Expanded uncertainties of preconcentration neutron activation measurements of extractable organo-chlorine,bromine and iodine compounds in bovine milk lipids

Milk is known to contain organohalogen compounds. A mixture of hexane and isopropanol was used to extract lipids from bovine milk and neutron activation analysis (NAA) was employed to measure extractable organohalogens in the lipids. The samples were irradiated in a neutron flux of 2.5 × 10¹¹ cm² s^?1 for 10 min, allowed to decay for 2 min, and counted for 10 min. Uncertainties associated with the preconcentration NAA measurements were investigated in detail. The mass fractions of halogens in mg kg^?1 and their relative expanded uncertainties in percent in bovine milk lipids were: 32 (8.4 %), 2.65 (9.8 %) and 0.211 (6.6 %) for Cl, Br and I, respectively.     

Complexation of Eu3+ with cone conformers of three substituted calix[4]arenes in nitrobenzene saturated with water

From extraction experiments and $ \gamma Accurate knowledge of the trace elemental concentrations in wheat and its products is of great importance from a nutritional point of view. In this study, six wheat samples were prepared from the agriculture research center of Arak named Sardari, Amir, MV-17, Batava, Karaj-2 and Alvand; they were analyzed by neutron activation method (NAA). In this method, Isfahan miniature reactor as a neutron source and relative NAA method has been used as the analysis type. In this design in order to record gamma spectrum the MCA system and high purity germanium detector were used. Finally, the concentration of the trace elements such as Br, K and Na value was determined for the Sardari, Amir, Alvand, MV-17, Batava, Karaj-2 wheat samples. The average concentration of trace elements in all wheat samples in the studied area are 2.41(0.8597?6.1175) mg kg^?1 for Br, 13.42(8.7063?24.696) mg kg^?1 for Na and 463.30(434.22?505.45) mg kg^?1 for K, respectively. These were compared with other reports results. This study has been conducted as the first time for this region.     

Large sample neutron activation analysis of dross for gold and silver

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.     

Selenium content of Argentinean infant formulae and baby foods by pseudo-cyclic instrumental neutron activation analysis coupled to Compton suppression

The selenium levels of Argentinean infant formulae and baby food were measured using the 162-keV gamma-ray of ^77mSe (t _½ = 17.4 s) by a pseudo-cyclic instrumental neutron activation analysis (PC-INAA) method in conjunction with Compton suppression spectrometry (CSS). For comparison purposes, 5 selected infant formulae were also analyzed for selenium by a radiochemical neutron activation analysis (RNAA) method. The selenium levels for three samples agreed between ±2.8 and 6.5 % while the other two differed by 12 and 17 % which could perhaps be attributed to sample inhomogeneity. The selenium content of cow milk-based infant formulae varied from 42–146 μg kg^?1 compared to 52–63 μg kg^?1 for soy-based milk formulae. In the case of baby foods, the selenium levels varied from 34 to 74 μg kg^?1. The detection limits for selenium by PC-INAA–CSS for all the samples analyzed in this work were between 8.5 and 65 μg kg^?1 depending on the major elements present in the samples, while it was 20 μg kg^?1 for the RNAA method. The expanded uncertainty (κ = 2) of the PC-INAA–CSS method was 7.0 % at the end of cycle #4 for a sample containing 73.7 μg kg^?1 selenium compared to the RNAA value of 24.2 % for a sample of 67.0 μg kg^?1 selenium content.     

Comparison of Different Analytical Techniques for the Determination of Organic Mercury

Abstract

Methods for the determination of (1) total organic mercury (Hg) using an extraction +neutron activation analysis, (2) the sum of methyl-Hg+phenyl-Hg using ¹³¹I^?-Cl^? exchange and (3) methyl-Hg using two different Westöö modifications, have been compared. Sample materials were 8 falcon livers, 5 pike livers and 2 pike muscles. Although differences were found between the methods, interaction effects caused by either sample inhomogeneity or bad performance of the analytical methods impeded a clear interpretation of the comparison. Total Hg in the samples was determined by neutron activation analysis (NAA) and atomic absorption spectrometry. The accuracy of the total Hg determination using NAA was verified by the analysis of certified reference material.

In addition to the other organic Hg determinations phenyl-Hg was determined separately in some of the samples by an isotope exchange method using ²⁰³Hg²⁺.

