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1.
The influences of atmospheric CO2 and H2O on the kinetics of the thermal decomposition of zinc carbonate hydroxide, Zn5(CO3)2(OH)6, were investigated by means of controlled rate evolved gas analysis (CREGA) coupled with TG. Although CO2 and H2O were evolved simultaneously in a single mass-loss step of the thermal decomposition, different effects of those evolved
gases on the kinetic rate behavior were observed. No distinguished effect of atmospheric CO2 was detected within the possible range of self-generated CO2 concentration. On the other hand, apparent acceleration effect by the increase in the concentration of atmospheric H2O was observed as the reduction of reaction temperature during the course of constant rate thermal decomposition. The catalytic
effect was characterized by the decrease in the apparent activation energy for the established reaction with increasing the
concentration of atmospheric H2O, accompanied by the partially compensating decrease in the pre-exponential factor. 相似文献
2.
The effect of atmospheric water vapor on the kinetic rate behavior of the thermal decomposition of copper(II) carbonate hydroxide,
Cu2CO3(OH)2, was investigated by means of TG-DTA coupled with a programmable humidity controller. With increasing water vapor pressure
p(H2O) from 0.8 to 10.6 kPa, a systematic reduction of the reaction temperature of the thermal decomposition was observed as the
continuous trend from the previous works at the lower p(H2O). Through a comparative kinetic analysis of the reaction at different p(H2O), a catalytic action of the atmospheric water vapor on the nucleation process at the first half of the reaction was identified
as the possible origin of the reduction of the reaction temperature. 相似文献
3.
Sara J. Palmer H. J. Spratt R. L. Frost 《Journal of Thermal Analysis and Calorimetry》2009,95(1):123-129
Thermal analysis complimented with evolved gas mass spectrometry has been applied to hydrotalcites containing carbonate prepared
by coprecipitation and with varying divalent/trivalent cation ratios. The resulting materials were characterised by XRD, and
TG/DTG to determine the stability of the hydrotalcites synthesised. Hydrotalcites of formula Mg4(Fe,Al)2(OH)12(CO3)·4H2O, Mg6(Fe,Al)2(OH)16(CO3)·5H2O, and Mg8(Fe,Al)2(OH)20(CO3)·8H2O were formed by intercalation with the carbonate anion as a function of the divalent/trivalent cationic ratio.
XRD showed slight variations in the d-spacing between the hydrotalcites. The thermal decomposition of carbonate hydrotalcites
consists of two decomposition steps between 300 and 400°C, attributed to the simultaneous dehydroxylation and decarbonation
of the hydrotalcite lattice. Water loss ascribed to dehydroxylation occurs in two decomposition steps, where the first step
is due to the partial dehydroxylation of the lattice, while the second step is due to the loss of water interacting with the
interlayer anions. Dehydroxylation results in the collapse of the hydrotalcite structure to that of its corresponding metal
oxides and spinels, including MgO, MgAl2O4, and MgFeAlO4. 相似文献
4.
《Journal of Coordination Chemistry》2012,65(18):1727-1734
Reaction of urea with sodium tetrachloroaurate(III) dihydrate and zinc(II) chloride has been investigated at room and elevated temperature (~90°C) producing three new compounds: [Au(urea)4]Cl3·2H2O, [Au2(NH2)2Cl2(NCO)(OH)]·H2O and 2ZnCO3·3Zn(OH)2. The infrared spectra were recorded and the observed bands were assigned. The binuclear gold complex and basic zinc carbonate basic were also investigated by thermal analysis, and general mechanisms describing their decompositions are suggested. 相似文献
5.
