Authors:V. Bhagavathy, M. Reddy, T. Rao, and A. Damodaran
A method is described for the simultaneous multielement determination of yttrium and lanthanides at microgram level. This is based on the preconcentration of these lanthanides on to 1-(2-pyridylazo)-2-naphthol (PAN) modified naphthalene. The optimal conditions for quantitative preconcentration viz., pH, amount of PAN modified naphthalene, time of stirring and aqueous phase volume were systematically evaluated. The quantitation of lanthanides was carried out by energy dispersive X-ray fluorescence analyzer, employing241Am annular source, via their characteristic K X-rays. The developed procedure gave reliable results in the analysis of xenotime samples.
Authors:Janhavi Rao, Mohan Kumar, L. Sathiyanarayanan, Savita Yadav, and V. Yadav
A sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for analysis of sertraline hydrochloride in the bulk drug and in formulations has been established and validated. Aluminum foil HPTLC plates precoated with silica gel 60F254 as stationary phase were used with toluene-ethyl acetate-ethanol-ammonia 8:2:0.5:0.1 (ν/ν). A compact spot was obtained for sertraline hydrochloride (RF 0.33 ± 0.02). Densitometric analysis was performed in absorbance mode at 273 nm. Regression analysis of calibration data revealed a good linear relationship (r2 = 0.9996 ± 0.02) between response and concentration over the range 2000–12000 ng per band. The method was validated for accuracy, precision, linearity, limits of detection and quantification, and robustness. Sertraline hydrochloride was subjected to acidic and alkaline hydrolysis, oxidation, dry heat treatment, and photodegradation. Peaks of degradation products were well resolved from that of the pure drug and had significantly different RF values. Statistical analysis showed the method enabled repeatable and selective analysis of sertraline hydrochloride. The method can be used for routine quantitative analysis of sertraline hydrochloride in the bulk drug and in formulations.
Authors:M. Charyulu, C. Karekar, V. Rao, and P. Natarajan
The dissolution of carbide fuels was tried with the aid of various oxidants like H2O2, NaBiO3, (NH4)2Ce(NO3)6, (NH4)2S2O8, and AgO in nitric acid medium. During the dissolution, the carbon dioxide liberated has been measured. Among the oxidants studied, H2O2 and NaBiO3 appeared to be more effective for dissolution of carbides. 200–300 mg of sintered uranium carbide sample dissolved within 15 minutes in the presence of oxidants H2O2 or NaBiO3. Mixed carbide sample (70%) was dissolved within 30 min, whereas plutonium carbide required more than one hour. From the resulting solutions uranium and plutonium could be determined by conventional redox methods. More than 97% of plutonium could be recovered and purified from the resulting carbide solutions by conventionally used anion exchange method.
A novel, rapid, and sensitive liquid chromatography-tandem mass spectrometric method was developed and validated for the simultaneous quantification of tenofovir, emtricitabine, and efavirenz in human plasma. Nevirapine was used as an internal standard. The analytes and the internal standard were extracted from human plasma sample by solid-phase extraction technique (SPE). The reconstituted samples were chromatographed on a Chromolith ROD C18 column (50 × 4.6 mm; 5 μ) by gradient elution using a mixture of ammonium acetate buffer (5 mM) and 0.1% formic acid in acetonitrile as the mobile phase at a flow rate of 1.0 mL min−1. The calibration curve obtained was linear (r2 ≥ 0.9990) over the concentration range of 2.5–650 ng mL−1 for tenofovir and 10–4000 ng mL−1 for emtricitabine and efavirenz. The results of the intra- and inter-day precision and accuracy studies were well within the acceptable limits. A run time of 2.5 min for each sample made it possible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies, and the authenticity in the measurement of clinical data is demonstrated through incurred samples reanalysis (ISR).
Authors:M. Oak, S. Tamhankar, V. Rao, and S. Misra
Ten dicoccum wheats were analyzed for their physico-biochemical and milling properties to evaluate the pasta making potential. Dicoccums showed higher protein content and mixograph midline peak values compared to durum variety MACS2846. Mixographic properties of dicoccums were poor compared to durums, due to lower functional visco elastic gluten content. Dicoccums were poorer in milling properties compared to durums, due to lower test weight and thousand-grain weight. Among dicoccums, DDK 1025 showed high micro SDS sedimentation volume and strong mixographic properties, but values were still lesser compared to durum MACS 2846. HMW glutenin subunits in recently developed/released dicoccums were similar to durum parents and were different from the older dicoccums. LMW glutenin subunits, however, were similar to dicoccum parents, except in DDK 1025 which showed LMW glutenin subunits similar to durum wheat. To breed high quality dicoccum wheat for pasta products, breeders should select superior glutenin subunits composition, along with better mixograph properties, keeping morpho-botanical characteristics of dicoccum wheat.
