Authors:A. Singh, A. Kumar, P. Jojo and Rajendra Prasad
Uranium content of soil samples collected from different states of India, namely Uttar Prades, Rajasthan and Kerala has been
estimated. The areas cover the normal background area, high background area and dumpyards of fertilizer factory and thermal
power plant. Plastic sheets were used as a detector for the registration of fission tracks resulting from the (n, f) reaction
on235U present in the sample due to the thermal neutrons from a nuclear reactor. The uranium concentration has been found to vary
from 0.24 to 9.20 μg/g in various soil samples. Higher levels of uranium were found in the vicinity of a coal fired power
plant. The present results may be useful for the radiation hygiene.
Authors:S. Godbole, P. Iyer, M. Jayanth Kumar and M. Sastry
Double sulfates of thallium and lanthanides form an interesting series of compounds with first fractional crystallization leading to the formation of tetrahydrated double sulfates. The radiation induced defects including changes in the oxidation states were studied by carrying out EPR investigations of -irradiated Tl (I) Ln (III) (SO4)2.4H2O (Ln=Sm, Eu and Nd) compounds. The important finding of these investigations is the formation of a radiation-induced paramagnetic center Tl2+ simultaneously with that of Eu2+, revealing their intrinsic association. Similar formation of Tl2+ was not observed in other rare earth salts, implying that the stability of the half-filled electronic configuration of Eu2+ may be responsible for the stabilization of Tl2+. Their relaxation back to Eu3+ and Tl+ simultaneously at 255 K gives further confirmation of their association and suggests that the matrix intrinsically does not favor the stabilization of Eu2+ as reported in a number of other matrices. The hyperfine coupling constant for Tl2+ was calculated using the Breit-Rabi equation and was found to be 80 GHz.
Authors:D. Das, Sumit Kumar, P. Pathak, B. Tomar and V. Manchanda
Release of long-lived radioactivity to the aquatic bodies from various nuclear fuel cycle related operations is of great environmental
concern in view of their possible migration into biosphere. This migration is significantly influenced by various factors
such as pH, complexing ions present in aquatic environment and sorption of species involving radionuclides on the sediments
around the water bodies. 241/243Am are two major radionuclides which can contribute a great deal to radioactivity for several thousand years. In the present
study, 241Am sorption on natural sediment collected from site near a nuclear installation in India, has been investigated under the
varying conditions of pH (3–10) and ionic strength [I = 0.01–1 M (NaClO4)]. The sorption of Am increased with pH of the aqueous medium [10% (pH 2) to ~100% (pH 10)], which was explained in terms
of the increased negative surface charge on the sediment particles. There was marginal variation in Am(III) sorption with
increased ionic strength (within error limits) of the aqueous medium suggesting inner-sphere complexation/sorption process.
Sediment was characterized for its elemental composition and structural phases using Energy Dispersive X-Ray (SEM-EDX) and
X-Ray Diffraction (XRD) techniques. Zeta-potential measurement at I = 0.1 M (NaClO4) suggested that Point of Zero Charge (pHPZC) was ~2, indicating the presence of silica as major component in the sediment. Kurabtov plot using sorption data as a function
of pH at fixed I = 0.1 M (NaClO4) indicated the presence of multiple Am(III) species present on the surface. Potentiometric titration of the suspension indicated
the presence of mineral oxide like behavior and assuming a generic nature (≡XOH) for all types of surface sites, protonation–deprotonation
constants and total number of sites have been obtained. The sorption data has been modeled using 2-pK Diffuse Double Layer
Surface Complexation Model (DDL-SCM). ≡XOAm2+ has been identified as the main species responsible for the sorption profile.
Authors:M. Muthukumar, Shekhar Kumar, P. Sinha, U. Mudali and R. Natarajan
Tri-iso-amyl phosphate is an alternate solvent, proposed in literature as an alternate to the PUREX/UREX solvent tri-n-butyl
phosphate for better physical properties. Its PVT properties and accurate expression for estimation of its vapour pressure
are not available in the literature. Recently PVT properties of TiAP were estimated by authors and its vapour pressure was
measured in a ASTM certified vapor pressure measurement system at temperatures ranging from 273.15 to 373.15 K. In this paper,
results of these studies are presented.