An instrument of controlled rate evolved gas analysis (CREGA) coupled with TG‐DTA was constructed for analyzing the influences of product gases on the kinetics and mechanism of the thermal decomposition of solids that produce more than one gaseous products at the same stage of reaction. The thermal decomposition of synthetic malachite, Cu2(OH)2CO3, was subjected to the measurements of CREGA‐TG under controlled concentrations of H2O and CO2 in the reaction atmosphere with taking account of self‐generated H2O and CO2 during the course of reaction. By a series of CREGA‐TG measurements carried out under various atmospheric conditions, it was reconfirmed that the reaction is accelerated and decelerated by the effects of atmospheric H2O and CO2, respectively. From the kinetic analysis of the CREGA‐TG curves and results of high temperature X‐ray diffraction measurements under various reaction atmospheres, it was revealed that the anomalous effects of atmospheric H2O on the reactivity and on the reaction rate of the thermal decomposition of synthetic malachite appear at the early stage of the reaction. Usefulness of the CREGA‐TG technique for measuring the kinetic rate data for the thermal decomposition of solids was demonstrated in the present study, by emphasizing the importance of quantitative control of self‐generated reaction atmosphere. © 2005 Wiley Periodicals, Inc. Int J Chem Kinet 37: 346–354, 2005 相似文献
6.
Timothy Biswick Alexandra Pacu?a Jerzy Podobinski 《Journal of solid state chemistry》2007,180(4):1171-1179
The steps associated with the thermal decomposition of Zn5(OH)8(NO3)2·2H2O and ZnOHNO3·H2O are re-examined. Previous reports have suggested that Zn5(OH)8(NO3)2·2H2O decomposes to ZnO via two intermediates, Zn5(OH)8(NO3)2 and Zn3(OH)4(NO3)2 whereas ZnOHNO3·H2O has been reported to decompose to ZnO via a Zn3(OH)4(NO3)2 intermediate. In this study, we demonstrate using TG, mass spectral analysis of evolved gases and in situ variable temperature powder X-ray diffraction analysis that, in fact, in the decomposition of Zn5(OH)8(NO3)2·2H2O an anhydrous zinc nitrate intermediate is also involved. We, additionally, show that the decomposition of ZnOHNO3·H2O to ZnO also involves the formation of an anhydrous zinc nitrate intermediate. The anhydrous zinc nitrate formed in both cases is poorly crystallised and this observation may explain why this phase could not be observed by PXRD analysis in the previous studies. 相似文献
7.
Timothy Biswick William Jones Aleksandra Pacuła Ewa Serwicka Jerzy Podobinski 《Solid State Sciences》2009,11(2):330-335
Zinc hydroxy acetate, Zn5(OH)8(CH3CO2)2·4H2O, has been prepared by the precipitation method. It has been demonstrated by FTIR analysis that, contrary to previous reports, the interaction of the acetate anion with the matrix cation is ionic. TG analysis, mass spectral analysis of the evolved gases, and in situ variable temperature PXRD and FTIR analysis have shown that decomposition of the material to ZnO involves the formation of Zn5(OH)8(CH3CO2), Zn3(OH)4(CH3CO2)2 and anhydrous zinc acetate (Zn(CH3CO2)2) as some of the acetate-containing intermediate solid products. The acetate anion is finally lost, at temperatures below 400 °C, as acetic anhydride, (CH3CO)2O. 相似文献
8.
Marques R. F. C. Zorel H. E. Crespi M. S. Jafelicci M. Paiva-Santos C. O. Varanda L. C. Godoi R. H. M. 《Journal of Thermal Analysis and Calorimetry》1999,56(1):143-149
The compound obtained via state solid reaction of the La2O3 and SrO oxides and expose the room atmosphere shows the crystallographic data of the compound reported as La2SrOx. However, thermogravimetric, differential thermal analysis and XRD with controlled temperature indicated that the stoichiometry
of the compound is 2La(OH)3-SrCO3, which structural parameters were determined by using the Rietveld method. It was verified that when the compound exposed
at room atmosphere, the mixture oxide absorbs H2O and CO2 producing hydroxide and carbonate of lanthanum and strontium, respectively, which thermal decomposition occurs by the same
steps, producing the La2O3-SrO.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
9.
