In-house setup for laboratory-based x-ray absorption fine structure spectroscopy measurements.

We report on a laboratory-based facility for in-house x-ray absorption fine structure (XAFS) measurements. The device consists of a conventional x-ray source for the production of the incident polychromatic radiation and a von Hamos bent crystal spectrometer for the analysis of the incoming and transmitted radiation. The reliability of the laboratory-based setup was evaluated by comparing the Cu K-edge and Ta L3-edge XAFS spectra obtained in-house with the corresponding spectra measured at a synchrotron radiation facility. To check the accuracy of the device, the K- and L-edge energies and the attenuation coefficients below and above the edges of several 3d, 4d, and 5d elements were determined and compared with the existing experimental and theoretical data. The dependence of the XAFS spectrum shape on the oxidation state of the sample was also probed by measuring inhouse the absorption spectra of metallic Fe and two Fe oxides (Fe2O3 and Fe3O4).

Distribution of aluminum over different T-sites in ferrierite zeolites studied with aluminum valence to core X-ray emission spectroscopy.

The potential of valence to core Al X-ray emission spectroscopy to determine aluminum distribution in ferrierite zeolites was investigated. The recorded emission spectra of four samples prepared with different structure directing agents exhibit slight variations in the position of the main emission peak and the intensity of its low energy shoulder. Theoretical calculations indicate that an increased intensity of the Kßx shoulder in the Al emission spectra can be linked to a predominant occupation of the T3 site by a single aluminum atom. This study thus suggests that valence to core X-ray emission spectroscopy can be applied to help determine the occupation of aluminum at crystallographic T-sites in zeolites.

Exploring the potential of a highly compressible microcrystalline cellulose as novel tabletting excipient in the compaction of extended-release coated pellets containing an extremely water-soluble model drug.

Compaction of controlled-release coated pellets into tablets is challenging because of the fusion of pellets and the rupturing of coated film. The difficulty in compaction intensifies with the use of extremely water-soluble drugs. Therefore, the present study was conducted to prepare and compact pellets containing pseudoephedrine hydrochloride as an extremely water-soluble model drug. The pellets were produced using an extrusion-spheronization technique. The drug-loaded pellets were coated to extend the drug release up to 12-h employing various polymers, and then they were compressed into tablets using microcrystalline cellulose Ceolus KG-801 as a novel tabletting excipient. The in vitro drug release studies of coated pellets and tablets were undertaken using the USP basket method in dissolution test apparatus I. The amount of drug released was analyzed at a wavelength of 215 nm. The combined coatings of hydroxypropyl methylcellulose and Kollicoat SR-30D yielded 12-h extended-release pellets with drug release independent of pH of dissolution medium following zero-order kinetics. The drug release from the tablets prepared using inert Celous KG-801 granules as tabletting excipient was found faster than that of coated pellets. However, a modification in drug release rate occurred with the incorporation of inert Ceolus KG-801 pellets. The drug dissolution profile from tablets containing 40% w/w each of coated pellets and inert granules along with 20% w/w inert pellets was found to be closely similar to that of coated pellets. Furthermore, the friability, tensile strength, and disintegration time of the tablets were within the USP specifications.

Kinetics of bromination of safranine by peroxydisulphate ion in presence of bromide ion.

Kinetics of bromination safranine by peroxydisulphate ion in presence of bromide ion has been investigated at various temperatures and ionic strengths. The rate followed first order kinetics in peroxy disulphate and bromide ion each, and zero order kinetics in safranine. A linear relation was obtained for the variation of logarithm of rate constant (log k) with the square root of ionic strength of the media (mu). The rate constants for the rate controlling step were evaluated and interpreted as a function of ionic strengths and temperatures. The values of activation parameters were also computed.