Solvent extraction of uranium(VI) from aqueous solutions of ammoniumthiocyanate has been investigated in the presence of dibenzo-18-crown-6. Uranium(VI)was quantitatively extracted from 1.0M ammonium thiocyanate using 0.01M dibenzo-18-crown-6in nitrobenzene. Back extraction of U(VI) was quantitative with various strippingagents. Separation of U(VI) from other elements was achieved from binary aswell as multicomponent mixtures. Uranium was determined in monazite sand andsyenite rock samples. The method is very simple, rapid and highly reproducible(approximately ±2%).
The use of ethyl-ga-isonitrosoacetoacetate (HEINA) for determination of palladium is reported. Pd can be estimated quantitatively from 0.5M to 2M HCl solution. Accurate results are obtained in 1M solution with an accuracy better than 1%. Decontamination values against platinum metals and other metals usually associated with Pd are greater than 105. The time required for gravimetric determination is about an hour, for radiochemical separation about 25 min and the recovery is better than 90%.
The objective of the present study was to report the stability of novel antiviral drug, valganciclovir based on the information obtained from forced degradation studies. Valganciclovir was subjected to forced hydrolytic (acidic, alkaline and neutral), oxidative, photolytic and thermal stress in accordance with the ICH guideline Q1A (R2). The drug showed labiality under only acidic and photoacidic conditions while it was stable to other stress conditions. Resolution of the drug and degradation products was achieved on a Hypersil Gold C-18 column (4.6 × 250 mm, 5 μm) utilizing acetonitrile (A) and potassium dihydrogen ortho phosphate buffer (pH 5.0; 0.01M) in the ratio of 5:95 (v/v) at a flow rate of 0.6 ml/min and at the detection wavelength 252 nm. The major acidic stress degradation product was characterized by LC-MS/MS and its fragmentation pathway was proposed. Validation of the LC-DAD method was carried out in accordance with ICH guideline. The method met all required criteria and was applied for analysis of commercially available tablets.
Metal carboxylato-hydrazinates are very good precursors for the synthesis of metal as well as mixed metal oxides as these
decompose to nanosized oxides with high surface area most of the times at comparatively lower temperatures. In the present
study one such novel precursor nickel manganese fumarato-hydrazinate (NiMn2(C4H2O4)3·6N2H4) has been prepared and characterized by XRD, FTIR and chemical analysis. The thermal decomposition of the precursor has also
been studied by isothermal, differential thermal and thermogravimetric analysis. The precursor shows two-step dehydrazination
followed by decarboxylation to form NiMn2O4. The infrared spectra show N-N stretching frequency at 965 cm−1, which confirm the bidentate bridging hydrazine. XRD confirms the formation of single phase NiMn2O4.
n-Octylaniline in bezene was used for the extractive separation of molybdenum (VI) from hydrochloric acid medium. Molybdenum(VI) was extracted quantitatively from 10 ml aqueous solution 1.5M in hydrochloric acid and 10M in lithium chloride into 10 ml of 10%n-octylaninline in benzene. It was stripped from the organic phase with 5% aqueous ammonia solution and estimated spectrophotometrically with thiocyanate at 465 nm. The interference of various ions has been studied in detail and conditions have been established for the determination of molybdenum(VI) in synthetic mixtures and alloy samples.
Complex formation of Th(IV), U(IV), Np(IV), and Pu(IV) with fluoride ions in aqueous perchloric acid solution of 1M ionic strength has been studied potentiometrically, using a fluoride ion selective electrode. A highly acidic medium was essential to prevent hydrolysis and disproportionation of the tetravalent actinide ions. A procedure developed earlier in this laboratory for studying the fluoride complexes of hexavalent actinides was successfully extended to this work. The
1 values follow the trend Th(IV)<U(IV)>Np(IV)>Pu(IV), and
2 values the trend Th(IV)<U(IV)>Np(IV)<Pu(IV), while
4 values followed an increasing order.
Authors:Pooja Sawant, S. Varma, B. N. Wani, and S. R. Bharadwaj
In this article, the role of the preparation route and calcinations temperature on the thermal expansion and conductivity of BaCe0.8Y0.2O3−δ (BCY) has been studied. In particular, the samples were synthesized by means of the solid-state reaction and by a sol–gel route. BCY has been suggested as proton conducting electrolyte for intermediate-temperature solid oxide fuel cells (IT-SOFCs). Proton conductivity strongly depends on the densification of the material as well as the crystal structure, which is generally influenced by the preparation procedure. It was found that a single phase material could be achieved at 1000 °C for the samples prepared through the sol–gel route with ~96% packing density. In case of ceramic route, single phase could be obtained at higher temperatures (1200 °C) and does not lead to good density values. The ceramic synthesis produces BCY material in cubic symmetry where as the gel–citrate complexation route leads to homogenous orthorhombic BCY. The conductivity measurements of sample synthesized by two different routes were investigated by means of impedance spectroscopy and electron microscopy. A comparative study of thermal expansion behavior of BCY synthesized by different route was carried out.
Authors:P. Sawant, S. Prabhu, P. Kalsi, and K. Pendharkar
Individual monitoring of radiation workers handling Pu in various nuclear installations requires the detection of trace levels
of plutonium in bioassay samples. It is necessary to develop methods that can detect urinary excretion of Pu in fraction of
mBq range. Therefore, a sensitive method such as fission track analysis has been developed for the measurement of trace levels
of Pu in bioassay samples. In this technique, chemically separated plutonium from the sample and a Pu standard were electrodeposited
on planchettes and covered with Lexan solid state nuclear track detector (SSNTD) and irradiated with thermal neutrons in APSARA
reactor of Bhabha Atomic Research Centre, India. The fission track densities in the Lexan films of the sample and the standard
were used to calculate the amount of Pu in the sample. The minimum amount of Pu that can be analyzed by this method using
doubly distilled electronic grade (E. G.) reagents is about 12 μBq/L.
Authors:R. Sawant, G. Rizvi, N. Chaudhuri, and S. Patil
Fluoride complexing of Np(V) has been studied using fluoride ion selective electrode (F-ISE). Free fluoride ion concentrations in the presence of Np(V) were measured at 0.1 and 1.0M ionic strength. The data were used to calculate the stability constant of the fluoride complex of Np(V) and the values obtained are reported here.
Authors:R. Sharma, P. Kalsi, L. Sawant, S. Vaidyanathan, and R. Iyer
An iterative computational method for the determination of metal ions in aqueous solutions which form reversible couples such as Fe(II)/Fe(III), Pu(III)/Pu(IV) etc. by controlled potential coulometry has been developed. The method involves carrying out the electrolysis to about 95–97% and calculating the total amount present in the sample by an iterative computational method. The method utilizes the direct application of the Nernst equation. The important criterion to be met is that the coulogram of the couple should strictly obey the Nernst equation. The validity of the method has been checked by analyzing about 50 samples of a standard iron solution. Results of analysis of mixtures of Pu and Fe by the iterative technique show that the interference of Fe can almost entirely be eliminated. However, analysis of Pu samples by this procedure gives results about 2–3% lower than the expected value. A careful examination of the experimental coulograms of Pu in lM HClO4 indicates a slight deviation from the theoretical coulogram, where as those of Fe match exactly.