The extraction properties of Th/IV/, Pa/V/, U/VI/ and Np from nitric acid solutions into 1-phenyl-3-methyl-4-benzoylpyrazolone-5 /PMBP/ in toluene were studied, using singlestep batch and continuous H-centrifuge methods. The effects of acid and extractant concentration, temperature and phase contact time on the extraction were investigated.
Effects of relative humidity conditions in the irradiation chamber and of temperature of the chamber on the response of 3 mm thick light blue poly (methyl methacrylate) sheets have been studied. The response was measured spectrophotometrically at 402, 450, 596 and 612 nm. The response of the dosimeter is independent of the relative humidity (12–97%) during irradiation if the response is measured within 24 h of irradiation. If the response is measured after longer storage time, the absorbance at 402 and 450 nm increases significantly. At these two wavelengths the response of the dosimeter is also independent of the temperature of the irradiation chamber in the range of 0 to 40 °C. However, at higher temperatures (60, 80 °C), the response is not uniform.
A copper, zinc and aluminium mixed oxides sample having the nominal composition 0.25 CuO/0.03 ZnO/Al2O3 was prepared by impregnating Al(OH)3 with copper and zinc nitrate solutions, drying at 100 °C then heating in air at 600 °C. The obtained solid was exposed to different doses of -rays (20–160 Mrad). The surface characteristics namelySBETVP andr of different treated adsorbents were determined from N2 adsorption isothems measured at –196 °C. The catalytic activity of various irradiated solids was determined by following up the kinetics of CO-oxidation by O2 at 150–200 °C. The results showed that the doses up to 80 Mrad resulted in no significant change in theSBET but increased slightly theVP (20%) of the treated adsorbents. The irradiation at 160 Mrad caused an increase of 20% in theSBET of the irradiated solid sample. The catalytic activity increased progressively by increasing the dose, a dose of 160 Mrad brought about an increase of 140% in the catalyst's activity. The apparent activation energy of the catalytic reaction decreased monotonically by increasing the absorbed dose of -rays which was attributed to a parallel induced decrease in the value of pre-exponential term of the Arrhenius equation. The observed increase in the catalytic activity due to -irradiation has been interpreted as a result of increasing the concentration of catalytically-active sites contributing in chemisorption and catalysis of CO-oxidation via a possible fragmentation of CuO crystallites.
A solvent extraction procedure for rapid separation of uranium from complex nuclear reaction product mixtures is suggested. The procedure has been tested in batch experiments with tracer amounts of representative elements. It has also been tested with fission products and uranium tracer using the continuous chemical separation system SISAK at the Mainz TRIGA reactor.
Effects of humidity and light conditions /fluoroscent light, sunlight and diffuse sunlight/ on the response of 2 mm thick clear polymethylmethacrylate /PMMA/ dosimeter during irradiation and during postirradiation storage were determined spectrophotometrically at 305 and 314 nm. The results showed that irradiation of dosimeters at 12–97% relative humidity did not result in any change in the response upto 2 weeks of post-irradiation storage. However, there is some decrease in the response at higher humidities />76%/ for longer storage time. Post-irradiation storage and dosimeters at constant relative humidity conditions between 35 and 97% had no effect on the response up-to 3 weeks. Post-irradiation storage at lower relative humidity /12%/ showed some decrease in the response for longer periods. The response of dosimeter is not very sensitive to short time exposure to diffuse sunlight and fluorescent light. However, a significant increase in the optical density was observed during exposure of dosimeters to direct sunlight.
The aqueous solution of coumarin has been studied spectrophotometrically as a -ray dosimeter and effects of temperature and light conditions on the stability of response during post-irradiation storage have been studied. Post-irradiation storage at room temperature in dark showed that after a very small increase in absorbance within the first 6 d, the response of the dosimeter was stable up to 42 d. At lower temperature (–15 °C), there was some decrease in absorbance within the first 24 h followed by a stable response up to 35 d. For post-irradiation storage at higher temperatures (40, 60 °C) the dosimeter, apart from some initial increase in absorbance, showed a nearly stable response up to 25 d. The effect of different light conditions during post-irradiation storage has also been studied. When stored in fluorescent light the response was almost stable from 6 d till about 40 d. In diffuse sunlight, the response was stable up to about 35 d at 360 nm and 370 nm but showed a somewhat unstable behavior at 347 nm. The dosimetric solutions were unstable when exposed to direct sunlight.
