Thermokinetic parameter evaluation by DSC and TAM III along with accountability of mass loss by TG from the thermal decomposition analyses of benzoyl peroxide

2015 ◽  
Vol 122 (3) ◽  
pp. 1143-1150 ◽  
Author(s):  
Ming-Hsun Lee ◽  
Jiann-Rong Chen ◽  
Mitali Das ◽  
Tung-Feng Hsieh ◽  
Chi-Min Shu
Keyword(s):  
Thermal Decomposition ◽  
Mass Loss ◽  
Benzoyl Peroxide ◽  
Thermokinetic Parameter ◽  
Parameter Evaluation

scholarly journals Thermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III)—a single-source precursor for antimony sulfide thin films

2021 ◽  
Author(s):  
Jako S. Eensalu ◽  
Kaia Tõnsuaadu ◽  
Jasper Adamson ◽  
Ilona Oja Acik ◽  
Malle Krunks
Keyword(s):  
Thin Films ◽  
Thermal Decomposition ◽  
Mass Loss ◽  
Solid Phase ◽  
Evolved Gas Analysis ◽  
Gas Analysis ◽  
Thermal Decomposition Mechanism ◽  
Product Analysis ◽  
Gaseous Species ◽  
Single Source Precursor

AbstractThermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III) (1), a precursor for Sb2S3 thin films synthesized from an acidified aqueous solution of SbCl3 and KS2COCH2CH3, was monitored by simultaneous thermogravimetry, differential thermal analysis and evolved gas analysis via mass spectroscopy (TG/DTA-EGA-MS) measurements in dynamic Ar, and synthetic air atmospheres. 1 was identified by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR) measurements, and quantified by NMR and elemental analysis. Solid intermediates and final decomposition products of 1 prepared in both atmospheres were determined by X-ray diffraction (XRD), Raman spectroscopy, and FTIR. 1 is a complex compound, where Sb is coordinated by three ethyldithiocarbonate ligands via the S atoms. The thermal degradation of 1 in Ar consists of three mass loss steps, and four mass loss steps in synthetic air. The total mass losses are 100% at 800 °C in Ar, and 66.8% at 600 °C in synthetic air, where the final product is Sb2O4. 1 melts at 85 °C, and decomposes at 90–170 °C into mainly Sb2S3, as confirmed by Raman, and an impurity phase consisting mostly of CSO 2 2− ligands. The solid-phase mineralizes fully at ≈240 °C, which permits Sb2S3 to crystallize at around 250 °C in both atmospheres. The gaseous species evolved include CS2, C2H5OH, CO, CO2, COS, H2O, SO2, and minor quantities of C2H5SH, (C2H5)2S, (C2H5)2O, and (S2COCH2CH3)2. The thermal decomposition mechanism of 1 is described with chemical reactions based on EGA-MS and solid intermediate decomposition product analysis.

scholarly journals Study of thermal behavior of phytic acid

2013 ◽  
Vol 49 (2) ◽  
pp. 275-283 ◽  
Author(s):  
André Luis Máximo Daneluti ◽  
Jivaldo do Rosário Matos
Keyword(s):  
Thermal Decomposition ◽  
Thermal Behavior ◽  
Mass Loss ◽  
Kinetic Study ◽  
Phytic Acid ◽  
Absorption Spectroscopy ◽  
Elemental Analysis ◽  
Reaction Order ◽  
Dehydration Process ◽  
Thermogravimetric Method

Phytic acid is a natural compound widely used as depigmenting agent in galenic cosmetic emulsions. However, we have observed experimentally that phytic acid, when heated to 150 ºC for around one hour, shows evidence of thermal decomposition. Few studies investigating this substance alone with regard to its stability are available in the literature. This fact prompted the present study to characterize this species and its thermal behavior using thermal analysis (TG/DTG and DSC) and to associate the results of these techniques with those obtained by elemental analysis (EA) and absorption spectroscopy in the infrared region. The TG/DTG and DSC curves allowed evaluation of the thermal behavior of the sample of phytic acid and enabled use of the non-isothermal thermogravimetric method to study the kinetics of the three main mass-loss events: dehydration I, dehydration II and thermal decomposition. The combination of infrared absorption spectroscopy and elemental analysis techniques allowed evaluation of the intermediate products of the thermal decomposition of phytic acid. The infrared spectra of samples taken during the heating process revealed a reduction in the intensity of the absorption band related to O-H stretching as a result of the dehydration process. Furthermore, elemental analysis results showed an increase in the carbon content and a decrease in the hydrogen content at temperatures of 95, 150, 263 and 380 °C. Visually, darkening of the material was observed at 150 °C, indicating that the thermal decomposition of the material started at this temperature. At a temperature of 380 °C, thermal decomposition progressed, leading to a decrease in carbon and hydrogen. The results of thermogravimetry coupled with those of elemental analysis allow us to conclude that there was agreement between the percentages of phytic acid found in aqueous solution. The kinetic study by the non-isothermal thermogravimetric method showed that the dehydration process occurred in two stages. Dehydration step I promoted a process of vaporization of water (reaction order of zero), whereas dehydration step II showed an order of reaction equal to five. This change in reaction order was attributed to loss of chemically bonded water molecules of phytic acid or to the presence of volatile substances. Finally, the thermal decomposition step revealed an order of reaction equal to one. It was not possible to perform the kinetic study for other stages of mass loss.

