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In this work, we report the distribution ratios of Zr(IV), Co(II), Sb(V) and Nb(V) using polyaniline in HCl, HF, oxalic acid and HF + HCl solutions. Distribution ratios were determined by batch method using radiotracer technique. Further, the separation factors and the %-uptake of metal ions were calculated and compared. Among the media studied, separation factors for Co(II), Sb(V) and Nb(V) with respect to Zr(IV) were the highest in 1 M HCl and the values are 52, 108 and 404 respectively. The results of this study can be utilized for designing an ion-exchange process for the decontamination of zircaloy pressure tubes used in the Pressurized Heavy Water Reactors.

The effects of gamma irradiation on a lignocellulosic biosorbent—coir pith were studied in view of its utilization for separation of metal ions of nuclear importance. The biosorbent was irradiated up to a dosage of 3.6 MGy using a 60Co source. Physicochemical changes induced by γ irradiation in coir pith, were investigated using fourier transform infrared spectroscopy, thermogravimetric and differential thermal analysis. Irradiation in air had negligible effect on the chemical structure of coir pith. However, irradiation in aqueous medium partially altered the chemical linkages in coir pith; which reflected in marginal decrease in its sorption capacity for strontium.

Sorption of niobium on silica colloids was studied using radiotracer technique in the pH range of 2–11 in NaClO4 medium. Silica was characterized using X-ray diffraction, light scattering and surface area measurements. The point of zero charge for silica colloids was about pH 2. The sorption of niobium was >99 % in the pH range of 3–9 and was slightly lower (~95 %) below pH 3 and above pH 9. The quantitative sorption in the pH range 3–9 could be explained by surface complexation model. The small reduction in sorption was attributed to the existence of small fraction of niobium as cationic species at pH ≤ 2 and anionic species above pH 9. Presence of humic acid was found to have negligible effects on the sorption characteristics.

A simple, fast and sensitive instrumental neutron activation analysis (INAA) method has been optimized for the determination of trace concentrations of chlorine in five types of samples namely zirconium oxide, zircaloy 2, zircaloy 4, Zr–Nb alloy and Zr–Sn alloy samples. The samples were neutron irradiated for short duration (1 min) using pneumatic carrier facility of Dhruva research reactor at a neutron flux of 5 × 1013 cm−2 s−1 and measurement of 1,642.7 keV gamma-ray of 38Cl was carried out using a 40 % HPGe detector coupled to 8 k MCA. Concentrations of chlorine were found to be in the range of 9–575 mg kg−1. The 3σ detection limits of chlorine were in the range of 0.1–2.7 mg kg−1 for various samples.

The Fifth Symposium on Nuclear Analytical Chemistry (NAC-V) was organized at BARC, Mumbai during January 20–24, 2014 with more than 300 participants. It was sponsored by the Board of Research in Nuclear Sciences, Department of Atomic Energy (DAE), India and organized in cooperation with the IAEA and coorganized by the IANCAS. A total of 240 contributed abstracts along with 27 invited talks and 10 invited short talks were presented in 15 technical sessions. Selected 54 full papers of NAC-V have been accepted after review for publication in special issue of JRNC.

In this study we present quantitative elemental analysis techniques like energy dispersive X-ray fluorescence analysis and instrumental neutron activation analysis to assess the impact of industrial discharge on environment. Two cases are discussed, i.e., (a) enrichment of zinc levels in the soil (1080 ± 76 mg kg−1) and zinc uptake ranging between 628 and 40 mg kg−1 in edible plants and cereals grown in agricultural fields near an active zinc smelter, Rajasthan; (b) depth-wise distribution of Cr, Pb and other metals in the sediment core samples from Sundarban wetland, West Bengal, indicating waste discharge from tanneries and other industries.

The pneumatic carrier facility (PCF) of Dhruva reactor is being extensively used for neutron activation analysis (NAA) studies pertaining to research work as well as routine sample analysis. It is useful for the determination of trace elements using short and medium half-lives radioisotopes produced in neutron activation with available higher neutron flux (~5 × 1013 cm−1 s−1). Solid samples placed in high density polypropylene capsule, are irradiated for 1 min duration and radioactive assay is carried out by high resolution gamma ray spectrometry. Design aspects of PCF and various applications to samples of diverse matrices using NAA are presented.

Boron is an important element in nuclear technology. A comparative study was carried out for the determination of boron in borosilicate glass, boron carbide and graphite samples by wet-chemical and nuclear analytical methods. Wet chemical methods namely titrimetry, Inductively Coupled Plasma Mass Spectrometry and ICP Optical Emission Spectrometry and nuclear analytical methods namely Particle Induced Gamma-Ray Emission and Nuclear Reaction Analysis were used. Boron concentrations were in trace (mg kg−1) level in graphite and percentage level in borosilicate glass and boron carbide.

The k 0-based neutron activation analysis method was applied for multielement determination in black and yellow serpentines along with two associated minerals namely altered and unaltered dolomites and intrusive rock dolerite, obtained from the asbestos mines of Cuddapah basin, Andhra Pradesh, India. Concentrations of 20 elements were determined and they were used to predict the process of formation of fibrous chrysotile asbestos. Majority of elements as well as REEs reveal the contribution of elements from both dolerite and dolomite during the process of contact metamorphism in forming the mineral serpentine.

