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1.
The thermal decomposition of a series of compounds has been studied by thermogravimetry, mass spectrometry, nuclear magnetic
resonance and elemental analysis. The combined use of mass spectrometry and thermogravimetry (MS and TG) in the analysis of
these compounds has allowed characterization of the fragmentation pattern which was the objective of this research. The gaseous
products, volatile condensed products and solid residues were identified by NMR and MS. Based on the product of thermal decomposition,
the mechanism of thermal decomposition has been derived. 相似文献
2.
硫酸氢钾(KHSO4,A.R)是一种重要的无机化工原料。在化肥工业中,它是生产复合肥硫酸铵钾(KNH4SO4)的主要原料之一。为了找到工业上生产复合肥硫酸铵钾的最佳工艺条件,提高其产率和经济效益,并且开发其新的应用领域,迫切需要该化合物准确的热力学数据作为理论分析的依据。 硫酸氢钾的导热系数,溶解度,熔点等部分热物性数据[1-3]已有报道,但是,迄今为止,文献中未见到它的低温热容和热分解过程的详细报道。本文用精密自动绝热热量计直接测定了硫酸氢钾在78-373K温区的热容,并且将实验热容值用最小二乘… 相似文献
3.
The heat capacities of KHSO 4 crystal (A.R.) have been measured with a small sample precision automated adiabatic calorimeter over the temperature range from 78 to 373 K.The experimental results have shown that there is no phase transition or thermal anomaly in this temperature region for the present crystal.The experimental heat-capacity data have been fitted to a smoothed curve with the aid of the least square method.In addition, the process of the thermal decomposition has been studied by TG analysis. 相似文献
4.
以酒石酸、硝酸氧锆和硝酸铅为原料,合成出了双金属盐酒石酸铅锆,采用有机元素分析、X射线荧光光谱和FTIR对其进行了表征。在程序升温条件下,利用TG/DTG、DSC、固相原位反应池/FTIR联用技术,研究了酒石酸铅锆的热行为和热分解机理,描述了酒石酸铅锆的热分解过程,分析得出其最终分解产物为ZrO2、PbO和C。利用螺压工艺制备了含酒石酸铅锆的推进剂样品,研究了酒石酸铅锆对双基系推进剂燃烧性能的影响,分析了其燃烧催化作用。结果表明,酒石酸铅锆对双基系推进剂的燃烧具有良好的催化作用,是一种高效的燃烧催化剂;酒石酸铅锆热分解的最终产物PbO是催化燃烧的主要活性物质,推进剂燃烧过程中形成了氧化铅-铅循环催化体系,而锆和碳则起辅助催化的作用。 相似文献
5.
A comparative study of phase -boundary and diffusion-controlled reactions has been carried out using thermogravimetric data. The results reported support the hypothesis that a single TG diagram does not allow the determination of whether a solid decomposition reaction is controlled by a diffusion mechanism or governed by the movement of an interface coming from a nucleation process. However, the analysis of both a single TG diagram and an isothermal curve might be a quick and valid way for discerning between these mechanisms. These statements are confirmed by studying the thermal decomposition kinetics of Ba(OH) 2 and CaCO 3. 相似文献
6.
The effects of aluminum (Al) and nickel (Ni) powders
of various grain sizes on the thermal decomposition of ammonium perchlorate
(AP) were investigated by TG and DSC in a dynamic nitrogen atmosphere. The
TG results show that Al powders have no effect on the thermal decomposition
of AP at conventional grain size, while the nanometer-sized Ni powders (n-Ni)
have a great influence on the thermal decomposition of AP with conventional
and superfine grain size. The results obtained by DSC and an in situ FTIR
analysis of the solid residues confirmed the promoting effects of n-Ni. The
effects of n-Ni have been ascribed to its enhancement on the gas phase reactions
during the second step decomposition of conventional grain size AP. 相似文献
7.
Zinc formate dihydrate has been synthesized and characterized by powder X-ray diffraction, elemental analysis, FTIR spectra
and thermal analysis. The molar heat capacity of the coordination compound was measured by a temperature modulated differential
scanning calorimetry (TMDSC) over the temperature range from 200 to 330 K for the first time. The thermodynamic parameters
such as entropy and enthalpy vs. 298.15 K based on the above molar heat capacity were calculated. The thermal decomposition characteristics of this compound
were investigated by thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). TG curve showed that the
thermal decomposition occurred in two stages. The first step was the dehydration process of the coordination compound, and
the second step corresponded to the decomposition of the anhydrous zinc formate. The apparent activation energy of the dehydration
step of the compound was calculated by the Kissinger method using experimental data of TG analysis. There are three sharply
endothermic peaks in the temperature range from 300 to 650 K in DSC curve. 相似文献
8.
