Authors:J. Madarász, E. Beregi, J. Sztatisz, I. Földvári, and G. Pokol
Sintering processes in the Y2O3–Al2O3–B2 O3 system and its subsystems (Y2O3–B2O3 and Al2 O3–B2O3) have been investigated by using combined DTA and XRD measurements to get a better understanding of solid state chemical
changes resulting in the formation of yttrium aluminum borate (YAl3(BO3)4, YAB) phase and to study the possible role and contribution of various simple borates formed also in the former processes.
Two new exothermic heat effects of YBO3 formation have been detected by DTA in the Y2O3–B2O3 system between 720 and 980C. In the Al2O3–B2O3 system a new experimental XRD profile of Al4B2O9 was observed. Formation of these borates seems to promote the nucleation of double borate YAB below 1000C. Conversion of
Al4B2O9 to Al18B4 O33 was observed after a long term (10 h) sintering at 1050C. Similarly, an increased formation of YAB has been observed as
a product of the sintering reaction between YBO3 and Al18B4O33 at 1150C. The two latter single borates are found to be identical with the high temperature decomposition products of YAB.
Authors:D. Kozma, Klára Tomor, C. Novák, G. Pokol, and E. Fogassy
Racemic malic acid (I) was resolved by R-α-phenylethylamine(II). The S-(−)-I.R-(+)-II diastereoisomer was in excess in the precipitated salt. DSC curves and X-ray powder diffractograms proved that the diastereoisomeric salt mixture precipitated during the resolution was isomorphous with the optically pure S-(−)-I.R-(+)-II salt. The diastereoisomeric salt mixture containing the R-(−)-I.R-(+)-II salt in abundance bound crystal solvate (water or methanol) when produced by the total evaporation of the mother liquor, while the optically pure R-(−)-I.R-(+)-II salt crystallized without solvate. It is generally assumed that solid solution formation takes place when the two diastereoisomers are alike and the high similarity results in less efficient enantiomer separation.
Authors:V. Leovac, R. Petković, A. Kovács, G. Pokol, and Katalin Szécsényi
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.
Authors:D. Kozma, C. Novák, G. Pokol, and E. Fogassy
The products obtained in the optical resolution of the N-methylamphetamine by the Pope-Peachy method, using half equivalent R, R-tartaric acid and half equivalent hydrochloric acid in absolute ethanol were investigated by thermoanalytical methods. The DSC measurements of the precipitated salts provide sufficient information for following the progress of the resolution. In this way, the results of the resolution can be estimated with the precision of about 5% optical purity.
Authors:Margit Bán, J. Madarász, Petra Bombicz, G. Pokol, and S. Gál
Composition and structure of crystals of unknown origin, crystallizing spontaneously from ethylenediamine on standing, has
been determined by elemental analysis, FTIR, 1H and 13C NMR spectroscopy and X-ray diffraction. The crystal with molecular formula C6H14N4 has been found to be a highly symmetric
saturated imino compound with double-ring structure, and unambiguously identified as trans-1,4,5,8-tetraazodecalin by 1H NMR and powder X-ray diffraction based on both its specific AA'BB' spin coupling system and simulated XRD pattern calculated
from available data of previous single crystal structure determination, respectively. Simultaneous TG/DTA measurement shows
one-step degradation of this compound. The volatile decomposition products have been followed by both TG/DTA-MS and TG-FTIR.
Group of the largest fragments (m/z=80, 81 and 82) observed by TG/DTA-MS corresponds to an aromatic 1,4-diazine (pyrazine). In the EGA-FTIR spectrum of released
gaseous species measured at the highest evolution rate by TG-FTIR, ethylenediamine can be identified as another decomposition
Authors:C. Novák, G. Pokol, K. Tomor, J. Kőmíves, and S. Gál
The gibbsite →χ-alumina decomposition (in air) and theχ-alumina → boehmite transformation (under hydrothermal conditions) were investigated isothermally. Reaction products were characterized by TG and X-ray diffraction.
Authors:R. Illés, Cs. Kassai, G. Pokol, E. Fogassy, and D. Kozma
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.
Authors:J. Madarász, M. Krunks, L. Niinistö, and G. Pokol
Identification and monitoring of gaseous species released during thermal decomposition of the title compound 1, Zn(tu)2Cl2, (tu=thiourea, (NH2)2C=S) have been carried out in flowing air atmosphere up to 800°C by both online coupled TG-EGA-FTIR and simultaneous TG/DTA-EGA-MS.
The first gaseous products of 1, between 200 and 240°C, are carbon disulfide (CS2) and ammonia (NH3). At 240°C, an exothermic oxidation of CS2 vapors occurs resulting in a sudden release of sulphur dioxide (SO2) and carbonyl sulphide (COS). An intense evolution of hydrogen cyanide (HCN) and beginning of the evolution of cyanamide
(H2NCN) and isothiocyanic acid (HNCS) are also observed just above 240°C. Probably because of condensation and/or polymerization
of cyanamide vapors on the windows and mirrors of the FTIR gas cell optics, some strange baseline shape changes are also occurring
above 330°C. Above 500°C the oxidation process of organic residues appears to accelerate which is indicated by the increasing
concentration of CO2, while above 600°C zinc sulfide starts to oxidize resulting in the evolution of SO2. All species identified by FTIR gas cell were also confirmed by mass spectrometry, except for HNCS.