A. G. C. Nair

Selective preconcentration and determination of iodine species in milk samples using polymer inclusion sorbent

A method to determine low levels of iodine species namely I(-) and IO(3)(-) in aqueous samples was developed and applied to milk and milk powder samples. It is based on selective preconcentration of I(-) in polymer inclusion sorbent (PIS) and neutron activation analysis (NAA) of I(-) sorbed in PIS. The PIS was found to be highly selective for I(-) in presence of IO(3)(-) and other anions commonly present in the milk samples. In order to preconcentrate total I(-)+IO(3)(-) content in the PIS, IO(3)(-) was reduced to I(-) using a mixture of acetic acid and ascorbic acid. It was found that total iodine content in milk could be determined with epithermal neutron activation analysis (ENAA). A scheme was developed to determine I(-), IO(3)(-) and total iodine. The developed method was applied to milk reference materials (NIST SRM-1549 and IAEA-RM-153 milk powder) and a commercially available milk powder. The scheme for estimation of iodine in different forms was validated by using reference material NIST SRM-1549.

Molecular iodine preconcentration and determination in aqueous samples using poly(vinylpyrrolidone) containing membranes

Membranes for preconcentration of molecular iodine were developed by two different routes: (i) UV-grafting of 1-vinyl-2-pyrrolidone in the pores of microporous poly(propylene) host membrane (grafted membrane), and (ii) physical immobilization of preformed poly(vinylpyrrolidone) (PVP) in a plasticized cellulose triacetate matrix to form the polymer inclusion membrane (PVP-PIM). The UV-grafted PVP-membrane was found to be hydrophilic (water uptake capacity=166 wt.%), while the PVP-PIM was found to be highly hydrophobic ( approximately 2 wt.%). PVP-PIM was found to uptake only I(2) from aqueous sample whereas I(2) and I(3)(-) were sorbed in the grafted membrane. This selectivity of PVP-PIM towards I(2) was attributed to its hydrophobicity that allows only neutral I(2) to interact with PVP in the membrane matrix. Thus, the selective preconcentration and quantitative determination of I(2) in aqueous sample was carried out using PVP-PIM. As PVP-PIM was optically transparent, the characteristic absorbance of PVP-I(2) complex (lambda(max)=361 nm) could be used for quantitative determination of I(2) in the membrane. The instrumental neutron activation analysis (INAA) of the I(2)-loaded PIM samples indicated that 82% could be sorbed into the PIM samples from the solution within 10 min of equilibration time. This membrane was applied to I(2) determinations in the samples of (131)I radiotracer. The concentration level of iodine species in these samples were in sub-ppb level. Therefore, these samples were ideal for testing the preconcentration efficiency of the membrane towards I(2) by monitoring the radioactivity of (131)I. The amounts of I(2) in the aqueous samples were standardized by conventional solvent extraction of I(2) with the chloroform for validating the preconcentration efficiency of PVP-PIM. The detection limit of I(2) in aqueous samples by INAA hyphenated with PVP-PIM was found to be 0.3ppb for a sample size of 25mL.

Application of 140La and 24Na as intrinsic radiotracers for investigating catalyst dynamics in FCCUs

Instrumental neutron activation analysis (INAA) of fluid catalytic cracking (FCC) catalyst samples was carried out with an objective to identify activable elements and evaluate its suitability for use as an intrinsic radiotracer for tracing catalyst itself in Fluid Catalytic Cracking Units (FCCUs) used in petroleum refining. Two catalyst samples obtained from two different refineries were analyzed. Twelve different elements were identified in each catalyst sample and their respective concentrations were determined. From the recorded gamma-ray spectra, it was found that lanthanum-140 ((140)La) and sodium-24 ((24)Na) were the predominantly present and suitable radionuclides that could be used as radiotracers for tracing catalyst in FCCUs. Lanthanum being present in much higher concentration forms the major component of the radiotracer after irradiation. Based on the results of INAA, appropriate quantities of the catalyst samples were irradiated with neutrons to produce the desired amount of activity of lanthanum-140 and sodium-24 to be used as radiotracers for tracing the catalyst itself in a pilot as well as an industrial-scale FCCU. The residence time distribution (RTD) of catalyst was measured and analyzed to determine mean residence time (MRT). The axial dispersion model (ADM) was used to simulate the measured RTD data and investigate the degree of axial mixing. The results of the experiments were used to improve the design of pilot-scale FCCU and optimize the performance of the industrial-scale FCCU.

Multi-element analysis of soil from the north-western region of India by neutron activation analysis using the single comparator method with special reference to selenium toxicity

The single comparator (k0) instrumental neutron activation analysis (INAA) was employed to determine the elemental composition of soil from the north-western region of India. The radiometric assay was carried out using high resolution gamma-ray spectrometry. Seventeen elements were detected including selenium whose concentration was found to be in the range of 1.02 to 6.79 mg/g.

Characterisation of UO2 powders by radioactive adsorption

Abstract It has earlier been shown that radioactive adsorption may be used to characterise the sintering behaviour of UO 2 powders prepared through calcination of ADU. The present paper reports the effect of temperature and concentration on the adsorption of Mn ++ ions on UO 2 powders of varying sinterability. The variation of the density of the adsorbed Mn ++ ions on UO 2 surface follows the classical Langmuir type isotherm. The effect of temperature on the adsorption characteristic is employed to evaluate the bond strength between Mn ++ ions and the powder surface. The bond strength is highest for the 1023 K calcined powder and decreases with rise in the decomposition temperature of the ADU. However 873 K calcined powder shows lower bond strength despite the increase in the total adsorption. The reasons for the anomalous behaviour of 873 K calcined powder are not understood. These studies show that the concentration of the adsorbed species on the surface provides a measure of the sinterability and integral activity of the powder.

Determination of phosphorus using derivative neutron activation

For the determination of phosphorus in different matrices, the derivative neutron activation analysis is especially applicable to aqueous samples, since the conventional neutron activation analysis is not useful for the determination of phosphorus. Phosphorus when reacted with ammonium molybdate 4 hydrate and ammonium metavanadate forms molybdo vanado phosphoric acid. This complex is preconcentrated by extracting into methyl isobutyl ketone. The organic phase containing the molybdo vanado phosphoric acid is neutron activated and the phosphorus is determined through the activation product of 52V. Preparation of this complex, its stoichiometry, application to trace level determination of phosphorus and improved detection limit are discussed. This method was applied for the analysis of industrial effluent samples.

Separation of rare earths by reverse phase partition chromatography

Individual separation of rare earth isotopes from lanthanum to lutetium has been carried out using reverse phase partition chromatography and analyzed by γ-ray spectrometric technique. HDEHP from FLUKA and BDH on inert support celite has been used as extracting agent, whereas hydrochloric acid of different molarities was used as eluting agent. Good separation between individual rare earths has been achieved but the elution pattern differs based on the HDEHP from FLUKA and BDH.