Three salts of phenylenediammonium diperchlorate have been prepared and characterized by X-ray crystallography. Their thermal decomposition has been studied by thermogravimetry (TG), differential thermal analysis (DTA), and explosion delay (DE) measurements. The kinetics of thermal decomposition was evaluated by model fitting and isoconversional methods using TG data. The oxidation-reduction reactions near the surface of thermolysing perchlorates may be responsible for the decomposition followed by explosion. The possible pathways of thermolysis have also been proposed. 相似文献
9.
The better use of agricultural residues is expected, when they are mostly disposed of improperly and it is often burned in
the natural environment. This study of the thermal decomposition of residues was performed from the coffee crop for energy
purposes and in this case was used thermal analysis techniques for such assessment. The TG/DTG and DSC curves showed that
the thermal decomposition occurs in four consecutive events and it is predominantly exothermic. The first mass loss evidenced
in TG/DTG curves has an endothermic peak in DSC curve, which it can be associated with the water liberation of the material.
This first thermal event also can be related to the liberation of volatile compounds present in the sample, which is also
corroborated by the endothermic peak. The other events of mass loss are related with the thermal decomposition of the material.
This decomposition has an exothermic behavior, which is positively applied to the main aim of this scientific research: the
coffee straw use like biomass energy font. The thermoanalytical techniques were satisfactory in the characterization of this
material. 相似文献
10.
Ammonium dinitramide (ADN) is a promising high energy oxidizer for rocket propellants because it offers a good oxygen balance and has a significant energy content. As a result, ADN-based energetic ionic liquid propellants (EILPs) have been studied, based on ADN combined with urea and monomethyl ammonium nitrate (MMAN). The thermal decomposition of ADN in the condensed phase affects the combustion of both pure ADN and ADN-based EILPs; thus, it is important to understand the reactions of EILPs in the condensed phase. The present study assessed the reactivity of ADN mixtures in the condensed phase, focussing on hydrogen abstraction reactions with NO2· formed from the thermal decomposition of ADN. The potential energy surfaces of these reactions were obtained using ab initio calculations. The effects of functional groups and of carbon chain length on hydrogen abstraction by NO2· were examined. Mixtures of ADN with urea and acetamide (AA) as amide compounds, and with MMAN and monoethanol amine nitrate (MEAN) as nitrate salts, were examined. Thermal analysis was conducted to investigate the properties of these mixtures, using differential scanning calorimetry (DSC). The calculation results shows that AA and MEAN are more reactive with ADN than urea and MMAN, which is supported by the DSC data. Hydrogen abstraction by NO2· is evidently an important condensed phase reaction in ADN mixtures, and substances having alkyl groups and longer carbon chains are more highly reactive. 相似文献
11.
Three dimethylanilinium sulfates (DMAS) have been prepared and characterised by elemental and spectral studies. Thermal decomposition of these salts has been studied by TG and simultaneous TG-DTG technique and kinetic parameters were evaluated from both dynamic and isothermal TG data using mechanism based kinetic equations. The thermal decomposition pathways have also been suggested and it has been found that DMAS salts give dimethyl aminobenzenesulfonic acids (DMABSA) via solid state reaction. The primary step in the thermal decomposition involves proton transfer followed by sulfonation.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献
12.
本文为进一步弄清Dy(NO3)3.3H2O与B15C5在丙酮中的配合行为, 作者用改进的半微量相平衡方法, 研究了Dy(NO3)3.3H2O-B15C5-CH3COCH3三元体系在18℃时的溶解度, 并进一步分离制备配合物, 研究了配合物的红外光谱, 热力学等性质. 相似文献
13.
The thermal decomposition of nitrocellulose ( NC) 12.1% N, has been studied with regard to kinetics, mechanism, morphology and the gaseous products thereof, using thermogravimetry (TG), differential thermal analysis (DTA), IR spectroscopy, differential scanning calorimetry (DSC) and hot stage microscopy. The kinetics of the initial stage of thermolysis of NC in condensed state has been investigated by isothermal high temperature infrared spectroscopy (IR). The decomposition of NC in KBr matrix in the temperature range of 142–151°C shows rapid decrease in O?NO 2 band intensity, suggesting that the decomposition of NC occurs by the rupture of O?NO 2 bond. The energy of activation for this process has been determined with the help of Avrami-Erofe'ev equation ( n=1) and is ≈188.35 kJ·mol ?1. Further, the IR spectra of the decomposition products in the initial stage of thermal decomposition of NC, indicates the presence of mainly NO 2 gas and aldehyde. 相似文献
14.
用3,5-二硝基水杨酸和硝酸铈为原料,制备了3,5-二硝基水杨酸铈(CeDNS),采用元素分析、X射线荧光光谱和FTIR对其进行了表征。用TG和DSC以及变温固相原位反应池/傅立叶变换红外光谱(RS-FTIR)联用技术研究了3,5-二硝基水杨酸铈的热分解机理,对主放热反应的DSC峰进行了数学处理,计算得到了动力学参数和动力学方程。结果表明,3,5-二硝基水杨酸铈的分解反应共有3个阶段,其中包括一个脱水吸热过程和一个主放热过程,主分解反应发生在第2阶段,主分解反应的表观活化能 Ea与指前因子 A分别为:159.17 kJ·mol -1 和10 11.33 s -1,主分解阶段的反应机理服从Avrami-Erofeev方程( n=1/4),主分解反应的动力学方程为:dα/d t=10 11.33×4(1-α)[-ln(1-α)] 3/4e -1.92×104/T。 相似文献
15.
