Preliminary study of the thermally stimulated blue luminescence of ulexite

In this paper, novel results on the blue thermally stimulated luminescence (TSL) emission of ulexite (NaCaB₅O₆(OH)₆·5H₂O) have been studied. The four maxima appearing at 60, 110, 200 and 240°C on the TSL glow curves of this borate could be respectively associated to: (i) the first dehydration (NaCaB₅O₆(OH)₆·5H₂O→NaCaB₅O₆(OH)₆·3H₂O), (ii) the creation-annihilation of the three-hydrated phase, (iii) the Na-coordinated chains dehydroxylation and the starting point of the alkali self-diffusion through the lattice and (iv) the amorphisation of the lattice. These results are fairly well correlated with the differential thermal analyses (DTA), in situ thermal observations under environmental scanning electron microscope (TESEM) and thermal X-ray diffraction (TXRD) techniques.     

Dehydration and dehydroxylation of reduced charge montmorillonite

Reduced charge montmorillonites (RCM) were prepared by the thermal treatment of lithiumsaturated montmorillonite. Samples prepared by mild thermal treatment with lithium contained more water sorbed than the original montmorrilonite. When RCMs were prepared, part of the lithium cations reacted with hydroxyl groups in the octahedral sheet and released protons, which reacted with the structure. Acid treatment probably enhanced the surface area. which was reflected in the amount of water sorbed. Deprotonation of hydroxyl groups was proved by the measurements of the ignition loss. The heating of lithium saturated montmorillonite at higher temperatures brough about the collapse of the interlayers and a decrease in the amount of water sorbed.     

The dehydration of copper(II) acetate monohydrate

The thermal dehydration of copper(II) acetate hydrate has been studied between 353 and 406 K, over a range of humidities. The dehydration is controlled by nucleation-and-growth kinetics at low temperatures, with an activation energy of 154 kJ·mol⁻¹, which changes to contracting-disc kinetics at higher temperatures with a lower activation energy of 76 kJ·mol⁻¹. Frequency factors have also been derived; the value for the high temperature process is low (10⁷s⁻¹) and that for the low temperature step is high (10¹⁷s⁻¹). Optical microscopy has been used to clarify the bulk kinetics; there is evidence for a reactive layer at the surface of the decomposing solid. In celebration of the 60^th birthday of Dr Andrew K. Galwey     

Non-isothermal kinetics of dehydration of equilibrium swollen poly(acrylic acid) hydrogel</o:p>

Summary Kinetics of dehydration of equilibrium swollen poly(acrylic acid) hydrogel was investigated using methods of non-isothermal thermal analysis. Methods of Kissinger, Coats-Redfern, Van Krevelen and Horowitz-Metzger were applied for determination the kinetics parameters: activation energy (E), pre-exponent (lnA) as well as the kinetics model ƒ(69) for the process of hydrogel dehydration under different heating rates. An existence of good agreement between determined values of kinetic parameters (Eand A), which were obtained applying different methods under the same heating rate. Functional relationship between changes of kinetic parameters of dehydration and changes of heating rate was established. An existence of compensation effect is accepted and explanation of compensation effect appearance during the hydrogel dehydration is suggested.     

Deshydratation de l'alun d'ammonium

Dehydration of hydrated ammonium alum is a function of physical gaseous pressure. During dehydration, two kinds of partially dehydrated amorphous alum appears. These solids differ in texture and residual water composition.

     

Equilibria of formation and dehydration of the carbinolamine intermediate in the reaction of benzaldehyde with hydrazine

Measurement of polarographic limiting currents at equilibria made it possible at pH 3-7 to simultaneously determine concentrations of benzaldehyde, of its hydrazone and of the carbinolamine derivative. The dependence of concentration of carbinolamine at equilibrium on pH indicated presence of its di-, mono-, and unprotonated forms. Acid dissociation constants of the formation (pK_a¹≈3.2) of the diprotonated form and of the dissociation of the monoprotonated form of carbinolamine (pK_a²≈4.7) were estimated. The equilibrium constants of formation (K₁) and dehydration (K₂) of the carbinolamine intermediate were determined.     

氧化铝的改性及其在合成气直接制二甲醚反应中的应用

 采用浸渍法制备了经硼、磷和硫的含氧酸根阴离子改性的γ-Al2O3, 以其为甲醇脱水活性组分,与铜基甲醇合成活性组分CuO-ZnO-Al2O3组成双功能催化剂,并在连续流动加压固定床反应器上考察了催化剂对合成气直接制二甲醚反应的催化性能. 结果表明, SO2-4改性可以显著提高γ-Al2O3的甲醇脱水活性,从而提高产物中二甲醚的选择性和一氧化碳的转化率. 此外,还详细研究了SO2-4改性条件如SO2-4含量、焙烧温度及前驱物种类的影响. 结果表明,当SO2-4含量为10%, 焙烧温度为550 ℃时,二甲醚的选择性及一氧化碳的转化率最高; SO2-4前驱物的种类对其改性效果的影响很小.     

Thermal decomposition of Cd(CH3COO)2·2H2O studied by a coupled TG-DTA-MS method

The thermal decomposition of cadmium acetate dihydrate in helium and in air atmosphere has been investigated by means of a coupled TG-DTA-MS method combined with X-ray diffraction analysis. Dehydration of Cd(CH₃COO)₂·2H₂O is a two-stage process with Cd(CH₃COO)₂·H₂O as intermediate. The way of Cd(CH₃COO)₂ decomposition strongly depends on the surrounding gas atmosphere and the rate of heating. CdO, acetone and CO₂ are the primary products of decomposition in air. In helium decomposition goes by two parallel and consecutive reactions in which intermediates, Cd and CdCO₃, are formed. Metallic cadmium oxidizes and cadmium carbonate decomposes giving CdO. Some of the metallic cadmium, depending on the heating rate and the concentration of oxygen, evaporates. Acetone is partially oxidized in secondary reactions with oxygen. This revised version was published online in July 2006 with corrections to the Cover Date.     

Thermal and spectroscopic investigations of new lanthanide complexes with 1,2,4-benzenetricarboxylic acid

The new 1,2,4-benzenetricarboxylates of lanthanide(III) of the formula Ln(btc)·nH₂O, where btc is 1,2,4-benzenetricarboxylate; Ln is La-Lu, and n=2 for Ce; n=3 for La, Yb, Lu; and n=4 for Pr-Tm were prepared and characterized by elemental analysis, infrared spectra and X-ray diffraction patterns. Polycrystalline complexes are isotructural in the two groups: La-Tm and Yb, Lu. IR spectra of the complexes show that all carboxylate groups from 1,2,4-benzentricarboxylate ligands are engaged in coordination of lanthanide atoms. The thermal analysis of the investigated complexes in air atmosphere was carried out by means of simultaneous TG-DTA technique. The complexes are stable up to about 30°C but further heating leads to stepwise dehydration. Next, anhydrous complexes decompose to corresponding oxides. The combined TG-FTIR technique was employed to study of decomposition pathway of the investigated complexes.     

乙醇在杂多酸上的氧化、脱水和程序升温脱附研究

合成了两个系列具有Keggin结构的12-钒钼磷酸和钨钼磷酸,研究了它们对乙醇氧化、脱水的催化反应。借助程序升温脱附技术研究了反应物及产物乙醇、乙烯、乙醚等在样品上的程脱作用。讨论了钨、钒取代部分钼原于后对杂多酸酸性及氧化性能的影响。