Fabrication of mesoporous ZnO nanosheets from precursor templates grown in aqueous solutions 总被引:1,自引:0,他引:1
Keita Kakiuchi Eiji Hosono Toshio Kimura Hiroaki Imai Shinobu Fujihara 《Journal of Sol-Gel Science and Technology》2006,39(1):63-72
Mesoporous ZnO nanosheets were successfully prepared by pyrolytic transformation of zinc carbonate hydroxide hydrate, Zn4CO3(OH)6·H2O. The nanosheets were initially formed as assemblies on glass substrates during chemical bath deposition (CBD) in aqueous
solutions of urea and zinc acetate dihydrate, zinc chloride, zinc nitrate hexahydrate, or zinc sulfate heptahydrate at 80°C.
It was key to induce heterogeneous nucleation of Zn4CO3(OH)6·H2O by promoting a gradual hydrolysis reaction of urea and controlling the degree of supersaturation of zinc hydroxide species.
Morphology of Zn4CO3(OH)6·H2O was largely influenced by the anions present in the CBD solutions. The Zn4CO3(OH)6·H2O nanosheets were transformed into wurtzite ZnO by heating at 300°C in air without losing the microstructural feature. 相似文献
10.
Hongfei Cheng Qinfu Liu Shuai Zhang Shaoqing Wang Ray L. Frost 《Journal of Thermal Analysis and Calorimetry》2014,116(2):887-894
The products evolved during the thermal decomposition of the coal-derived pyrite/marcasite were studied using simultaneous thermogravimetry coupled with Fourier-transform infrared spectroscopy and mass spectrometry (TG-FTIR–MS) technique. The main gases and volatile products released during the thermal decomposition of the coal-derived pyrite/marcasite are water (H2O), carbon dioxide (CO2), and sulfur dioxide (SO2). The results showed that the evolved products obtained were mainly divided into two processes: (1) the main evolved product H2O is mainly released at below 300 °C; (2) under the temperature of 450–650 °C, the main evolved products are SO2 and small amount of CO2. It is worth mentioning that SO3 was not observed as a product as no peak was observed in the m/z = 80 curve. The chemical substance SO2 is present as the main gaseous product in the thermal decomposition for the sample. The coal-derived pyrite/marcasite is different from mineral pyrite in thermal decomposition temperature. The mass spectrometric analysis results are in good agreement with the infrared spectroscopic analysis of the evolved gases. These results give the evidence on the thermal decomposition products and make all explanations have the sufficient evidence. Therefore, TG–MS–IR is a powerful tool for the investigation of gas evolution from the thermal decomposition of materials. 相似文献
11.
Hongfei Cheng Qinfu Liu Jing Liu Bo Sun Yanxia Kang Ray L. Frost 《Journal of Thermal Analysis and Calorimetry》2014,116(1):195-203
The products evolved during the thermal decomposition of kaolinite–urea intercalation complex were studied by using TG–FTIR–MS technique. The main gases and volatile products released during the thermal decomposition of kaolinite–urea intercalation complex are ammonia (NH3), water (H2O), cyanic acid (HNCO), carbon dioxide (CO2), nitric acid (HNO3), and biuret ((H2NCO)2NH). The results showed that the evolved products obtained were mainly divided into two processes: (1) the main evolved products CO2, H2O, NH3, HNCO are mainly released at the temperature between 200 and 450 °C with a maximum at 355 °C; (2) up to 600 °C, the main evolved products are H2O and CO2 with a maximum at 575 °C. It is concluded that the thermal decomposition of the kaolinite–urea intercalation complex includes two stages: (a) thermal decomposition of urea in the intercalation complex takes place in four steps up to 450 °C; (b) the dehydroxylation of kaolinite and thermal decomposition of residual urea occurs between 500 and 600 °C with a maximum at 575 °C. The mass spectrometric analysis results are in good agreement with the infrared spectroscopic analysis of the evolved gases. These results give the evidence on the thermal decomposition products and make all explanation have the sufficient evidence. Therefore, TG–MS–IR is a powerful tool for the investigation of gas evolution from the thermal decomposition of materials and its intercalation complexes. 相似文献
12.