Authors:S. R. Sagi, Karri V. Ramana, and M. S. Prasada Rao
Thallium(III) was precipitated with oxalic acid in the presence of 0.025M RbNO3 (or 0.0125M Rb2SO4) in 0.1M HNO3 (or 0.05M H2SO4). Chemical analysis of the solid obtained corresponds to the formula Rb[TlIII(C2O4)2]·4 H2O. Thermal studies (TG, DTG and DTA) indicated the dehydration and redox decomposition of the thallic salt to the thallous salt, and finally to a mixture of rubidium carbonate and oxides of thallium(I) and thallium(III). Infrared absorption spectra, microscopic observations and X-ray diffraction data were used to characterize the original salt, as well as the intermediates formed during the thermal decomposition of the salt. On the basis of these results, the salt may be represented as: Rb[TlIII(C2O4)2(H2O)2]·2 H2O.
Authors:G. V. Rama Rao, U. V. Varadaraju, S. Venkadesan, and S. L. Mannan
The high temperature superconducting compound YBa2Cu3O72212;δ (Y-123) is synthesised by sol-gel process using various precursors viz., acetate, acetate-citrate, nitrate-citrate and acrylamide. The phase purity of the final product depends on the homogeneity of the gels which intern depends on the bonding of the metal ions in the gels. The samples prepared by acrylamide and nitrate-citrate gel routes yielded phase pure Y-123 compound with better superconducting properties. The mechanism of formation of Y-123 in all these four gel routes is established by characterising the gels and intermediate phases using TG, DTA and XRD techniques. Kinetic analysis is carried out on the mass loss data using the method proposed by Phadni's and Deshpande. Avrami-Erofeev nuclei growth in case of acrylamide, diffusion controlled process in nitrate-citrate and phase boundary reaction mechanisms in case of acetate-citrate gels are found to be responsible for the formation of Y-123 phase.
Authors:M. Swarnalatha, S. Audilakshmi, C.V. Ratnavathi, B. Dayakar Rao, and J.V. Patil
Sorghum can be an alternative to corn for industrial uses, especially in drought prone areas of the world. Sorghum cultivars with high potential of grain and starch yields are needed to continuously meet the industrial demands. We have studied the genetics of grain yield and starch content of sorghum to decide the breeding procedure to develop suitable cultivars for starch industry. The genetic material from 8 × 8 diallel (28 F1 and 8 parents) was grown in a randomized complete block design, with three replications at Directorate of Sorghum Research, Hyderabad, India. Observations were recorded on seven agro-morphological and two grain quality traits including grain yield and starch content. Correlation studies revealed that the grain hardness was negatively correlated to starch and positively correlated to grain yield, panicle weight and days to flowering. Variance due to specific combining ability effects was greater in magnitude for both starch content and grain yield. Bi-parental crossing in F2 will help in getting pure lines with high starch content and high grain yield. The parents chosen for breeding program need to be good combiners for starch and grain yields to obtain superior hybrid. One MS line, 422B was a good combiner for grain yield, high starch content and 100 grain weight, and had good per se performance.
Authors:T. V. Vittal Rao, Ashok Kumar, V. N. Vaidya, and S. K. Mukerjee
A recent study has indicated the feasibility of recycling of chemicals from alkaline waste generated in the preparation of
UO3 microspheres by the internal gelation process. Present paper investigates the recycle process, the volume of the secondary
uranium waste. Result shows that prior to start the recycle process, the waste solution should be freed from uranium by ion-exchange.
Optimized experimental condition to achieve maximum reduction in the volume of uranium based waste is discussed.
Authors:G. Reddy, Pritty Rao, J. Ramana, S. Vikramkumar, V. Raju, and Sanjiv Kumar
The paper describes the determination and depth profiling of oxygen in thin oxide films using 18O(p,α)15N nuclear reaction. The excitation function of 18O(p,α)15N nuclear reaction exhibits a resonance at 629 keV and a plateau at 730 keV with uniform cross-section. The resonance is used
to determine the depth profile of oxygen in films while the plateau, to estimate its overall concentration. The resonance,
characterized by a width of 2.1 keV enables high-depth resolution (~20 nm) measurements and has a probing depth of more than
a micron. The paper presents depth profile measurements of oxygen in several metal oxide films (SiO2, TiO2 and HfO2) using this resonance. Possible interferences arising from 15N(p,α)12C, 19F(p,α)16O and 11B(p,α)2α nuclear reactions are also discussed. It has been shown that it can serve as a suitable alternative to 3.05 MeV 16O(α,α)16O resonant scattering which is generally used for depth profiling oxygen. It is, in fact, more reliable and precise in materials
that witness significant large angle multiple scattering. It can also be advantageously used to monitor 18O, when used as a tracer.