During this work, size fractionation technique “ultra filtration” is used in physical speciation of thorium in organic rich groundwater. Laboratory simulated experiments were carried out to study the physical speciation of thorium in aquatic environment having elevated level of dissolved humus material classified as dissolved organic carbon (DOC). Samples were collected from organic rich environment having DOC in the range of 50–60 µg mL−1. Th(IV) ions are extremely particle reactive having K d value of the order of 105–6, hence to avoid adsorption on suspended particulate matter, spiking of the solution with Th(NO3)4 was carried out in ground water samples after filtering through 450 nm pore size using suction filtration. Particles in dissolved state (colloids) ranging between 220 nm were separated using suction filtration assembly having a membrane with a pore diameter of 220 nm. Thereafter, solution was sequentially passed through the ultra-filtration membranes having pore diameters of 14 nm [300 k NMWL (nominal molecular weight limit)], 3.1 nm (50 k NMWL), 2.2 nm (30 k NMWL), 1.6 nm (10 k NMWL) and 1.1 nm (0.5 k NMWL) by using “Stirred Ultra-filtration Cells”, operating in concentration mode. Thorium has only one stable oxidation state i.e. IV, under all redox conditions in natural waters and therefore, its speciation is dominated by its interaction with various fractions of DOC. Experimental results show 50–60 % of the spiked Th is in association with fraction enriched with particles of 10 k NMWL (1.6 nm) followed by fraction enriched with particle of 0.5 k NMWL and

The total metal concentration and bioaccessible concentration of Cr, Mn, Fe, Cu, Zn, Se in Momordica charantia, Asparagus racemosus, Terminalia arjuna and Syzyzium cumini were measured by instrumental neutron activation analysis and by inductively coupled plasma mass spectrometry analysis (ICP-MS). The bioaccessible concentrations were determined in the gastrointestinal digest obtained after treating dried powdered samples sequentially in gastric and intestinal fluid of porcine origin at physiological conditions. The bioaccessible concentration of Fe was in the range of 58–67 mg kg−1, Mn was 10.2–14.6 mg kg−1, Cu was 3.7–4.8 mg kg−1 and Zn was 10.6–18.4 mg kg−1, were within the safety limits set for vegetable food stuff set by Joint FAO/WHO. The bioaccessibility of Zn, an essential element, was high (40–50 %) in M. charantia and in S. cumini. In addition, the total metal contents and bioaccessible concentration of Ni, Se, Cd and Pb in these samples were measured by ICP-MS. The total Cd content in S. cumini (2.6 ± 0.2 mg kg−1) and its bioaccessible concentration (0.6 mg kg−1) were strikingly high as compared to the other samples. Though total Hg contents were determined by ICP-MS, but their bioaccessible concentrations were below the detection limit (0.036 mg kg−1).

As a part of inter comparison exercise of an IAEA Coordinated Research Project on large sample neutron activation analysis, a large size and non standard geometry size pottery replica (obtained from Peru) was analyzed by k 0-based internal monostandard neutron activation analysis (IM-NAA). Two large size sub samples (0.40 and 0.25 kg) were irradiated at graphite reflector position of AHWR Critical Facility in BARC, Trombay, Mumbai, India. Small samples (100–200 mg) were also analyzed by IM-NAA for comparison purpose. Radioactive assay was carried out using a 40 % relative efficiency HPGe detector. To examine homogeneity of the sample, counting was also carried out using X–Z rotary scanning unit. In situ relative detection efficiency was evaluated using gamma rays of the activation products in the irradiated sample in the energy range of 122–2,754 keV. Elemental concentration ratios with respect to Na of small size (100 mg mass) as well as large size (15 and 400 g) samples were used to check the homogeneity of the samples. Concentration ratios of 18 elements such as K, Sc, Cr, Mn, Fe, Co, Zn, As, Rb, Cs, La, Ce, Sm, Eu, Yb, Lu, Hf and Th with respect to Na (internal mono standard) were calculated using IM-NAA. Absolute concentrations were arrived at for both large and small samples using Na concentration, obtained from relative method of NAA. The percentage combined uncertainties at ±1 s confidence limit on the determined values were in the range of 3–9 %. Two IAEA reference materials SL-1 and SL-3 were analyzed by IM-NAA to evaluate accuracy of the method.

As a part of QA/QC of k 0-based internal monostandard neutron activation analysis (IM-NAA), three types of synthetic multielement standards (SMELS) were analyzed using pneumatic fast transfer system irradiation position of KAMINI reactor, IGCAR. Radioactive assay of activation products was carried out by high resolution gamma ray spectrometry. IM-NAA was used to determine relative concentration ratios of 22 elements with respect to gold internal monostandard. Absolute concentrations were calculated using assigned concentration of Au in all the types of SMELS. Z-score values within ±1 at 95.5 % confidence level and percentage deviations within ±5 % indicated good quality of the results by IM-NAA in most of the cases. Using this methodology, an ilmenite mineral sample was analyzed and concentrations of 14 elements were determined using Sc as monostandard.

Four kidney stones collected from patients being treated in the Advance Urology Centre of PGIMR, Chandigarh were characterized using instrumental neutron activation analysis (INAA), energy dispersive X-ray fluorescence (EDXRF) and X-ray diffraction (XRD) techniques. For INAA, samples were irradiated in tray rod facility of Dhruva reactor, Mumbai and pneumatic fast transfer system of KAMINI reactor, IGCAR, Kalpakkam. Radioactive assay was carried out using HPGe detector coupled to 8k channel analyzer. Elements determined in the samples by INAA are Zn, Sr, Co, Fe, Cr, Sc, Se, Na and Mn. EDXRF was used for the quantification of Ca. XRD patterns showed that three of the kidney stones are calcium oxalate stone and the other one is uric acid stone. The concentrations of trace elements in general were found to be higher in calcium oxalate stones and positive correlation was observed in the concentrations of Ca with Sr and Zn.