P. S. Sokolov A. N. Baranov A. S. Alikhanyan M. I. Nikitin Zh. V. Dobrokhotova 《Russian Journal of Inorganic Chemistry》2007,52(12):1963-1967
The gas phase over nanocomposites consisting of zinc carbonate hydroxide (ZCH) Zn2(OH)2CO3 · xH2O(x = 1, 3) dispersed in a NaCl matrix has been characterized by high-temperature mass spectrometry and on-line FTIR spectroscopy coupled with thermal analysis. Volatile zinc-sodium chloro complexes are in equilibrium with ZCH-rich nanocomposites at 20–700°C under mass spectrometric conditions. This is evidence that sodium chloride reacts readily with zinc oxide nanoparticles. The thermal events in the ZCH-NaCl (Li2CO3) system have been investigated by differential scanning calorimetry. 相似文献
13.
R. L. Frost J. M. Bouzaid A. W. Musumeci J. T. Kloprogge W. N. Martens 《Journal of Thermal Analysis and Calorimetry》2006,86(2):437-441
The thermal
stability and thermal decomposition pathways for synthetic iowaite have been
determined using thermogravimetry in conjunction with evolved gas mass spectrometry.
Chemical analysis showed the formula of the synthesised iowaite to be Mg6.27Fe1.73(Cl)1.07(OH)16(CO3)0.336.1H2O
and X-ray diffraction confirms the layered structure. Dehydration of the iowaite
occurred at 35 and 79°C. Dehydroxylation occurred at 254 and 291°C.
Both steps were associated with the loss of CO2. Hydrogen
chloride gas was evolved in two steps at 368 and 434°C. The products of
the thermal decomposition were MgO and a spinel MgFe2O4.
Experimentally it was found to be difficult to eliminate CO2
from inclusion in the interlayer during the synthesis of the iowaite compound
and in this way the synthesised iowaite resembled the natural mineral. 相似文献
14.
T. Sato 《Journal of Thermal Analysis and Calorimetry》2005,82(3):775-782
Summary Indium hydroxides were prepared by the mixing of aqueous indium nitrate solution with sodium or ammonium hydroxide solutions
under various conditions. The thermal decomposition of the resulting materials was examined by thermogravimetry, differential
thermal analysis, X-ray diffraction study and infrared spectroscopy. It has been found that sodium hydroxide solution is more
suitable than the addition of ammonium hydroxide solution to prepare indium hydroxide in well crystallization; the thermal
decomposition of indium hydroxide, in which the composition is In(OH)3·xH2O where x£2, proceeds according to the following process: In(OH)3·xH2O?cubic In(OH)3?cubic In2O3 相似文献
15.
Prateek Bhojane Armel Le Bail Parasharam M. Shirage 《Acta Crystallographica. Section C, Structural Chemistry》2019,75(1):61-64
The successful attempt to solve the crystal structure of Co(CO3)0.5(OH)·0.11H2O (denoted CCH ), based on synchrotron powder diffraction data, leads to a drastic revision of the chemical formula to Co6(CO3)2(OH)8·H2O [hexacobalt(II) bis(carbonate) octahydroxide monohydrate] and to a hexagonal cell instead of the orthorhombic cell suggested previously [Porta et al. (1992). J. Chem. Soc. Faraday Trans. 88 , 311–319]. This results in a new structure‐type related to malachite involving infinite chains of [CoO6] octahedra sharing edges along a short c axis, delimiting tunnels having a three‐branched star section. All reports discussing cobalt hydroxycarbonates ( CCH ) without any structural knowledge and especially its topotactic decomposition into Co3O4 have, as a result, to be reconsidered. 相似文献
16.
