Li-, Na-, K-, Rb- and Cs-montmorillonites were saturated with benzidine, these organo-clay complexes heated under vacuum to
200°C and IR spectra recorded at various temperatures. Benzidine is mostly bound to interlayer cations through water molecules,
except in Cs-clay where bonding to hydrophobic water and to water molecules which are hydrogen bonded to the oxygen plane
predominates. During the thermal treatment water is lost and alkali, cations coordinate directly with benzidine. In Cs-, and
to some extent also in Rb- and K-montmorillonite, benzidine is oxidized to semiquinone and quinoidal cation during the thermal
The influence of thermal treatments on photoluminescence spectra of several minerals has been investigated. By applying step-wise
heating, new luminescence centres were detected which had been not previously recognized in the corresponding minerals. Luminsecence
centres appearing as result of valence changing during oxidizing heating include:
(UO2)2+ as a result of nonluminescent U6+ transformation in zircon, barite, francolite and chert;
Eu2+ as a result of nonluminescent Eu+ transformation in barite.
Luminescence centres which were most stable under thermal treatment were Fe3+ in zircon and Mn2+ in barite. Luminescence centres with similar spectral-kinetic properties but with different thermal stability which allowed
them to be separated and properly identified were different metaloxygen complexes (MeOn)m− in zircon.
Authors:Manal M. Fouad and Christine M. El-Maraghy
A rapid validated thin-layer chromatography (TLC)‒densitometric method has been developed for the simultaneous determination of 3 co-formulated drugs used for common cold and cough treatment. The studied drugs are paracetamol, pseudoephedrine, and chlorpheniramine maleate. The separation was achieved using silica gel 60 F254 plates and the developing system of methanol‒ toluene‒acetic acid (44:16:1, v/v). Densitometry scanning was performed at 254 nm. The method was validated as per the International Conference on Harmonization (ICH) guidelines and was successfully applied for the analysis of pharmaceutical preparation containing the cited ternary mixture without interference from excipients. There is no previously published TLC–densitometric method for the determination of the previously mentioned ternary mixture. The suggested method is rapid and of low cost, so it can be used for quality control analysis.
The solids formation behavior in a simulated high level liquid waste (HLLW) was experimentally examined, when the simulated HLLW was treated in the ordinary way of actual HLLW treatment process. Solids formation conditions and mechanism were closely discussed. The solids formation during a concentration step can be explained by considering the formation of zirconium phosphate, phosphomolybdic acid and precipitation of strontium and barium nitrates and their solubilities. For the solids formation during the denitration step, at least four courses were observed; formation of an undissolved material by a chemical reaction with each other of solute elements (zirconium, molybdenum, tellurium) precipitation by reduction (platinum group metals) formation of hydroxide or carbonate compounds (chromium, neodymium, iron nickel, strontium, barium) and a physical adsorption to stable solid such as zirconium molybdate (nickel, strontium, barium).
Five spices, cumin, coriander, clove, cinnamon and black pepper were irradiated by gamma-ray doses of 1.0 and 5.0 kGy and
thermoluminescence (TL) method was used for identification of the irradiation treatment. The TL response of the minerals isolated
from irradiated samples was much higher as compared to the mineral particles from unirradiated control samples. For the normalisation
of results the separated minerals were reirradiated to a normalisation dose of 1.0 kGy and the TL glow curve was recorded
a second time. By comparing the glow curves of irradiated and unirradiated samples, finding the ratio of the areas of first
and second glow curves (TL1/TL2) and comparing the shapes of the glow curves, all the irradiated and unirradiated samples were identified correctly.
Authors:A. Palamalai, S. Mohan, M. Sampath, R. Srinivasan, P. Govindan, A. Chinnusamy, V. Raman, and G. Balasubramanian
Some batches of233U oxide product obtained from the reprocessing treatment of irradiated thorium rods, called J-rods in our plant, have been found to contain thorium as much as 85% and iron above 5% as impurities. This product has to be purified before sending for fabrication of the fuel. The present purification method consists of the following three steps: (1) preferential dissolution of U3O8 as compared to thoria, (2) a novel solvent extraction process, and (3) preferential precipitation of Th as oxalate leaving behind the entire U in the filtrate. Development and application of the present purification method to the above233U oxide proxduct are presented in this paper.
Authors:K. Barcova, M. Mashlan, R. Zboril, and P. Martinec
The transformation mechanism of Fe cations in natural olivine after thermal treatments in air has been studied using mainly57Fe Mössbauer spectroscopy. -Fe2O3 nanoparticles appear as the primary Fe3+ phase in Mössbauer spectra of olivine samples heated at 600-900 °C. These nanoparticles are thermally unstable and they are transformed to -Fe2O3 with the increase of heating time. Another transformation mechanism of iron related with the complete decomposition of olivine structure has been observed at temperatures of 1000 °C and higher. The mixed oxide MgFe2O4 with the spinel structure and enstatite MgSiO3 were identified as iron-bearing decomposition products.
The resistance against radiation of the tertiary pyridine resins synthesized for the treatment of spent nuclear fuels and high level radioactive waste was evaluated. After irradiation at 10 MGy, only approximately 10% or less of the exchange groups were lost in HCl solutions regardless of their concentrations, while 3040% were lost in HNO3. The pyridine resin has shown remarkable resistance against radiation particularly in HCl solution. It has been revealed that the decomposition of pyridine type resins results from the scission of the principal chains. An irradiation study was conducted also on the quaternary ammonium resins. Quatemization ratio was found to be reduced in HNO3 solutions at 10 MGy irradiation.
Authors:A. Béres, I. Pálinkó, Á. Fudala, I. Kiricsi, Y. Kiyozumi, F. Mizukami, and J. Nagy
Mg-Al L(ayered) D(ouble) H(ydroxide) was prepared and its thermal behaviour was characterized by thermoanalytical methods
(TG, DTG, DTA), 27Al M(agic) A(ngle) S(pinning) NMR spectroscopy, X-ray diffractometry (XRD) and S(canning) E(lectron) M(icroscopy). Heat treatment
destroyed the layered structure, which could only be partially reconstituted by rehydration. On calcination mixed oxide with
the predominance of basic sites were formed. Pillaring the LDH with Fe(CN)64- anions was also performed. The material was characterized by XRD and BET measurements. Heat stability of the pillared substance
was investigated, too. Pillaring proved to be successful, however, decreased heat resistance was found in the intercalated
material relative to the guest LDH.
The phase changes in the solid state in E AlMgSi alloy are discussed. The dissolution and precipitation processes are investigated by DTA, and the results can be applied to control the technological parameters of dissolution heat treatments.