The k0-based internal monostandard instrumental neutron activation analysis (IM-INAA) method was applied for quantification of trace impurities in seven high purity aluminum samples used as fuel cladding in a research reactor. Samples along with BCS CRM 182 (Si–Al alloy) were irradiated in high flux reactor neutrons for 10–15 h. In situ detection efficiency, needed in concentration calculation ratio by IM-INAA, was obtained using gamma rays of activation products produced in the samples. Elemental concentration ratios obtained with respect to Fe (used as internal monostandard) were converted to absolute concentrations by determining concentration of Fe by relative method of NAA. Concentrations of ten trace elements (Sc, Cr, Co, Zn, Ga, La, Ce, Sm, W and Hf) including major element Fe were determined in this work. The method used is non-destructive in nature and does not need multielement standards. Results of IM-INAA were compared with those obtained by relative method of INAA and inductively coupled plasma atomic emission spectrometry (ICP-AES). Details of methodologies and results obtained by all methods are discussed and compared in the paper.

Present studies deal with supported liquid membrane (SLM) technique for the separation of thorium from hydrochloric acid (HCl) medium using Cyanex 923 as a carrier. Effects of feed acidity, strippant, and membrane pore size and membrane thickness on the transport of thorium have been studied in detail. The optimized parameters were applied for separation of thorium from a radioanalytical waste. Stability of the membrane and membrane support was investigated. Transport of thorium increased from 78.3 to about 93.7 % with increase in acidity from 0.5 to 2 M using 0.3 M Cyanex 923 in n-dodecane as carrier and 2 M ammonium carbonate as stripping phase. The transport of thorium decreased above 2 M HCl. An attempt was made to model the physicochemical transport of thorium in SLM and understand the mechanism of thorium transport.

An epithermal instrumental neutron activation analysis (EINAA) method using cadmium filter was standardized to determine trace concentrations of thorium in four samples of uranium oxide (U3O8) samples. Samples and thorium standards, wrapped with cadmium foil, were irradiated at a reactor neutron flux of about 1012 cm−2 s−1. Radioactive assay was carried out using a Compton suppressed anticoincidence gamma ray spectrometer consisting of HPGe-BGO detectors coupled to MCA. Concentrations of thorium in these samples were found to be in the range of 15–72 mg kg−1. EINAA results were validated by determining thorium concentrations in uranium matrix by standard addition method. EINAA results were compared with those obtained by two wet chemical methods namely ion chromatography (IC) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The results obtained by the three methods were found to be in good agreement, indicating further validity of the proposed EINAA method.

The green algae Chlorella (Chlorella pyrenoidosa) have the ability to bind high amounts of uranium(VI) in the pH range from 3 to 6. At pH 3 up to 20 % of the uranium is bound by the algal cells whereas the uranium removal by algal cell is almost complete at pH 5 and 6 in the concentration range of 4 × 10−4 to 1.6 × 10−3 M. Sorption capacities are in the range of 300–350 mg g−1 and 250–280 mg g−1 for fresh water and seawater respectively. Concentration of uranium was measured by inductively coupled plasma optical emission spectroscopy (ICP-OES) by using two different emission spectral lines at 409.014 and 424.167 nm. Environmental scanning electron microscopy (ESEM) complimented with energy dispersive X-ray (EDX) is used to characterize the binding sites of uranyl species on algal cell in the selected pH range. The micrographs show a regular distribution of U(VI) on the cell surface. Attenuated total reflectance-fourier transform infrared (ATRFTIR) spectrum of Chlorella indicates that the binding of U(VI) either to phosphodiesters (P–O–aryl/P–O–alkyl), and combination of amine, secondary amine and imine = NH respectively. These sites in Chlorella groups are mainly responsible for the removal and binding of U(VI) by formation of organic and/or inorganic uranyl phosphates.

In an attempt to evaluate radiation stability of several polymeric materials used as the support in supported liquid membrane studies for the transport of radionuclides from nuclear waste, flat sheets made from polytetrafluoroethylene, polysulfone, polyether sulfone, polyacrylonitrile and polyvinylidenefluoride were irradiated to varying extents using a 60Co gamma ray source and subsequently, the transport efficiency of the irradiated flat sheets were evaluated. The membrane integrity was assessed from the transport rates of Am3+ from a feed containing 3 M HNO3 into a receiver phase containing 0.01 M HNO3 as the strippant while 0.1 M TODGA (N,N,N′,N′-tetraoctyldiglycolamide) + 0.5 M DHOA (di-n-hexyloctanamide) in n-dodecane was used as the carrier extractant. The radiation stability of the membrane filters was evaluated after irradiating them up to 20 MRad absorbed dose in a gamma chamber.

