XPS characterization of YAlO3:Co single crystals

YAlO₃:Co (YAP:Co) single crystals have been obtained by the Czochralski method. The XPS spectra of YAP:Co annealed in reducing atmospheres: H₂, vacuum and vacuum plus H₂ are presented and discussed. As confirmed by magnetic measurements and the electron spectroscopy XPS the dopant concentration of Co is lower than a nominal one. The annealing processes removed colour centers due to relocation and some reduction of oxygen ions in the structure. The increased unit volume during the long annealing process may be caused by the change in some Co³⁺ ions into Co²⁺ ions. This explains the occurrence of the violet colour of the longtime annealed samples. The chemical shift analysis shows more ionic bond of Y–O than Al–O. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

THERMAL MANAGEMENT OF ALUMINIUM CELL BATH CRUST

When a consumed carbon anode in an aluminium electrolysis cell is replaced, the solid crust covering the anode and the bath is removed and transported in hopper cars to a cooling area where it remains for a period of one to four days, or more, to cool from a temperature of approximately 900°C to an acceptable temperature for autogenous milling, gas cleaning, product classification, and recycle to the process. This article addresses the possibility of processing the hot crust material more rapidly by using a separate or combined crushing/heat exchange system. Results of mechanical and thermal tests are presented and discussed. Mechanical tests demonstrated that it requires much less force to crush hot crust than cold crust samples. The thermal tests consisted of submitting both a single block and a bed of particles of the crust material to heating and cooling cycles to determine the convective heat transfer coefficient and the thermal diffusivity. The values obtained for the heat transfer coefficients were similar to those predicted by correlations, while the thermal diffusivity was larger than expected. Based on the results, a number of strategies to manage the crust material were proposed and analyzed from the perspectives of the plant conditions. Some of these options are briefly discussed and simulated. The results of the simulations indicate that in order to significantly reduce the cooling time, the size of the crust pieces should be reduced prior to cooling.     

New alkyl-phosphate bonded stationary phases for liquid chromatographic separation of biologically active compounds

A new type of bonded stationary phase for liquid chromatography, with the properties of immobilized artificial membranes, has been synthesized. Alkyl-phosphate adsorbents were obtained by modification of aminopropyl silica gel. The structures of the synthesized materials were confirmed by use of instrumental techniques--elemental analysis, infrared spectroscopy (FTIR), and (13)C and (29)Si CP/MAS NMR. Analysis revealed that the adsorbents mimic the phospholipids present in natural cell membranes. The new synthesized alkyl-phosphate stationary phases may be used for liquid chromatographic separation of biologically active compounds of different polarity.     

Study of the retention and selectivity of cholesterol bonded phases with different linkage spacers

The chromatographic properties of four cholesterol bonded phases with different structures were studied. The columns used were packed with a stationary phase containing a cholesterol molecule attached to the silica surface using different types of linkage molecules. As a basic characteristic of the bonded phases the hydrophobicity and silanol activity (polarity) were investigated. The presence of the polar amino and carboxyl groups in the structure of the bonded ligand strongly influences the polarity of the bonded phase. Columns were compared according to methylene selectivity using a series of benzene homologues and according to their shape and size selectivity using polycyclic aromatic hydrocarbons (PAHs). The measurements were done using MeOH–water and ACN–water mobile phases. The presented results show that the coverage density of the bonded ligands and length of the linkage strongly influence the retention and selectivity of cholesterol bonded phases.     

The self-absorption correction factors for 210Pb concentration in mining waste and influence on environmental radiation risk assessment

The radioactive lead isotope ²¹⁰Pb occurs in waste originating from metal smelting and refining industry, gas and oil extraction and sometimes from underground coal mines, which are deposited in natural environment very often. Radiation risk assessment requires accurate knowledge about the concentration of ²¹⁰Pb in such materials. Laboratory measurements seem to be the only reliable method applicable in environmental ²¹⁰Pb monitoring. One of the methods is gamma-ray spectrometry, which is a very fast and cost-effective method to determine ²¹⁰Pb concentration. On the other hand, the self-attenuation of gamma ray from ²¹⁰Pb (46.5 keV) in a sample is significant as it does not depend only on sample density but also on sample chemical composition (sample matrix). This phenomenon is responsible for the under-estimation of the ²¹⁰Pb activity concentration level often when gamma spectrometry is applied with no regard to relevant corrections. Finally, the corresponding radiation risk can be also improperly evaluated. Sixty samples of coal mining solid tailings (sediments created from underground mining water) were analysed. Slightly modified and adapted to the existing laboratory condition, a transmission method has been applied for the accurate measurement of ²¹⁰Pb concentration . The observed concentrations of ²¹⁰Pb range between 42.2?÷?11,700 Bq·kg^–1 of dry mass. Experimentally obtained correction factors related to a sample density and elemental composition range between 1.11 and 6.97. Neglecting this factor can cause a significant error or underestimations in radiological risk assessment. The obtained results have been used for environmental radiation risk assessment performed by use of the ERICA tool assuming exposure conditions typical for the final destination of such kind of waste.     

Study of solvation processes on cholesterol bonded phases

Four cholesterol bonded phases with different structures were investigated. The columns studied were packed with stationary phase containing cholesterol attached to the silica surface using different types of linkage molecules. The presence of the polar amino and carboxyl groups in the structure of the bonded ligand strongly influence on the solvation process. The possibility of hydrogen bonding, dipole-dipole and π-π electron interactions lead to preferential solvation of bonded ligands. The coverage density of bonded ligands and length of the linkage strongly influence the adsorption of solvent from the mobile phase. The removal of residual silanols during the hydrosilation procedure significantly influences solvation of the bonded phase. Excess isotherms of the commonly used solvents in RP HPLC (methanol and acetonitrile) were obtained using the minor disturbance method. For comparison of the stationary phases prepared on different silica gels the excess adsorbed amounts were calculated per volume of the stationary phase in the column. The hydrosilated UDC Cholesterol bonded phase is preferentially solvated by methanol whereas the highest coverage Cosmosil Cholester phase exhibit high adsorption of acetonitrile. Polar groups in the Amino-cholesterol type bonded phase are solvated with both solvent but the mechanisms of these processes are different.     

Site-selective and covalent labelling of the cysteine-containing peptide glutathione with a ferrocenyl group

Site-specific labelling of the cysteine-containing peptide glutathione with a ferrocene group was achieved by reaction with ferrocenylmethanol in aqueous acidic medium. The resulting peptide was shown to be a potent competitive inhibitor of the biologically important enzyme glutathione-(S)-transferase. This approach may prove general for the labelling of proteins with ferrocene.