The thermal decomposition of natural iowaite of formula Mg6Fe2(Cl,(CO3)0.5)(OH)16·4H2O was studied by using a combination of thermogravimetry and evolved gas mass spectrometry. Thermal decomposition occurs over
a number of mass loss steps at 60°C attributed to dehydration, 266 and 308°C assigned to dehydroxylation of ferric ions, at
551°C attributed to decarbonation and dehydroxylation, and 644, 703 and 761°C attributed to further dehydroxylation. The mass
spectrum of carbon dioxide exhibits a maximum at 523°C. The use of TG coupled to MS shows the complexity of the thermal decomposition
of iowaite.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
17.
J. M. Bouzaid R. L. Frost A. W. Musumeci W. N. Martens 《Journal of Thermal Analysis and Calorimetry》2006,86(3):745-749
The thermal
stability and thermal decomposition pathways for synthetic woodallite have
been determined using thermogravimetry in conjunction with evolved gas mass
spectrometry. Chemical analysis showed the formula of the synthesised woodallite
to be Mg6.28Cr1.72Cl(OH)16(CO3)0.36⋅8.3H2O and X-ray diffraction confirms the layered
LDH structure. Dehydration of the woodallite occurred at 65°C. Dehydroxylation
occurred at 302 and 338°C. Both steps were associated with the loss of
carbonate. Hydrogen chloride gas was evolved over a wide temperature range
centred on 507°C. The products of the thermal decomposition were MgO and
a spinel MgCr2O4. Experimentally
it was found to be difficult to eliminate CO2 from
inclusion in the interlayer during the synthesis of the woodallite compound
and in this way the synthesised woodallite resembled the natural mineral. 相似文献
18.
A combination of high resolution thermogravimetric analysis coupled to a gas evolution mass spectrometer has been used to study the thermal decomposition of synthetic hydrotalcites reevesite (Ni6Fe2(CO3)(OH)16·4H2O) and pyroaurite (Mg6Fe2(SO4,CO3)(OH)16·4H2O) and the cationic mixtures of the two minerals. XRD patterns show the hydrotalcites are layered structures with interspacing distances of around 8.0. Å. A linear relationship is observed for the d(001) spacing as Ni is replaced by Mg in the progression from reevesite to pyroaurite. The significance of this result means the interlayer spacing in these hydrotalcites is cation dependent. High resolution thermal analysis shows the decomposition takes place in 3 steps. A mechanism for the thermal decomposition is proposed based upon the loss of water, hydroxyl units, oxygen and carbon dioxide. 相似文献
19.
《Journal of Coordination Chemistry》2012,65(4):353-358
Abstract Reaction of copper and of copper in presence of zinc with glycylglycine H2Gg, H2NCH2CONHCH2COOH (in ratios 1:2 and 1:1:2, respectively), and an excess of hydrogen peroxide results in the formation of a novel peroxy complex [Cu(O2 2-) (H2Gg)2].2H2O and a mixed metal peroxo carbonate complex [Cu, Zn(O2 2-(CO3)(H2O)4], respectively. A notable feature of the reaction is the facile decomposition of the peptide bond at room temperature on addition of zinc to the system. 相似文献
20.
The analysis of the sequence of electron paramagnetic resonance (EPR) spectra of trace amounts of substitutional probing paramagnetic ions incorporated in (nano)crystalline samples submitted to isothermal and isochronal pulse annealing treatments can offer a wealth of information on the thermally induced compositional and structural changes of the host material. The potential of this new thermal analysis method is illustrated here with results of such investigations on the thermal decomposition of crystalline zinc hydroxide (Zn(OH)2) and anhydrous zinc carbonate basic (Zn5(CO3)2(OH)6) precursors containing trace amounts of substitutional Mn2+ probing ions into nanostructured zinc oxide-ZnO. The quantitative analysis of the sequence of isochronal pulse annealing EPR spectra could provide, besides the thermal decomposition curves of the two precursors, additional information about the structure of the resulting nanostructured ZnO, some of it hard to get by standard structural diffraction techniques. The analysis of both isochronal and isothermal pulse annealing EPR data was further used to investigate the crystallization mechanism of the initially formed nanostructured disordered ZnO and to quantitatively describe the further growth of the resulting ZnO nanocrystals with the increasing annealing temperature and duration. 相似文献