oligoesters. Pure PMMA and PMMA containing five and 20 wt% of four different oligoesters are separately prepared using bulk polymerization. The thermal properties of the materials studied using DSC, TG, TG–FTIR and Pyr–GC–MS are presented. The main volatile degradation products identified are CO, HCl, CO2, H2O, hexachlorocyclopentadiene, hexachloroendomethylene tetrahydrophthalic acid/anhydride and methyl methacrylate. A detailed mechanism for the influence of the degradation products of HET acid based oligoesters on the thermal degradation of PMMA is also presented.

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Abstract  

When ethylene-vinyl acetate copolymer, EVA, is heated, a two-stage thermal degradation occurs following its melting. The vinyl acetate content of the copolymer was determined to be 43.8% by using TA 2950 and TA 2050 thermogravimetric instruments. TG/FTIR was used to detect the evolved gas. Acetic acid and trans-1-R-4-R'-cyclohexane were the main products evolved from EVA in the first and second stage, respectively. The apparent activation energies were determined for both stages by differential methods.

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