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Abstract  

The optical resolution of racemic mandelic acid (I) by S-2-benzylamino-butanol (II) was performed in water, ethyl acetate, and water saturated ethyl acetate. It was found that the efficiency of the resolution is three times higher in water saturated ethyl acetate than in either water or ethyl acetate. The salt mixtures produced during the resolutions and the pure diastereoisomeric salts were analyzed by TG, DSC and X-ray powder diffraction measurements. The R-(-)-IS-(+)-II salt has the higher melting point and heat of fusion value which indicates that this is the more stable salt. Though the general assumption is that diastereoisomeric salt pairs of successful optical resolutions form eutectic systems, the R-mandelic acid-S-2-benzylamino-butanol and the S-mandelic acid-S-2-benzylamino-butanol system was found to behave in a different way. Melting did not start at or near the estimated eutectic temperature. The difference can be explained either by miscibility in the solid phase (solid solution) or by a blocked interaction between the crystals of the two solid salts. This unusual behaviour of the salt pair should be responsible for the unusual difference in the efficiency of the resolutions performed in different solvents

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Abstract  

In this study the combustion characteristics of crude oils (Karakuę and Beykan) in the presence of a limestone matrix were determined using the thermogravimetry (TG/DTG). Experiments were performed at a heating rate of 10C min-1, whereas the air flow rate was kept constant at 10 L h-1 in the temperature range of 20-900C. In combustion with air, three distinct reaction regions were identified in all crude oil/limestone mixtures studied known as low temperature oxidation (LTO), fuel deposition (FD) and high temperature oxidation (HTO). The individual activation energies for each reaction region may be attributed to different reaction mechanisms, but they do not give any indication of the contribution of each region to the overall reactivity of the crude oils. Depending on the characteristics, the mean activation energy of samples varied between 50.3 and 55.8 kJ mol-1.

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Summary Oxide materials belonging to the Sn-Ce-O system are very interesting due to their use as solid electrolytes in fuel cells, catalysts, sensors and photoanodes in solar cells. The aim of the present work is to investigate the thermal behaviour of some tin and cerium salt mixtures. Mixtures with different representative Sn:Ce atomic ratio were prepared by classical ceramic method using SnC2O4, Ce(SO4)2·4H2O and (NH4)2Ce(NO3)6 as starting compounds. The samples were investigated by means of TG/DTA methods in flowing and static air atmosphere. SnO2 and/or CeO2 were identified by X-ray diffraction and IR spectroscopy in the final decomposition products, depending on the initial composition of the both series. A different crystallinity degree of the solid products was observed depending on the Ce precursor.

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Abstract  

Differential scanning calorimetric (DSC) measurements have been carried out on Bi-Sn based amalgam precursors to be used in compact fluorescent lamps (CFLs) to study the changes in melting and solidifying behaviour caused by In dopant. The phase and elemental compositions of the samples have been characterized by using X-ray diffraction (XRD) and scanning electron microscopy-energy dispersive X-ray analysis (SEM-EDX), respectively. One of the endothermic peaks of the liquid amalgam formation shifted from 121°C to 112 and 105°C, with increasing content of 2.5 and 4.8 mass% In of samples, respectively.

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Abstract  

The enantioselectivity of the diastereomeric supramolecular compound (SMC) formation between O,O'-dibenzoyl-(2R,3R)-tartaric acid (DBTA) and chiral secondary alcohols was investigated. On the basis of TG measurements the DBTA:chiral alcohol molar ratio in the SMC-s is nearly 1:1. Among the investigated complexes the most stable SMC is trans-2-iodo-cyclohexanol-DBTA. The SMC forming capability and the enantioselectivity depends on the space filling of the alcohol side chain or ring. In the case of trans-2-halogen-cyclohexanols a relationship can be observed between the thermal stability of the SMC-s and the enantioselectivity of SMC forming.

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Abstract  

It is well known that SiO2 -based inorganic-organic hybrid materials present significant differences due to the organic moieties bound to the inorganic network and to the preparation conditions. In the present work the ageing effect on the thermal stability of the SiO2 -based inorganic-organic hybrid materials prepared using tetraethoxysilan (TEOS), triethoxymethylsilan (MTEOS), triethoxyvinylsilan (VTEOS), tetramethoxysilan (TMOS), trimethoxymethylsilan (MTMOS) and trimethoxyvinylsilan (VTMOS) was studied. TG/DTA-MS was used to study the decomposition process of the materials. The structural modifications of the materials during ageing were studied using spectral methods. The gels obtained starting with more reactive alkoxides, of methoxy-type, present more complex structures and are less stable during ageing.

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Reactions of divalent transition metal halides with 3,5-dimethyl-1-(hydroxymethyl)-pyrazole

Part 23. Transition metal complexes with pyrazole-based ligands

Journal of Thermal Analysis and Calorimetry
Authors: V. Leovac, R. Petković, A. Kovács, G. Pokol, and Katalin Szécsényi

Abstract  

Factors determining the complex formation reaction of copper(II), nickel(II) and cobalt(II) chloride and copper(II) bromide with 3,5-dimethyl-1-(hydroxymethyl)-pyrazole (HL) has been studied. Depending on experimental conditions, complexes with different composition were obtained: [CuCl2(dmp)]2 (I), [CuCl2(dmp)2]2 (II), [CoCl2(dmp)2] (III) (dmp=3,5-dimethylpyrazole), [CuBr(L)]2 (IV), [CoCl(L)(EtOH)]4 (V) and [NiCl(L)(EtOH)]4 (VI). The compounds were characterized by FTIR spectroscopy, solution conductivity and magnetic measurements. The crystal structure of [CoCl(L)(EtOH)]4 has been determined by single crystal X-ray diffraction. The thermal decomposition of the compounds was studied and found to be continuous for all of the compounds. The desolvation mechanism of [MCl(L)(EtOH)]4 (M=Co(II), Ni(II)) is explained on the basis of the route of complex formation of CoCl2 with HL.

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Thermally induced changes in the oxidation state of cerium(IV)

A study of carbonate and chloro complexes

Journal of Thermal Analysis and Calorimetry
Authors: J. Madarász, T. Leskelä, G. Pokol, and L. Niinistö

Abstract

Cesium hexachlorocerate(IV), Cs2CeCl6 (I) and sodium pentakis(carbonato)cerate(IV), Na6Ce(CO3)5·12H2O (II) have been investigated in air by simultaneous TG/DTA, FTIR and XRD in order to follow the oxidation state of cerium during their thermal treatment. The thermal decomposition of the hexachloro compound (I) is accompanied by a double change in the oxidation state of cerium. First, in an inner reduction-oxidation reaction, chlorine is evolved and a Cs2CeCl5 phase is obtained. The immediately starting oxidation of this Ce(III) species caused various phase transitions in the CeCl3-CsCl system formed. The presence of Cs3CeCl6 above 400°C can also be assumed and finally this phase also oxidizes into CeO2 with the formation of CsCl as by-product. In the case of the pentacarbonato complex (II), no Ce(III) species were detected. The final products of its decomposition were CeO2 and Na2CO3.

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