scholarly journals Solid-Phase Thermal Decomposition of 2,4-Dinitroimidazole (2,4-DNI)

1995 ◽  
Vol 418 ◽  
Author(s):  
Leanna Minier ◽  
Richard Behrens ◽  
Suryanarayana Bulusu
Keyword(s):  
Thermal Decomposition ◽  
Induction Period ◽  
Solid Phase ◽  
Low Molecular Weight ◽  
Ftir Analysis ◽  
Pyrolysis Products ◽  
Gaseous Products ◽  
Elemental Formula ◽  
Gas Formation ◽  
Primary Products

AbstractThe solid-phase thermal decomposition of the insensitive energetic aromatic heterocycle 2,4- dinitroimidazole (2,4-DNI: mp 265–274°C) is studied utilizing simultaneous thermogravimetric modulated beam mass spectrometry (STMBMS) between 200° and 247°C. The pyrolysis products have been identified using perdeuterated and N-labeled isotopomers. The products consist of low molecular-weight gases and a thermally stable solid residue. The major gaseous products are NO, CO2, CO, N2, HNCO and H2O. Minor gaseous products are HCN, C2N2, NO2, C3H4N2, C3H3N3O and NH3. The elemental formula of the residue is C2HN2O and FTIR analysis suggests that it is polyurea- and polycarbamate-like in nature. The rates of formation of the gaseous products and their respective quantities have been determined for a typical isothermal decomposition experiment at 235°C. The temporal behaviors of the gas formation rates indicate that the overall decomposition is characterized by a sequence of four events; 1) an early decomposition period induced by impurities and H2O, 2) an induction period where CO2 and NO are the primary products formed at relatively constant rates, 3) an autoacceleratory period that peaks when the sample is depleted and 4) a final period in which the residue decomposes. Arrhenius parameters for the induction period are Ea = 46.9 ± 0.7 kcal/mol and Log(A) = 16.3 ± 0.3. Decomposition pathways that are consistent with the data are presented.

Thermal Decomposition of Tobacco Cell-wall Polysaccharides

1977 ◽  
Vol 9 (3) ◽  
Author(s):  
A. Ohnishi ◽  
K. Katō
Keyword(s):  
Thermal Decomposition ◽  
Cell Wall ◽  
Nicotiana Tabacum ◽  
Thermal Reaction ◽  
Thermal Decomposition Mechanism ◽  
Tobacco Cell ◽  
Cell Wall Polysaccharides ◽  
Pyrolysis Products ◽  
Primary Products ◽  
Curie Point Pyrolysis

AbstractIn order to clarify the thermal decomposition mechanism of tobacco cell-wall polysaccharides, some of the primary pyrolysis products were investigated using a Curie-point pyrolysis technique. The major primary products of tobacco cellulose prepared from midribs of Nicotiana tabacum, heated at 460°C for 5 seconds in helium or in vacuum, were such 1,6-anhydrosugars as levoglucosan, 1,6-anhydrob-D-glucofuranose, 1,4,3,6-dianhydro-a-D-glucopyranose and levoglucosenone, and such furan compounds as 5-hydroxymethyl-2-furaldehyde and 2-furaldehyde. The major primary pyrolysis products of tobacco xylan prepared from stalks of Nicotiana tabacum were 3-hydroxy-2-penteno-1,5-lactone and 2-furaldehyde. Some discussions of the thermal reaction mechanism were presented, based on these results.

scholarly journals Thermal Decomposition of HMX: Low Temperature Reaction Kinetics and their Use for Assessing Response in Abnormal Thermal Environments and Implications for Long-Term Aging

1995 ◽  
Vol 418 ◽  
Author(s):  
Richard Behrens ◽  
Suryanarayana Bulusu
Keyword(s):  
Thermal Decomposition ◽  
Solid Phase ◽  
Test Sample ◽  
Storage Conditions ◽  
Kcal Mole ◽  
Decomposition Products ◽  
Gaseous Products ◽  
Thermal Environments ◽  
Higher Temperature

