Gamma-radiolytic decomposition of zirconium nitrate and its binary mixtures with potassium halides viz. KCl, KBr and KI has been studied at different compositions up to an absorbed dose of 550 kGy. Radiolytic decomposition has been found to decrease with the absorbed dose. It also varies with the concentration of zirconium nitrate in the binary mixtures. G(NO
) values are enhanced by the addition of halides but only at 75% composition. It is not affected so significantly by KI. A plot of G(NO
) vs. composition of the binary mixtures of the nitrates shows a somewhat parabolic curve with a minimum at 75% Zr(NO3)4+25% KX composition. A part of the energy absorbed by the system is being taken up by the halides depending upon their nature and concentration. Thermal decomposition shows slow decomposition, finally yielding an oxynitrate of indefinite composition.
A controlled potential coulometric method developed earlier for the determination of uranium in the presence of iron or plutonium using platinum working electrode was extended for individual determination of uranium and iron or plutonium in single aliquot. After uranium determination, Fe(III) or Pu(IV) in the aliquot is reduced electrolytically to Fe(II) or Pu(III) and subsequently determined by electrolytic oxidation to Fe(III) or Pu(IV), respectively. Analysis of synthetic solutions indicated that the values for uranium, iron and plutonium obtained by this method are reproducible within±0.2% and are in good agreement with values obtained using conventional redox methods 1, 2.
A controlled potential coulometric method for the determination of uranium in the presence of iron or plutonium using a platinum working electrode has been developed. The method consists of reduction of uranium in 8M H2SO4 by Ti(III) followed by destruction of excess Ti(III) and selective oxidation of Fe(II) or Pu(III) to Fe(III) or Pu(IV), respectively, by sodium nitrite. The U(IV) is subsequently determined by electrolytic oxidation at Pt electrode using Fe(III) as an intermediate. The method was employed for the determination of uranium in synthetic mixtures of U+Fe and U+Pu containing varying ratios of U/Fe or U/Pu. The precision obtained for uranium results was ±0.25%.
Enantiomeric resolution of two commonly used β-blockers, namely, (±)-propranolol and (±)-atenolol, has been achieved on silica gel layers which were bulkimpregnated with β-cyclodextrin. Solvent systems DMF-ethyl acetate-butanol (3:2:5, υ/υ) and butanol-acetic acid-ethyl acetate-ammonia (5:2:2:0.5, υ/υ) successfully resolved the enantiomers of (±)-propranolol and (±)-atenolol, respectively. The spots were located with iodine vapor. The effects of concentration of the chiral selector and mobile phase variation were also studied.
Double nitrates of Na and K having the composition 2MINO3·LnIII(NO3)3·2H2O(LnIII=Pr, Nd, Sm, Eu, Gd, Tb and Dy) and of Ni and Cu with the composition 3MII(NO3)2·2LnIII(NO3)3·24H2O (LnIII=La, Ce, Pr, Nd, Sm, Eu, Gd, Tb and Dy) have been prepared and their -radiolytic decomposition studied up to 500 kGy. G(NO
) values of K double nitrates at 230 kGy follow the order Dy3+>Pr3+=Nd3+=Sm3+>Tb3+>Eu3+> Gd3+·G(NO
) for NI double nitrates are higher than those of Cu double nitrates. Variation of G(NO
) with cationic radii and the number of f electrons in lanthanide ion show a minimum at Eu. Thermal decomposition studies of double nitrates were also carried out.
Coastal sediment samples are collected from the top surface layers of the sediments from Bombay to Kottilppad along the West
coast of India in order to understand the geochemical behaviour of231Pa and the activity ratios of231Pa/235U in this region of the Indian sub-continent. These coastal regions offer a unique advantage for studying the geochemistry
and transport of natural radioactivity due to the placer deposits of monazite in the southern part of India. The top layers
of the surface sediments are leached with 1.0M oxalic acid for the extraction of protactinium activities without attacking
the mineral core of the particles.233Pa tracer is added to the samples. The chemical recovery obtained by counting233Pa is found to vary from 40 to 90%. Total uranium leached from the sediment surface is determined by fluorimetric method and
the concentrations of235U in the leachates are calculated. Using these data, the activity ratios of231Pa/235U have been calculated. These ratios lie in the range of 11.0 to 21.0 for sediments from Bombay to Kottilppad. The data of231Pa activity indicates that there is a deficiency of231Pa in coastal waters of the ocean and that231Pa is removed by precipitation as soon as it is formed by radioactive decay of235U.231Pa is observed to be bound mostly to organic humous material on the surface of the sediment.
Measurements of thorium and uranium isotopic activity ratios have been carried out with top layers of the sediments of the
West coast of India in order to understand the behaviour and distribution of these isotopes in the coastal region. The southern
part of the West coast contains a large amount of placer deposits while the northern region is free from such deposits.
A method for controlled potential coulometric determination of neptunium by titration with internally electrolytically generated iron(II) has been developed. The method involves oxidation of Np to Np(VI) by Ce(IV), destruction of excess of Ce(IV) by NaNO2 followed by determination of neptunium by reduction of Np(VI) to Np(IV) by internal generation of Fe(II). The method was employed for various neptunium solution samples and a precision of ±0.25% at 2–5 mg level of neptunium was obtained.
Authors:A. Joshi, K. Rejith Kumar and H. Hinglajia
Highly significant temporal variations of salinity, Na
content were observed in the habitat. Although quantity of major amino acids was significantly different in leaves, stems and roots of
Rott. ex Willd., their concentrations did not reflect any temporal effects. Accumulation of sugars in vegetative organs and their fluctuations were not significant for thin leaved species
, but their content in
was affected by temporal changes. Amounts of Na
in plant organs were positively related with changes in salinity and mineral ion composition of the habitat. Two species remarkably differed in accumulating amino acids, sugars and mineral ions.
Quantitative determination of uranium in (U, Pu)O2 fuels is usually done by the DAVIES-GRAY method. High concentrations of phosphoric acid in the analytical waste generated by this method make the revocery of plutonium rather complex. Studies on the recovery of plutonium from nitric acid medium containing different concentrations of H3PO4 by conventional anion-exchange procedure reveal that more than 90% of the plutonium can be easily recovered when the phosphoric acid concentration is less than 0.5 M in the solution. A method was developed for the determination of uranium in the presence of plutonium, which involves the reduction of U(VI) to U(IV) by Fe(II) in a medium of 3.5M H3PO4 +4.5M H2SO4 instead of 10–11M H3PO4 so as to have the H3PO4 concentration 0.6M in the waste. A number of determinations of uranium in UO2(NO3)2 working standard solutions and (U, Pu) synthetic solutions with uranium at the 3–7 mg level were carried out by this method. The precision obtained was better than ±0.2% and the accuracy was also within the precision limits. The resulting analytical waste generated was directly subjected to anion exchange separation for the recovery of plutonium which was found to be more than 90%.