The main conclusion of the study was that there is a demand for reference materials certified for at least total organic Hg and methyl-Hg.     

New Developments in Activation Analysis for Material and Environmental Sciences

Activation analysis in general and mainly reactor neutron activation analysis (NAA) has been used extensively for measuring trace elements in high purity materials, particularly semiconductor materials. The advantages of NAA in determination of trace elements differ from one semiconductor material to another. For all of them the inherent properties of activation analysis especially those of non contamination with the reagents, low blanks and high sensitivity are the reasons for the choice of NAA as the main analytical procedure. These inherent properties are essential for analysis of high-purity materials where concentrations of ppb's and sub ppb's have to be measured. NAA is specially suitable for the determination of trace elements in silicon due to the very short lived very low activity induced by neutron reaction in silicon. This enables easy instrumental (i.e. without chemical separations) determination of trace elements in silicon. In the HFR reactor at Peten, Netherlands, a special facility was constructed for irradiation of silicon samples of Philips, in which silicon wafers of up to 15 cm diameter can be irradiated with 4 × 10¹³n. cm^?2. sec^?1 and the irradiation is done for 72–96 hours. using large Ge(Li) detectors (100 to 150cc) and long counting time (8–16 hours) they measured 22 elements in concentrations below ppb and 10 others between ppb and 300 ppm. Trace elements in germanium have been determined both instrumentally after very long decay time (100 days) or after short decay time removing the activities from the matrix by chemical separation. Trace elements in GaAs are determined only after chemical separtion. Several other semiconductor material such as Sc, Te, GaP and CuInS₂ were also determined by NAA. Some trace elements cannot be determined by neutron activation. Carbon, nitrogen and oxygen are determined by activation with protons, alphas or ³He particles. Boron and hydrogen are determined by prompt emission induced by charged particle activation, which gives not only the total concentration but also the depth profile. Carbon, nitrogen, oxygen and phosphorus were also determined by prompt proton activation analysis. The environmental samples studied by activation analysis can be divided into three categories: atmospheric aerosols, water samples and solid wastes. NAA of atmospheric aerosols have been used for their posible toxicological hazards, their source identification and for studies of atmospheric transport processes.     

Determination of 135Cs in nuclear power plant wastes by ICP-MS and k 0-NAA

A radiochemical method for the determination of ¹³⁵Cs in radioactive wastes has been adopted/developed. For the separation of cesium from other elements ammonium-molybdophosphate precipitation and cation exchange chromatography were used. The chemical yield of the method was about 60–100 %. ¹³⁵Cs was measured by two methods. In neutron activation analysis (NAA), Cs was irradiated with reactor neutrons. ¹³⁶Cs was detected by gamma spectrometry, wherefrom the activity/mass of ¹³⁵Cs was calculated according to the k ₀-standardization technique. The Cs containing fractions were measured by inductive coupled plasma mass spectrometry, as well. NAA and ICP-MS techniques were comparatively evaluated and a good agreement between the results was found. The activity concentration of ¹³⁵Cs in a couple of waste samples originating from VVER-440 type nuclear reactors was in the range of 1–5 Bq L^?1 (20–120 ng L^?1) while ¹³⁷Cs activity concentrations varied between 0.1 and 1 MBq L^?1.     

Determination of concentration of iodine in grass and cow milk by NAA methods using reactor neutrons

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?C2,002?mg?kg^?1. Concentration of iodine in milk after 12?h of feeding the cow with spiked grass was 871?±?56???g?L^?1 which was reduced to 334?±?32???g?L^?1 after 48?h.     

A new reflector structure for facility thermalizing D–T neutrons

A facility for thermalization of fast neutrons (14.2 MeV) emitted by compact deuterium–tritium (D–T) neutron generators (NGs) for thermal neutron activation analysis is proposed. Its final design is based on Monte Carlo calculations (MCNP5). To maximize the ratio between the thermal neutron flux and the total neutron flux and simultaneously to ensure the highest possible value of the thermal neutron flux at the output surface, the facility should consist of a two-layer reflector [tungsten (W)—the inner part, molybdenum—the outer part], a two-layer multiplier (W followed by lead), a moderator (polyethylene followed by magnesium fluoride) and a collimator (molybdenum and nickel near the output surface). For the D–T NG producing the maximum available neutron yield 10¹⁵ n s^?1, the facility provides the thermal neutron flux 2.0 × 10¹¹ n cm^?2 s ^?1 and a slightly higher fast neutron flux 2.3 × 10¹¹ n cm^?2 s^?1. To improve the ratio of the thermal neutron flux to the fast neutron flux (above 2.7) an addition of a silicon layer to the moderator and especially a proper adjustment and a threefold increase of the multiplier thickness is necessary.     