AbstractThe thermal decomposition of HMX between 175°C and 200°C has been studied using the simultaneous thermogravimetric modulated beam mass spectrometer (STMBMS) apparatus with a focus on the initial stages of the decomposition. The identity of thermal decomposition products is the same as that measured in previous higher temperature experiments. The initial stages of the decomposition are characterized by an induction period followed by two acceleratory periods. The Arrhenius parameters for the induction and two acceleratory periods are (Log(A)= 18.2 ± 0.8, Ea = 48.2 ± 1.8 kcal/mole), (Log (A) = 17.15 ± 1.5 and Ea = 48.9 ± 3.2 kcal/mole), (Log (A) = 19.1 ± 3.0 and Ea = 52.1 ± 6.3 kcal/mole), respectively. The data can be used to calculate the time and temperature required to decompose a desired fraction of a test sample that is being prepared to test the effect of thermal degradation on its sensitivity or burn rates. It can also be used to estimate the extent of decomposition that may be expected under normal storage conditions for munitions containing HMX. The data, along with previous mechanistic studies conducted at higher temperatures, suggest that the process that controls the early stages of decomposition of HMX in the solid phase is scission of the N-NO2 bond, reaction of the NO2 within a “lattice cage” to form the mononitroso analogue of HMX and decomposition of the mononitroso HMX within the HMX lattice to form gaseous products that are retained in bubbles or diffuse into the surrounding lattice.

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.

Thermal decomposition and isomerization ofcis-permethrin and β-cypermethrin in the solid phase

2001 ◽  
Vol 58 (2) ◽  
pp. 183-189 ◽  
Author(s):  
Paola González Audino ◽  
Susana A Licastro ◽  
Eduardo Zerba
Keyword(s):  
Thermal Decomposition ◽  
Solid Phase

The slow oxidation of methane

1956 ◽  
Vol 235 (1201) ◽  
pp. 158-173 ◽  
Keyword(s):  
Activation Energy ◽  
Hydrogen Peroxide ◽  
Induction Period ◽  
Hydrofluoric Acid ◽  
Pressure Rise ◽  
Pressure Change ◽  
Kcal Mole ◽  
Gaseous Products ◽  
Oxidation Of Methane ◽  
Reproducible Manner

Mixtures of methane and oxygen behave in a reproducible manner at temperatures of 440 to 520°C and initial pressures of 100 to 350 mm when reacting in Pyrex vessels freshly cleaned with hydrofluoric acid. The apparent order of the reaction ranged from 2∙3 to 2∙6 and the overall activation energy from 29 to 41 kcal/mole. Analyses of the products formed have been made, together with measurements of pressure change. Formaldehyde is formed from the commencement of the reaction including the induction period, but its concentra­tion reaches a maximum near the stage where the pressure rise is a maximum, and then falls off. Hydrogen peroxide is also formed, less rapidly in the earliest stage, but its rate of formation overtakes that of formaldehyde and it reaches an even higher concentration. No other peroxides were detected, nor was methanol found. Hydrogen was present in the gaseous products. These observations are not in full accord with some of the conclusions derived from earlier investigations.

Co-pyrolysis kinetics of sewage sludge and oil shale thermal decomposition using TGA–FTIR analysis

2016 ◽  
Vol 118 ◽  
pp. 345-352 ◽  
Author(s):  
Yan Lin ◽  
Yanfen Liao ◽  
Zhaosheng Yu ◽  
Shiwen Fang ◽  
Yousheng Lin ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Sewage Sludge ◽  
Oil Shale ◽  
Ftir Analysis ◽  
Pyrolysis Kinetics ◽  
Kinetics Of

scholarly journals The influence of the nature and textural properties of different supports on the thermal behavior of Keggin type heteropolyacids

2006 ◽  
Vol 71 (3) ◽  
pp. 235-249 ◽  
Author(s):  
Alexandru Popa ◽  
Viorel Sasca ◽  
Mircea Stefanescu ◽  
Erne Kis ◽  
Radmila Marinkovic-Neducin
Keyword(s):  
Thermal Stability ◽  
Thermal Decomposition ◽  
Thermal Behavior ◽  
Solid Phase ◽  
Textural Properties ◽  
Nitrogen Adsorption ◽  
Active Phase ◽  
Support Surface ◽  
Sem Images ◽  
The Stability

In order to obtain highly dispersed heteropolyacids (HPAs) species, H3PMo12O40 and H4PVMo11O40 were supported on various supports: silica (Aerosil - Degussa and Romsil types) and TiO2. The structure and thermal decomposition of supported and unsupported HPAs were followed by different techniques (TGA-DTA, FTIR, XRD, low temperature nitrogen adsorption, scanning electron microscopy). All the supported HPAs were prepared by impregnation using the incipient wetness technique with a 1:1 mixture of water-ethanol. Samples were prepared with different concentrations to examine the effect of loading on the thermal behavior of the supported acid catalysts. The thermal stability was evaluated with reference to the bulk solid acids and mechanical mixtures. After deposition on silica types supports, an important decrease in thermal stability was observed on the Romsil types and a small decrease on the Aerosil type. The stability of the heteropolyacids supported on titania increased due to an anion-support interaction, as the thermal decomposition proceeded in two steps. The structure of the HPAs was not totally destroyed at 450 ?C as some IR bands were still preserved. A relatively uniform distribution of HPAs on the support surface was observed for all compositions of the active phase. No separate crystallites of solid phase HPAs were found in the SEM images.