The Fourth International Symposium on Nuclear Analytical Chemistry (NAC-IV) was organized at the Bhabha Atomic Research Centre (BARC), Department of Atomic Energy, Mumbai, India during November 15–19, 2010. NAC-IV was held in India for the first time. Previous three NAC symposia (NAC I-III) were held in Canada; Halifax (1985), Toronto (1992) and Halifax (2001). These symposia are organized periodically to provide a forum to exchange information on recent developments and applications of nuclear analytical chemistry. The NAC-IV symposium was sponsored by the Board of Research in Nuclear Sciences (BRNS), Department of Atomic Energy (DAE), India, and co-organized by the Indian Association of Nuclear Chemists and Allied Scientists (IANCAS). About 300 delegates from various units of DAE & Academic Institutes in India and 27 overseas delegates from 13 different countries participated in NAC-IV. Dr. Srikumar Banerjee, then Chairman of the Atomic Energy Commission (AEC) and Secretary, DAE, Government of India, inaugurated NAC-IV and Dr. R. K. Sinha, Chairman, AEC (then Direcor, BARC) presided over the inaugural session. Dr. Banerjee in his keynote address spoke about some interesting applications of analytical techniques in general and the role of nuclear analytical techniques (NATs) in particular in both R&D and nuclear reactor technology. Dr. Sinha emphasized the role of different NATs including neutron activation analysis (NAA) and prompt gamma ray NAA (PGNAA) in various programs of BARC and DAE, and also gave a brief account of the nuclear analytical facilities at BARC. Dr. Banerjee released the Book of Abstracts of NAC-IV and Dr. Sinha released the IANCAS Special Bulletin. Dr. A. V. R. Reddy, Head, Analytical Chemistry Division, BARC, and Convener, organizing Committee and Co-Chairman of the NAC-IV Technical Committee welcomed the delegates and outlined the theme of NAC-IV. Dr. V. Venugopal, Chairman of NAC-IV and then Director, Radiochemistry and Isotopes (RC&I) Group, BARC, emphasized that NATs using reactor and accelerator facilities were very important to obtain results with high precision and accuracy. Prof. A. Chatt of Dalhousie University, Canada, President of the NAC symposia series as well as the Co-Chairman of the NAC-IV Technical Committee, gave a brief account of the main objectives of these symposia. He informed that the Journal of Radioanalytical and Nuclear Chemistry (JRNC), has agreed to publish the peer-reviewed full papers of NAC-IV in two issues of JRNC. Dr. R. Acharya, RCD, BARC and Secretary of NAC-IV proposed a vote of thanks. The scope of NAC-IV included conventional and prompt gamma-ray activation analysis, alpha, X-ray & gamma-ray spectrometry, nuclear analytical chemistry in nuclear fuel cycle, nuclear track techniques, nuclear probes and ion beam analysis techniques, radioisotope tracer methodologies, speciation studies, QA/QC in measurements, applications of NATs to archaeological, biological, environmental, geological, industrial, nutritional, nuclear and pharmaceutical materials, nuclear forensics and safety studies. The technical program consisted of 30 invited talks A. V. R. Reddy Analytical Chemistry Division, BARC, Trombay, Mumbai 400 085, India e-mail: avreddy@barc.gov.in

In case of natural catastrophic nuclear accident scenario like Daiichi Nuclear Power Plant (NPP) Fukushima, Japan (11 March 2011) and industrial nuclear accidents like Chernobyl, USSR (March 1986), thousands of curies of activity goes in the public domain and contaminate the drinking water system in the area around the accidental zone. In view of this there is a need to evolve methodology for decontamination of the drinking water without compromising the drinking water quality. During this work humic coated colloidal suspension of geothite(α-FeO(OH)) followed by ultrafiltration were used to decontaminate the water having 239+240Pu and 241Am in the concentration range of 10–100 Bq L−1. Polydispersive colloids of goethite were generated by controlled oxidation of FeSO4 in the presence of NaOH. Size characterization, morphology and elemental profiling of goethite suspension and their aggregation with increase in the concentration of humic acid was studied by using dynamic light scattering and scanning electron microscope hyphenated with energy dispersive spectrometry. Experimental results clearly indicate preferential association of Pu and Am with goethite suspension dominated with 30 nm colloids. The impact of humus material on selectivity of Pu and Am by goethite was studied in the concentration range of 10–100 μg mL−1 of humic acid. This selectivity is further enhanced linearly with the increase in concentration humic acid from 10 to 60 μg mL−1 and thereafter it remains constant. Goethite suspension having a coating of 60 μg mL−1 of humic acid was successfully utilized to decontaminate the water. Goethite suspension was separated from the groundwater using Ultra filtration cell with membrane having 500 NMWL (nominal molecular weight limit).

Instrumental and preconcentration methods of neutron activation analysis (NAA) have been standardized for the determination of concentration of iodine in grass and cow milk samples, respectively. To study the transfer of iodine from grass to milk, known quantity of grass spiked with potassium iodide solution was fed to a cow. The spiked grass samples and milk samples, obtained from the cow after the ingestion of spiked grass, were collected. Iodine was separated from the milk samples chemically using Dowex 1X8 anion exchange resin. Spiked grass and ion exchange resin samples were neutron irradiated and radioactive assay was carried out using a 45 % relative efficiency HPGe detector coupled to an 8k channel analyzer. Iodine concentrations in spiked grass samples were found to be in the range of 1,487–2,002 mg kg−1. Concentration of iodine in milk after 12 h of feeding the cow with spiked grass was 871 ± 56 μg L−1 which was reduced to 334 ± 32 μg L−1 after 48 h.

Thorium along with its daughter products present in the soil is one of the major contributors to the external gamma dose in the environment. To establish the dose levels, quantification of thorium contents in soil samples is very important. As a part of pre-operational environmental radiological surveillance, a total of 23 soil and six sand samples were collected from different locations around the proposed nuclear power plant site of Jaitapur, Maharashtra. Thorium concentrations in these samples were determined by instrumental neutron activation analysis (INAA). Samples were irradiated with neutrons in Apsara reactor at a neutron flux of ~5 × 1011 cm−2 s−1 and radioactive assay was carried out using high resolution gamma ray spectrometry. Relative method of INAA was used for quantification of thorium utilizing 311.9 keV gamma ray of 233Pa, the daughter product of 233Th. The concentrations of thorium in the soil and sand samples were in the ranges of 4.0–18.8 and 1.2–6.2 mg kg−1 respectively.