Zinc ferrite nanocomposite was synthesized via thermal decomposition of zinc acetate and iron nitrate at three different temperatures (350, 450, and 550 °C). The influence of the thermal decomposition of precursors on the formation zinc ferrites was studied by differential thermal gravimetry and thermogravimetry (TG). The TG curve shows two steps for the thermal decomposition with mass loss of 17.3 % at 78 °C and 63.3 % at 315 °C. The prepared zinc ferrites nanocomposite was characterized by X-ray diffraction and scanning electron microscopy. The X-ray diffractograms of ZnFe 2O 4 shows that a crystalline phase, spinel system is formed. SEM micrograph of the zinc ferrite nanocomposite indicates the formation of uniformly spherical 48-nm nanograins. The properties of the zinc ferrite phase were strongly dependent on their calcinations temperature and molar ratio of precursors. 相似文献
16.
A novel two-dimensional metal organic framework MgBTC [MgBTC(OCN) 2·2H 2O, where BTC = 1,3,5-benzenetricarboxylate] has been synthesized solvothermally and characterized by single crystal XRD, powder
XRD, FT-IR spectra. The low-temperature molar heat capacities of MgBTC were measured by temperature modulated differential
scanning calorimetry (TMDSC) over the temperature range from 190 to 350 K for the first time. No phase transition or thermal
anomaly was observed in the experimental temperature range. The thermodynamic parameters of MgBTC such as entropy and enthalpy
relative to reference temperature of 298.15 K were derived based on the above molar heat capacities data. Moreover, the thermal
stability and decomposition of MgBTC was further investigated through thermogravimetry (TG)-mass spectrometer (MS). Four stages
of mass loss were observed in the TG curve. TG-MS curve indicated that the products of oxidative degradation of MgBTC are
H 2O, N 2, CO 2 and CO. The powder XRD showed that the mixture after TG contains MgO and graphite. 相似文献
17.
Strontium zirconyl oxalate hexahydrate (SZO) is prepared and characterized by chemical analysis and IR spectral studies. Its thermal decomposition studies have been made using thermogravimetry (TG) and differential thermal analysis (DTA). The decomposition has been found to proceed through three major steps (i) a three stage dehydration, (ii) decomposition of the oxalate and (iii) decomposition of carbonate to strontium zirconate. Carbon dioxide is found to be trapped in the solid during the decomposition of the oxalate. The identification of residues at various stages has been done by IR spectra and chemical analysis. 相似文献
18.
The thermal decomposition of 31 drugs containing sulphonamides, antituberculous agents, dyes, an oxidant, carboxylic acid derivatives and formaldehyde, expectorants and codeine phosphate has been studied by differential thermal analysis (DTA) and thermogravimetry (TG). The DTA, TG and differential TG curves have been used for identification of the drugs and their qualitative and quantitative analysis. The results for 18 of the drugs were in good agreement with those calculated from the formulation. 相似文献
19.
Ammonium dinitramide (ADN) is one of the several promising new solid propellant oxidizers. ADN is of interest because its oxygen balance and energy content are high, and it also halogen-free. One of the most important characteristics of a propellant oxidizer, however, is stability and ADN is known to degrade to ammonium nitrate (AN) during storage, which will affect its performance. This study focused on the effects of aging on the thermal decomposition mechanism of ADN. The thermal behaviors of ADN and ADN/AN mixtures were studied, as were the gases evolved during their decomposition, using differential scanning calorimetry (DSC), thermogravimetry–differential thermal analysis-infrared spectrometry (TG–DTA-IR), and thermogravimetry–differential thermal analysis-mass spectrometry (TG–DTA-MS). The results of these analyses demonstrated that the decomposition of ADN occurs via a series of distinct stages in the condensed phase. The gases evolved from ADN decomposition were N 2O, NO 2, N 2, and H 2O. In contrast, ADN mixed with AN (to simulate aging) did not exhibit the same initial reaction. We conclude that aging inhibits early stage, low temperature decomposition reactions of ADN. Two possible reasons were proposed, these being either a decrease in the acidity of the material due to the presence of AN, or inhibition of the acidic dissociation of dinitramic acid by NO 3 ? . 相似文献
20.
热重法(TG)是一种动态测量技术,可在程序升温或降温情况下对给定物质或体系提供一个连续的,以温度或时间为函数的重量变化曲线,所以由它跟踪反应能给出反应动力学的有关信息。这种非等温法与早期使用的等温法相比,有快速、连续和需要较少实验数据等优点,近年来在动力学研究方面得到广泛应用,但还只限于研究下列几种类型的简单 相似文献
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