Authors:A. Goel, R. Goel, G. Jain Jain, R. Singh Singh, F. Ahmad Ahmad, and G. Singh Singh
A new, specific, sensitive, selective, precise, and reproducible high-performance thin-layer chromatographic (HPTLC) method has been established for study of the stability of 3-acetyl-11-keto-β-boswellic acid (AKBA). HPTLC was performed on aluminium foil plates coated with 200 μm silica gel 60F254. Linear ascending development with toluene-ethyl acetate 7:3 (v/v) was performed at room temperature (25 ± 2°C) in a twin-trough glass chamber saturated with mobile phase vapour. Compact bands (RF 0.52 ± 0.02) were obtained for AKBA. Spectrodensitometric scanning was performed in absorbance mode at 250 nm. Linear regression analysis of the calibration plots showed there was a good linear relationship (r2 = 0.9989 ± 0.0002) between peak area and concentration in the range 200–1200 ng band−1. The method was validated for precision, recovery, robustness, specificity, and detection and quantification limits, in accordance with ICH guidelines. The limits of detection and quantification were 3.06 and 9.29 ng band−1, respectively. The recovery of the method was 99.35–100.21%. AKBA was subjected to various stress test conditions — acid and alkali hydrolysis, oxidation, photodegradation, and dry and wet heat treatment. Degradation products were well resolved from the pure drug with significantly different RF values. Statistical analysis showed the method could be successfully applied for the estimation of AKBA in herbal extract and in nanoparticles. Because the method could effectively separate the drug from its degradation products, it can be regarded as stability-indicating.
Authors:S. Ahmad, G. K. Jain, Md. Faiyazuddin, Z. Iqbal, S. Talegaonkar, Y. Sultana, and F. J. Ahmad
A new, simple, selective, precise, robust and stability-indicating high-performance thin-layer chromatographic (HPTLC) method has been established for analysis of terbinafine hydrochloride (TH) in the bulk drug and in pharmaceutical formulations. Separation was achieved on aluminium plates precoated with silica gel 60F254, with toluene-ethyl acetate-formic acid 4.5:5.5:0.1 (v/v) as mobile phase. Densitometric analysis was performed at 284 nm. Compact bands of TH were obtained at RF 0.31 ± 0.02. Linearity (r2 = 0.9985), limit of quantification (35 ng per band), recovery (97.6−101.6%), and precision (≤2.19) were satisfactory. The method was applicable for routine analysis and accelerated stability testing of TH in pharmaceutical drug-delivery systems. Because the method can effectively separate the drug from its degradation products, it can be used as a stability-indicating method.
Authors:G. A. El-Shobaky, A. S. Ahmad, A. N. Al-Noaimi, and H. G. El-Shobaky
Basic cobalt and copper carbonates were prepared by precipitation from solutions of their nitrates using KHCO3 at room temperature in CO2 atmosphere. The thermal decomposition of the prepared basic carbonates was studied by means of TG and DTA techniques and the phases produced were identified by XRD measurements. The products obtained at 400‡C were subjected to different doses of gamma-rays (40–160 M rad) and the thermal stabilities of these solids were investigated.
Authors:A. Al-Noaimi, G. El-Shobaky, A. Ahmad, and H. El-Shobaky
The effects of -irradiation (20–160 Mrad) and lithium oxide doping (0.75–6 mol%) on the surface and catalytic properties of unloaded Co3O4 solid have been investigated. The surface characteristics of various solids were determined from nitrogen adsorption isothems taken at –196 °C and their catalytic activities were measured by following the kinetics of CO-oxidation by O2 at 100–150 °C using a static method. The results showed that -rays brough about a decrease of 21% inSBET of Co3O4 due to widening of its pores and led also to a considerable increase in its catalytic activity. A maximum increase of 91% was observed upon exposure to a dose of 80 Mrad. Lithium oxide-doping at at 500 °C resulted in an increase of 150% inSBET of treated solid without changing its mean pore radius. This treatment was also accompanied by an increase of about 50% in its catalytic activity measured at 150 °C. Gamma-irradiation and Li2O-doping of unloaded Co3O4 did not change the magnitude of apparent activation energy of catalysis of CO-oxidation by O2 but increased the concentration of catalytically active sites contributing in the catalytic process. In other words, -rays and lithium oxide doping did not alter the mechanism of catalytic oxidation of CO by O2 over unloaded cobaltic oxide solid.