The pneumatic fast transfer system position at KAMINI reactor, Indira Gandhi Centre for Atomic Research, India was characterized by determining the epithermal neutron flux shape factor (α) and the sub-cadmium to epithermal neutron flux ratio (f) for k 0-based Neutron Activation Analysis (k 0-NAA). For determination of α value, bare, Cd-ratio and Cd-cover methods were employed using dual and multi monitors namely Au, Zr and Zn. For calculation of f, Au and Zr monitors were used in the case of bare method and Au monitor was used for cadmium ratio and cadmium cover methods. The determined α-value of PFTS indicated a hard epithermal neutron spectrum and the f value indicated about 96 % thermal neutron component. For validation of k 0-NAA method, reference materials namely NIST SRM 1646a (Estuarine Sediment) and BCS Nb-stabilized Stainless Steel (BCS/SS No.261/1) were analyzed. The percentage errors of the determined concentration values of elements were within ±5 % with respect to the certified values and the Z-score values at 95 % confidence level were within ±2 in most of the cases.

The main objective of this work is the accurate measurement of uranium in the potable water sources of Muktsar district of Punjab, India. In the present work, a laser fluorimetry technique was used for the analysis of uranium. Inductively coupled plasma mass spectrometry (ICPMS) technique was also applied to verify and compare the uranium content analyzed using laser technique. About 16 samples from waterworks, bore wells, and hand pumps that supply the drinking water to local population were collected for this purpose. An indigenous laser fluorimeter supplied by RRCAT, Indore was employed for the analysis. Uranium concentrations obtained were in the range from 0 to 10 μg L−1 in ten samples, 11–30 μg L−1 in three samples, and more than 100 μg L−1 in three samples namely Channu ground water, Warning Khera pump, and Killanwale village hand pump. The USEPA guideline value for uranium in safe drinking water is 30 μg L−1. Also, a data comparison with similar studies carried out in other countries is presented.

Nickel contents in different finished product alloys were determined using a k0-based internal monostandard instrumental neutron activation analysis (IM-INAA) method. Five stainless steels (SS) and three high nickel alloys were analyzed by IM-INAA. BCS CRMs 225/1 (low alloy steel) and 466 (austenitic SS) and NIST SRM 247 (high Ni alloy) were analyzed to evaluate the accuracy of the method. The results of CRMs and SS were found to be in good agreement with certified or specified values. The Ni contents in the high nickel alloys were also determined by relative method of NAA for verification. Nickel contents in BCS CRM 466 and SS 316M were determined by UV–Visible spectrophotometry and the values were found to be in good agreement with IM-INAA results.

Downcore variation of trace metals in sediment cores along the coastal line is one of the markers to assess the intrusion of industrial pollutants into the aquatic environment. Fifty sediment core samples from the Mumbai Harbour Bay (MHB), were studied for the trace element content. MHB is a recipient of effluents from different industries situated all along its coast around Thane–Belapur region. The average concentrations of Titanium (Ti), Manganese (Mn), Iron (Fe), Nickel (Ni), Copper (Cu), Zinc (Zn) were determined by inductively coupled plasma-optical emission spectroscopy and complemented by analysing with energy dispersive X-ray fluorescence spectrometry. In addition to this, depth profiles of K and Ca were also studied to assess the homogeneity of the geological strata of the region. Trace metals such as Cu, Ni and Zn show enrichment between 16 to 28 cm, whereas, uniform distribution through out the core was observed for K, Ca, Ti, Mn and Fe. Chronology of the heavy metal deposition was predicated based on the average sedimentation rate (0.92 ± 0.08 cm year−1) derived using depth-wise 137Cs concentration profile in core of bottom sediment. The results of the analysis showed that MHB had received excess inputs of Cu, Ni and Zn in the year 1981, 1988 and 1982, respectively. Surface concentration of Cu, Ni, Zn and Fe compared to the reference site indicates moderate pollution in the recent years whereas for elements K, Ca, Ti and Mn, the values are normal indicating MHB unpolluted for the latter elements.

In northern part of Indian sub-continent, As related environmental and health issues receive attention from all over the world. Forty-eight sediment samples were collected from the Ganga Alluvial Plain (GAP) and its weathering products (from the Gomati River) for the study of As distribution and mobilization. These sediment samples were analyzed by Instrumental Neutron Activation Analysis (INAA) method using Cirus Research Reacter of Bhabha Atomic Research Centre, Mumbai. Average As concentrations in the GAP sediments (10.44 mg kg−1), the Gomati River bed sediments (1.36 mg kg−1) and the Gomati River suspended sediments (5.30 mg kg−1) were reported. Significant decrease of As content from the alluvial sediments to the river sediments is a clear indication of its mobilization by chemical weathering processes of mineral biotite. Present study demonstrates the importance of INAA for quantification and mobilization of As and improves our understanding related to As related environmental issues in northern India and elsewhere.

Three commonly used medicinal plants, e.g., Adhatoda vasica, Cassia fistula, and Withania somnifera grown in two contrasting environmental conditions, namely from copper mining site and from control site corresponding to soil not contaminated with Cu, to understand correlations between high Cu bioaccumulation in medicinal plants on their antioxidant activities. Concentrations of some essential metals, e.g., Cr, Mn, Fe, Cu, Zn, and Se in the leaves of these plants were measured by instrumental neutron activation analysis. The Cu levels in the samples from mining site were in the range of 32.6 to 57.2 mg/kg, which were 5–7 folds higher than the control samples, while Cr levels were about 2-folds higher in the mining site. Speciation studies of Cr revealed negligible content of toxic hexavalent Cr. Antioxidant assay of these plants from both the sampling sites, measured as total phenolic content, total flavonoid content, 2,2′-diphenyl-1-picrylhydrazyl, free radical scavenging ability, and chelating ability with ferrous ions exhibited maximum activity for A. vasica, while that of W. somnifera was minimum. However, the variations in the antioxidant activities for each medicinal plant species from mining site and control site did not reveal significant differences.