scholarly journals An Improved Procedure for the Preparation of Thrombin Low Molecular Weight Substrates - Peptide p-Nitroanilides

2018 ◽  
Vol 1 (4) ◽  
pp. e00057 ◽  
Author(s):  
A.A Chistov ◽  
A.V. Talanova ◽  
M.V. Melnikova ◽  
S.S. Kuznetsova ◽  
E.F. Kolesanova
Keyword(s):  
Molecular Weight ◽  
Solid Phase ◽  
Solid Phase Peptide Synthesis ◽  
Potassium Sulfate ◽  
Polymer Support ◽  
Low Molecular Weight ◽  
Chromogenic Substrate ◽  
Peptide Substrates ◽  
Terminal Amino ◽  
Hydrolysis Of

Low molecular weight chromogenic thrombin peptide substrates, p-nitroanilides of short peptides protected at their N-terminal amino group, were prepared by solid-phase peptide synthesis on polystyrene-divinylbenzene polymer with trityl groups with preliminary attached p-phenylene diamine moiety. After the cleavage from the resin peptide p-aminoanilides were mildly oxidized to p-nitroanilides with the mixture of potassium sulfate and persulfate. Adsorption onto polymer support Bio-Beads SM-2 with further elution by acetonitrile allowed easy separating peptide p-nitroanilides from the oxidizer and obtaining the thrombin chromogenic substrate preparations with the target substance contents of not less than 95% and yields of 30-40%. Thrombin effectively catalyzed hydrolysis of the prepared substrates with KM and Vmax values of 29-134 mM and 0.03-1/16 mM/s, respectively.

scholarly journals Iron reduction from concentrates of hydrometallurgical dressing

2021 ◽  
Vol 64 (10) ◽  
pp. 728-735
Author(s):  
I. A. Rybenko ◽  
O. I. Nokhrina ◽  
I. D. Rozhikhina ◽  
M. A. Golodova ◽  
I. E. Khodosov
Keyword(s):  
Experimental Study ◽  
Thermal Decomposition ◽  
Thermodynamic Modeling ◽  
Iron Reduction ◽  
Solid Phase ◽  
Experimental Studies ◽  
Statistical Processing ◽  
Reducing Agent ◽  
Volatile Components ◽  
Software Complex

The article presents results of theoretical and experimental studies of the processes of iron solid-phase reduction from an iron-containing concentrate obtained as a result of hydrometallurgical dressing of ferromanganese and polymetallic manganese-containing ores with coals of grades D (long-flame) and 2B (brown). The method of thermodynamic modeling using TERRA software complex was used to study the reducing properties of hydrocarbons by calculating equilibrium compositions in the temperature range of 373 - 1873 K. The authors obtained the dependences of compositions and volume of the gas phase formed as a result of the release of volatile components during heating on the temperature for the coals of the grades under consideration. As a result of thermodynamic modeling, the optimal temperatures and consumption are determined, which ensure the complete iron reduction from an iron-containing concentrate. The results of experimental studies were obtained by modern research methods using laboratory and analytical equipment, as well as methods of statistical processing. Results of the coals analysis carried out using the Setaram LabSys Evo thermal analyzer showed that the process of thermal decomposition of coals of the studied grades proceeds according to general laws. The process of thermal decomposition of long-flame coal proceeds less intensively than of brown coal. The results of an experimental study of the processes of thermal decomposition of reducing agents have shown that volumes of the gas phases, formed when coals are heated to a temperature of 1173 K in an argon atmosphere, practically coincide with the calculated values. As a result of thermodynamic modeling and experimental study, the optimal consumption of D and 2B grades of coal is determined at a temperature of 1473 K. The best reducing agent with a minimum specific consumption is long-flame coal of D grade. When determining the optimal amount of reducing agent in charge mixtures during the study of metallization processes, it was found that with an excess of reducing agent, it is possible to achieve almost complete extraction (98 - 99 %) of iron from the concentrate.

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