Authors:D. Das, P. Pathak, S. Kumar and V. Manchanda
Sorption behavior of 241Am (~10−9 M) on naturally occurring mineral pyrite (particle size: ≤70 μm) has been studied under varying conditions of pH (2–11),
and ionic strength (0.01–1.0 M (NaClO4)). The effects of humic acid (2 mg/L), other complexing anions (1 × 10−4 M CO32−, SO42−, C2O42− and PO43−), di- and trivalent metal ions (1 × 10−3 M Mg2+, Ca2+ and Nd3+) on sorption behavior of Am3+ at a fixed ionic strength (I = 0.10 M (NaClO4)) have been studied. The sorption of 241Am on pyrite increased with pH from 2.8 (84%) to 8.1 (97%). The sorption of 241Am decreased with ionic strength at low pH values (2 ≤ pH ≤ 4), but was insensitive in the pH range of 4–10, suggesting the
formation of outer-sphere complexes on pyrite surface at lower pH, and inner-sphere complexes at higher pH values. The sorption
of 241Am increased in the presence of (i) humic acid (5 < pH < 7.5), and (ii) C2O42− (2 < pH < 3). By contrast, other complexing anions such as (carbonate, phosphate, and sulphate) showed negligible influence
on 241Am sorption. The presence of Mg2+, Ca2+ ions showed marginal effect on the sorption profile of 241Am; while the presence of Nd3+ ion suppressed its sorption significantly under the conditions of present study. The sorption of 241Am on pyrite decreased with increased temperature indicating an exothermic process.
A stability-indicating gradient reverse-phase liquid chromatographic method was developed for the quantitative determination of process-related impurities and forced degradation products of oxcarbazepine in pharmaceutical formulation. The method was developed by using Inertsil cyano (250 × 4.6 mm) 5 μm column with mobile phase containing a gradient mixture of solvent A (0.01 M sodium dihydrogen phosphate, pH adjusted to 2.7 with orthophosphoric acid and acetonitrile in the ratio of 80:20 v/v) and B (50:40:10 v/v/v mixture of acetonitrile, water, and methanol). The flow rate of mobile phase was 1.0 mL min−1. Column temperature was maintained at 25°C and detection wavelength at 220 nm. Developed reverse-phase high-performance liquid chromatography (RP-HPLC) method can adequately separate and quantitate five impurities of oxcarbazepine, namely imp-A, imp-B, imp-C, imp-D, and imp-E. Oxcarbazepine was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. Oxcarbazepine was found to degrade significantly in acid, base, and oxidative stress conditions. The degradation products were well resolved from oxcarbazepine and its impurities. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness.
Authors:N. Kumar, D. Sangeetha, R. Goyal and P. S. Reddy
A simple, selective, and stability-indicating reverse phase liquid chromatographic method has been developed and validated for the simultaneous determination of impurities and forced degradation products of quetiapine fumarate. The chromatographic separation was achieved on Inertsil-3 C8, 150 mm × 4.6 mm, 5 μm column at 35°C with UV detection at 217 nm using gradient mobile phase at a flow rate of 1.0 mL/min. Mobile phase A contains a mixture of 0.01 M di-potassium hydrogen orthophosphate (pH 6.8) and acetonitrile in the ratio of 80:20 (v/v), respectively, and mobile phase B contains a mixture of 0.01 M di-potassium hydrogen orthophosphate (pH 6.8) and acetonitrile in the ratio of 20:80 (v/v), respectively. The drug product was subjected to the stress conditions of oxidative, hydrolysis (acid and base), hydrolytic, thermal, and photolytic degradation. Quetiapine fumarate was found to degrade significantly in acid, base, and oxidative stress conditions. The degradation products were well resolved from main peak and its impurities. The mass balance was found to be in the range of 96.6–102.2% in all the stressed conditions, thus proved the stability-indicating power of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness.
Authors:P. Jojo, A. Kumar, T. Ramachandran and R. Prasad
Soil samples collected at the Indian Antarctic station Maitree, situated at the Schirmachar Oasis and belonging to the East Antarctic charnockite provinces have been analysed to determine trace uranium concentrations. The fission track technique using Makrofol-KG as the track detector was used for the analyses. Finely powdered samples and pellets were irradiated with thermal neutrons from a nuclear reactor. Uranium concentrations were obtained from the tracks of the detector. Uranium concentrations were found to vary from 0.036 to 0.364 ppm in the samples investigated. The low levels of uranium indicate the absence of human intervention with the lithosphere in this region.
Authors:R. Kumar, G. Baheti, M. Chacharkar and P. Khatri
The corrosion of aluminium has been studied employing the irradiation in situ by neutrons from252Cf and gamma radiations from60Co. The effects of irradiation indicated the absence of pitting, suppression of the corrosion rate, i. e., quantitative reduction in corrosion when measured as weight loss as compared with unirradiated specimens. A protective grayish layer had emerged on the specimen surface which was akin to that formed in simulated experimental conditions carried out in presence of hydrogen peroxide. The possible mechanisms of the elimination of pitting and formation of grayish layer on the surface are discussed.
The trace uranium concentrations have been determined in tobacco obtained from different brands of commercially available cigarette, beedi, chewing tobacco and also in pan masala, using fission track registration technique. Consumption of tobacco orally or by smoking may result in the intake of radioactive elements into the human body causing hazardous effects. External detector method was employed for the determination of uranium using Makrofol-KG as the fission track detector. The range of uranium was found to vary between 0.066–0.106 ppm, 0.042–0.079 ppm and 0.043–0.092 ppm, in tobacco from samples of cigarette, beedi and chewing tobacco, respectively, and between 0.073–0.203 ppm in pan masala samples.