Kidney stones obtained from six patients belonging to the stone belt region of India (Punjab) were analyzed for inorganic constituents using instrumental neutron activation analysis (INAA) and energy dispersive X-ray fluorescence (EDXRF) techniques. For INAA, samples were irradiated along with IAEA RM Soil 7 as reference standard in CIRUS reactor, BARC, Mumbai. Gamma activity of irradiated samples was measured using a 45% relative efficiency HPGe detector coupled to 8 k channel analyzer. EDXRF method was used for determination of concentration of Ca. The concentrations of ten elements namely Ca, Na, K, Mn, Co, Cr, Zn, Br, Sm and Cl, are reported and discussed.

The present work describes the application of radiotracer technique for studying uptake of arsenic on titanium hydroxide, commercial titanium dioxide (TiO2) powder (anatase) and synthesized mesoporous titania beads in acidic, neutral, and alkaline conditions. Sol–gel templating method was used to prepare titania–polysaccharide composites, with different polymer contents. Mesoporous titania was obtained by heat treatment of the composite beads in a controlled environment. The synthesis process was optimized, using thermogravimetry analysis. X-ray diffraction patterns confirmed the formation of anatase pure phase titania (TiO2) at 700 °C in different environments, and scanning electron microscopy studies confirmed uniform pore size distribution. The effect of surface area, polymer content and pH on uptake of arsenic(III) and (V) on the synthesized titania beads was also investigated. Arsenic(V) was found to be retained quantitatively on the titania beads synthesized from 0.8% polymer content titania–polymer composite precursor in neutral to alkaline conditions. Details of the results obtained are discussed.

The intake of leafy vegetables in daily diet is very important to meet our nutritional needs. Vegetables provide the essential elements which are necessary and recommended for human growth. However, due to rapid industrialization and urbanization our environment becomes polluted and this affects the normal growth of agricultural products and composition of environmental species. The elemental concentrations present in the environmental samples are good indicators to assess the toxicological levels due to pollution affects. In the present work we have analysed several vegetable plant samples by instrumental neutron activation analysis to determine the elemental concentrations at major, minor and trace levels. The leafy vegetables like spinach, red leafy veagetable, pui, gourd leaf, lettuce and katoua were chosen as these are extensively consumed by local peple in eastern part of India. We have determined 15 elements in the above mentioned vegetable samples and some of these are essential elements and some are toxic elements. It was found that Na and K were present as major elements, Fe and Zn as minor elements and As, Ce, Cr, Co, La, Mo, Rb, Sc, Sm, Sr as trace elements. The concentration level of Cr was found to be higher than that of recommended value certified by WHO and National environment quality control for human consumption. The validation of our analytical results have been performed by the Z-score tests through the determination of concentrations of the elements of interest in certified reference materials.

Large sample neutron activation analysis of dross from India Government Mint, Mumbai was carried out for quantification of gold (Au) and silver (Ag) using graphite reflector position of Advanced Heavy Water Reactor critical facility at Bhabha Atomic Research Centre, Mumbai. The k 0-based internal monostandard NAA was used to calculate concentration ratios of Au and Ag with respect to sodium (Na), which was used as an internal monostandard. The concentration ratio values of Au to Na of varying mass of dross showed that mass ≥2 g was the representative sample size for analysis. Concentrations of gold and silver were found to be in the range of 200–400 and 1200–1700 mg kg−1, respectively in three different samples.

Direct determination of uranium in the concentration range of 8 μg L−1 to mg L−1 in water samples originating from different geochemical environments has been done using Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). Uranium detection with 2–3% RSD (relative standard deviation) has been achieved in water samples by optimizing the plasma power, argon and sheath gas flow. These parameters were optimized for three different emission lines of uranium at 385.958, 409.014 and 424.167 nm. Interference arising due to the variation in concentration of bicarbonate, sodium chloride, calcium chloride, Fe and dissolved organic carbon (DOC) on the determination of uranium in water samples was also cheeked as these are the elements which vary as per the prevailing geochemical environment in groundwater samples. The concentration of NaHCO3, CaCl2 and NaCl in water was varied in the range 0.5–2.0%; whereas Fe ranged between 1 and 10 μg mL−1 and DOC between 0.1–1%. No marked interference in quantitative determination of uranium was observed due to elevated level of NaHCO3, CaCl2 and NaCl and Fe and DOC in groundwater samples. Concentration of uranium was also determined by other techniques like adsorptive striping voltametry (AdSv); laser fluorimetry and alpha spectrometry. Results indicate distinct advantage for uranium determination by ICP-OES compare to other techniques.

Nuclear and commercial grade graphite samples were analysed by instrumental neutron activation analysis (INAA) using high flux reactor neutrons. Eleven elements (Na, K, As, Sc, Fe, Cr, Co, Zn, La, Ce, and Sm) were determined in eight samples of graphite (two nuclear grade and six commercial grade) by irradiating at a neutron flux of 3 × 1013 cm−2 s−1 in CIRUS reactor and assaying the activity by high-resolution gamma ray spectrometry using 40% relative efficiency HPGe detector coupled to an MCA. Concentrations of elements were determined by relative method of INAA. Results of both types of graphites as well as detection limits achieved by INAA method are discussed in the paper.