scholarly journals Flammability and Thermal Kinetic Analysis of UiO-66-Based PMMA Polymer Composites

Polymers ◽  
2021 ◽  
Vol 13 (23) ◽  
pp. 4113
Author(s):  
Ruiqing Shen ◽  
Tian-Hao Yan ◽  
Rong Ma ◽  
Elizabeth Joseph ◽  
Yufeng Quan ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Mass Loss ◽  
Polymer Composites ◽  
Flame Retardants ◽  
Loss Rate ◽  
Mass Loss Rate ◽  
Protective Layer ◽  
Average Mass ◽  
Microscale Combustion Calorimeter ◽  
Combustion Calorimeter

Metal–organic frameworks (MOFs) are emerging as novel flame retardants for polymers, which, typically, can improve their thermal stability and flame retardancy. However, there is a lack of specific studies on the thermal decomposition kinetics of MOF-based polymer composites, although it is known that they are important for the modeling of flaming ignition, burning, and flame spread over them. The thermal decomposition mechanisms of poly (methyl methacrylate) (PMMA) have been well investigated, which makes PMMA an ideal polymer to evaluate how fillers affect its decomposition process and kinetics. Thus, in this study, UiO-66, a common type of MOF, was embedded into PMMA to form a composite. Based on the results from the microscale combustion calorimeter, the values of the apparent activation energy of PMMA/UiO-66 composites were calculated and compared against those of neat PMMA. Furthermore, under cone calorimeter tests, UiO-66, at only 1.5 wt%, can reduce the maximum burning intensity and average mass loss rate of PMMA by 14.3% and 12.4%, respectively. By combining UiO-66 and SiO2 to form a composite, it can contribute to forming a more compact protective layer, which shows a synergistic effect on reducing the maximum burning intensity and average mass loss rate of PMMA by 22.0% and 14.7%, respectively.

Measurement of Thermal Decomposition Temperature and Rate of Sodium Hydride

2020 ◽  
Author(s):  
Munemichi Kawaguchi
Keyword(s):  
Thermal Decomposition ◽  
Mass Loss ◽  
Heating Temperature ◽  
Fission Products ◽  
Sodium Hydride ◽  
Decomposition Temperature ◽  
Cold Trap ◽  
Thermal Decomposition Temperature ◽  
Heating Rates ◽  
Fundamental Research

Abstract In decommissioning sodium-cooled fast reactors, the operators can be exposed to radiation during dismantling of cold trap equipment (C/T). The C/T is higher dose equipment because the C/T trapped tritium of fission products during the operation to purify the sodium coolant. In this study, thermal decomposition temperature and rate of sodium hydride (NaH) were measured as a fundamental research for development of “thermolysis” process prior to the dismantling. We measured the thermal decomposition temperature and rate using NaH powder (95.3%, Sigma-Aldrich) in alumina pan with ThermoGravimetry-Differential Thermal Analysis (TG-DTA) instrument (STA2500 Regulus, NETZSCH Japan). The heating rates of TG-DTA were set to β = 2.0, 5.0, 10.0 and 20.0 K/min. The DTA showed endothermic reaction and the TG showed two-steps mass-loss over 580K. This first-step mass-loss was consistent with change of chemical composition of the NaH with heating (NaH → Na+1/2H2). The thermal decomposition temperature and rate were obtained from the onset temperature of the mass-loss and the simplified Kissinger plots, respectively. Furthermore, we set to the thermal decomposition temperature of around 590K, and the mass-loss rates were measured. As a result, over 590K, the thermal decomposition occurred actively, and showed good agreement with the estimation curves obtained by the simplified Kissinger plots. The thermal decomposition rate strongly depended on the heating temperature.

Mechanism of reactions initiated by thermal decomposition of benzoyl peroxide in polyamide

1982 ◽  
Vol 24 (12) ◽  
pp. 2991-3000 ◽  
Author(s):  
G.G. Makarov ◽  
Yu.A. Mikheyev ◽  
G.B. Pariiskii ◽  
L.M. Postnikov ◽  
D.A. Toptygin
Keyword(s):  
Thermal Decomposition ◽  
Benzoyl Peroxide

FREE-RADICAL REACTIONS WITH AROMATIC ETHERS: PART I. BENZOYL PEROXIDE WITH ANISOLE

1962 ◽  
Vol 40 (7) ◽  
pp. 1461-1470 ◽  
Author(s):  
Brian M. Lynch ◽  
Ralph B. Moore
Keyword(s):  
Thermal Decomposition ◽  
Free Radical ◽  
Benzoyl Peroxide ◽  
Radical Reactions ◽  
Free Radical Reactions

A re-examination of the products of thermal decomposition of benzoyl peroxide in anisole has resolved anomalous findings by previous workers. The expected phenylation of the substrate is accompanied by appreciable benzoyloxylation, and the distribution of isomers in the phenylation and benzoyloxylation products has been examined; the theoretical implications of the results are discussed.

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