The k 0 based internal monostandard neutron activation analysis was used to analyze 41 ancient pottery samples from three major locations of Andhra Pradesh state, India, belonging to two different age groups namely Megalithic and Buddhist periods. Samples were irradiated with neutron flux obtained from CIRUS reactor and radioactive assay was carried out using a 40% relative efficiency HPGe detector coupled to 8 k MCA. Concentration ratios of 21 elements were calculated with respect to internal monostandard Sc. Absolute concentrations for six (three each from both Megalithic and Buddhist periods) representative samples along with a modern pottery were obtained for comparison. Elemental concentration ratios with respect to Sc were used for grouping of these archaeological samples. Preliminary grouping of these artifacts was done using La/Ce values, and the grouping was confirmed by statistical cluster analysis using eleven selected trace elements. The IAEA RM SL-3 sample was analysed for validation of the method, where in both concentration ratios and absolute concentrations were calculated.

During this work highly particle reactive nature of thorium was exploited for the separation of Th from aquatic stream containing U/Th. The Kd value of Th(IV) ions is 106 which is two order of magnitude higher than uranium (IV & VI). Laboratory simulated experiments were conducted to study the preferential removal of thorium by using siliceous material having particle size of about 2,000 μm. Siliceous material was prepared by decomposing the organic layer on soil particles by giving treatment with HNO3 and H2O2. Experimental solutions were generated by spiking the surface water with Th (NO3)4 and UO2(NO3)2. Experimental results shows preferential uptake of Th compared to U by siliceous material. This association is further improved by coating the siliceous material with high and low molecular weight organic materials i.e. humic and fulvic acid, respectively. Characterization of the organic material was done by ATR–FTIR whereas determination of Th was done by ICP-OES and alpha spectrometry. Experimental results clearly showed that Th and U sorption capacity is 1 and 0.3 μg mg−1 (w/w), respectively, in case of siliceous material. Thorium sorption is increased five and eight times in the case of coating with fulvic acid and humic acid, respectively. Whereas the same does not shows any pronounced impact on sorption of uranium.

During this work selective separation of uranium from rock phosphate and columbite mineral was done before its quantitative estimation by using Inductively Coupled Plasma Optical Emission Spectrometery (ICP-OES). Uranium from the rock phosphate and columubite was extracted by sodium peroxide fusion followed by leaching in 2 M HNO3. To avoid spectral interference in the estimation of uranium by ICP-OES, the selective separation of uranium from the leachate was carried out by using two different extractants, 30% Tributyl Phophates (TBP) in CCl4 and a equi-volume mixture of Di(2-ethylhexyl) phosphoric acid (D2EHPA) & TBP in petrofin. Uranium was stripped from the organic phase by using 1 M ammonium carbonate solution. Determination of uranium by ICP-OES was done after dissolving the residue left after evaporation of ammonium carbonate solution in 4% HNO3. The concentration of the uranium observed in the rock phosphates samples was 40–200 μg g−1 whereas in columbite samples the concentration range was 100–600 μg g−1. Uranium concentration evaluated by ICP-OES was complimented by gamma & alpha spectrometry. Concentration of uranium evaluated by gamma spectrometry in case of rock phosphate and coulmbite was in close agreement with the uranium content obtained by ICP-OES. Uranium determination by alpha spectrometry showed only minor deviation (1–2%) from the results obtained by ICP-OES in case of rock phosphates whereas in case of coulmbites results are off by 20–30%.

The k 0-based internal monostandard neutron activation analysis (IM-NAA) method was used for the analysis of 30 large and non-standard geometry ancient pottery samples obtained from Buddhist sites of Andhra Pradesh, India. One freshly finished pottery and a sun-drenched pottery were also analyzed for comparison. Samples were irradiated in thermal column facility of Apsara reactor and also in graphite reflector position of critical facility of Bhabha Atomic Research Centre. Radioactive assay was carried out using a 40% relative efficiency HPGe detector coupled to MCA. Concentration ratios of 15 elements with respect to Sc were determined. The La/Ce values as well as statistical cluster analysis utilizing concentration ratios of elements were used for grouping/provenance of the potteries.

For standardization of k 0-based instrumental neutron activation analysis, k 0-factors for short-lived nuclides (half-lives—11 s to 37 min) of elements F, Se, Sc, Al, V, Ti, Cu, Ca, Mg, I, and Cl with respect to gold (197Au) were determined using pneumatic carrier facility (PCF) at CIRUS reactor of BARC, Mumbai. Characterization of PCF was carried out by cadmium-ratio method using Au and Zr. The experimental k 0-factors of the isotopes were found to be in good agreement with the recommended k 0-factors in most of the cases, as evident from the values of % error and U-score at 95% confidence level. The method was validated by determining concentrations of elements through their short-lived nuclides in one type of the synthetic multielement standards (SMELS-I) obtained from SCK-CEN, Belgium. The method was also applied for determination of concentrations of some of the elements in two reference materials of IAEA, SL-3, and SL-1.

Mobilisation of alpha emitting radionuclides from silicious base sample is one the challenging task for environmental radiochemist. During this study, rapid and complete dissolution of the siliceous base samples were carried out by optimizing temperature, pressure and power of the microwaves. The Pu-239+240 in digested samples was pre-concentrated by scavenging Fe as Fe(OH)3. Pu-239+240 was isolated from the Fe(OH)3 by co-precipitating Pu with Bi(PO4) in HNO3 medium at pH 2. Pu-239+240 was separated from Bi(PO4) and other transuranics by passing through cation and anion exchange resin. Pu-239+240 was counted by alpha spectrometry after electroplating on stainless steel planchet. The detection limits achieved for Pu-239+240 was 60 μBq/g (2.6 × 10−14 g/g). Pu-242 was used as a tracer for the evaluation of recovery of Pu-239+240. Samples prepared after complete destruction of matrix in microwave, showed 10–20% higher concentration of Pu-239+240 compared to conventional acid leached. Consistent recovery in the range of 97–99% for Pu-242 were observed in microwave digested samples whereas inconsistent results were observed in acid leached samples where the recoveries were in the range of 75–86%. Siliceous matrix degradation was tracked by monitoring the surface morphology and composition of the residue left at various stages of digestion using Scanning Electron Microscope (SEM) coupled with Energy dispersive X-ray spectrometer (EDS).

In the Nawanshahr–Hoshiarpur region of Punjab, India, more than 1000 hectares of agricultural land is significantly affected by high levels of selenium (Se). Studies were carried out to examine Se levels in soil and crops such as wheat grains, wheat husk, rice, maize and mustard using neutron activation analysis. The Se concentrations in soil and crop products were found to be ranging from 2.7 to 6.5 mg kg−1 and 13 to 670 mg kg−1, respectively, indicating significantly high selenium in these crop products. Two reference materials were analysed for Se contents by INAA as controls.

Brahmi (Bacopa monnieri) leaves, known as nervine tonic in Ayurveda, and its aqueous (BA), methanolic (BM) and aqueous–methanolic (BAM) extracts were analyzed for 7 minor (Al, Fe, Na, K, Ca, P, Cl) and 18 trace (As, Au, Ba, Br, Co, Cr, Cu, Hf, Hg, La, Mn, Rb, Se, Sm, Sr, Th, V, Zn) elements by INAA. BAM extract showed maximum contents of Na, K, Cl and significant amounts of Mn, Co, Zn. It was also found as effective scavenger of DPPH radicals with 33.5% total phenolic content, highest γ-ray radioprotective effect and higher anti lipid peroxidation activity.

Ground water samples obtained from West Bengal, India were analyzed for total arsenic and its inorganic species contents by instrumental neutron activation analysis (INAA). Two anion exchange separation methods using Dowex 1X8 in chloride and acetate forms were standardized for the speciation of As(III) and As(V) using radiotracers. The method by Dowex 1X8 in the acetate form was validated using synthetic mixtures of As(III) and As(V), and applied to water samples; the species concentrations were determined by INAA. The accuracy of the INAA method was evaluated by analyzing the NRCC CRM DORM-2 for total arsenic.

Laboratory simulated experiments have been conducted to study the association of 239,240Pu with pseudo-colloids of iron in groundwater samples having dissolved organic carbon (DOC) in the range of 10–60 mg L−1. Ultra-filtration membranes have been used to partition colloidal components into seven different size range of

Studies on bioaccessibility of elements were carried out by in-vitro gastrointestinal digestion simulation method combined with neutron activation analysis (NAA) using NH4HCO3 as an alternate base to commonly used base of NaHCO3. The effect of two bases namely NaHCO3 and NH4HCO3 on the bioaccessibility of the elements namely Br, Fe, K, La, Na, Rb, Sm and Zn from wheat seeds, fresh wheatgrass and commercial wheatgrass tablet was investigated. The bioaccessible concentrations of the elements were determined by neutron activation analysis (NAA). The bioaccessible concentrations of samples digested using NH4HCO3 were found to be higher by 10–15% for most of the elements than that observed using NaHCO3. In the case of fresh wheatgrass, the differences were as high as 50%. The present study indicated that NH4HCO3 can be used as a base instead of NaHCO3 in in-vitro gastrointestinal digestion simulation method.

A non-destructive assay technique based on prompt gamma-ray neutron activation analysis for the determination of 238U to 232Th ratio in the mixed oxide fuel materials has been established. The method uses closely spaced high energy gamma-rays in the region of 4000 keV to 4150 keV enabling it to be applied for samples of any geometry and thickness without having any correction for gamma-ray attenuations and detection efficiencies.

A summary of k0-based R&D work on neutron activation analysis (NAA), internal mono standard NAA (IM-NAA) and prompt gamma-ray NAA (PGNAA) is presented. The k0-based NAA was standardized by characterizing irradiation sites of research reactors, validated using reference materials and applied to samples of different origin. Recently IM-NAA method was developed, validated for small and large size samples and applied for the analysis of large size as well as non-standard geometry samples. Studies on PGNAA included characterization of neutron beam, determinations of detection efficiency and prompt k0-factors, and analytical applications.

Four plant parts (leaves, roots, fruits and seeds) of twenty samples of sixteen antidiabetic herbs including three commercially marketed capsules have been analyzed for 6 minor (Na, K, Ca, Cl, Mg, and P) and 21 trace (As, Ba, Br, Ce, Co, Cr, Cs, Cu, Eu, Fe, Hg, La, Mn, Rb, Sb, Sc, Se, Sm, Th, V and Zn) elements by instrumental neutron activation analysis (INAA). Further, Ni, Cd and Pb contents were determined by AAS. Elemental data were validated by simultaneously analyzing reference material (RM), MPH-2 Mixed Polish Herbs. Several elements such as Cr and V (1–2 μg/g), Rb (10–40 μg/g), Cs (80–300 ng/g), Se (∼100 ng/g) and Zn (25–60 μg/g) play an important role in diabetes mellitus. Interelemental linear correlations have been observed for Cu vs. Zn (r = 0.89) and Rb vs. Cs (r = 0.87). K/P ratio varies in a narrow range with a mean value of 6.2 ± 1.4. Toxic elements As and Hg were found in