Rare earth element (REE) in surface mangrove sediment by instrumental neutron activation analysis

A study is carried out on the concentrations of rare earth element (REE) elements present in surface mangrove sediments from 10 locations throughout west coast Malaysia. In carrying out the analysis, the best and most convenient method being the instrumental neutron activation analysis (INAA). Samples were obtained, dried, crushed to powdery form and samples prepared for INAA. All the samples for analysis were weighted approximately 150 mg for short irradiation and 200 mg for long irradiation time. As calibration and quality control procedures, blank samples, standard reference material SL-1 were then irradiated with thermal neutron flux of 4 × 10¹² cm^?2 s^?1 at the MINT TRIGA Mark II research reactor which operated at 750 kW by using a pneumatic transport facility. The REE elements of surface sediment samples in this study are Dy, Sm, Eu,Yb, Lu, Tb, La and Ce. It was found that the level of concentrations of all the REE elements varies in the range (0.35–117.4 mg/kg). The geochemical behavior of REEs in surface sediments and normalized pattern (chondrite and shale) has been studied. The degree of sediments contaminations were computed using an enrichment factor. The results showed that the enrichment factor varied in the range (0.75–6.75).     

Design,construction and characterization of a prompt gamma activation analysis facility at the Oregon State University TRIGA<Superscript>®</Superscript> reactor

A prompt gamma neutron activation analysis facility has been designed, built, and characterized at the Oregon State University TRIGA^® reactor. This facility was designed for versatile multi-elemental analyses. The facility utilizes the leakage neutrons originating from beam port #4 of the Oregon State University TRIGA^® reactor. The neutrons are collimated through a series of lead and Boral^® collimators, and filtered through both a bismuth filter and single-crystal sapphire. Samples are irradiated in a sample chamber outside the biological shielding of the reactor, and the resulting gamma radiation produced from neutron interactions within the sample is monitored using a high-purity germanium detector (HPGe). The thermal and epithermal neutron fluxes were measured using gold-foil irradiations and found to be 2.81 × 10⁷ and 1.70 × 10⁴ cm^?2 s^?1, respectively. The resulting cadmium ratio was 106. Measured detection limits for boron, chlorine, and potassium in a NIST SRM 1571 orchard leaf were 5.6 × 10^?4 mg/g, 8.2 × 10^?2 mg/g, and 1.0 mg/g, respectively. Detection limits for additional elements and samples are presented.     

Analysis of bioaccessible concentration of trace elements in plant based edible materials by INAA and ICPMS methods

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).     

Application of INAA for phyto-accumulation study of selenium by chickpea plant

The phyto-accumulation efficacy of selenium (Se) from soil by chickpea plant is reported. Chickpea plants were grown in soil having different concentrations (1–4 mg kg^?1) of Se. Samples of soil and different parts of chickpea plants in Se rich soil were analyzed for determination of Se concentrations by instrumental neutron activation analysis (INAA). Samples were irradiated in self-serve facility of CIRUS reactor, BARC, Mumbai at a neutron flux of the order of 10¹³ cm^?2 s^?1. The gamma activity at 264.7 keV of ⁷⁵Se (119.8 d) was measured using a 45% relative efficiency HPGe detector coupled to MCA. Dependence of Se distribution in soil and plants on its spiking concentration was evaluated in this work. The Se concentrations determined in plant parts grown in control soil and in soil spiked with Se (4 mg kg^?1) are in the range of 0.6–0.8 and 65–68 mg kg^?1 respectively.     

Determination of aluminium contents in selected food samples by instrumental neutron activation analysis

Food and food products are the main sources of Aluminium entering the human body. In order to know aluminium contents in food and food products, selected 26 samples from local market were analyzed by instrumental neutron activation analysis (INAA) using reactor neutrons and high resolution gamma-ray spectrometry. INAA using 1,779 keV γ-ray of ²⁸Al (2.24 min) was used for aluminium concentrations in the range of 33–529 mg kg^?1. Two NIST standard reference materials (SRMs) and two IAEA reference materials (RMs) were analyzed by INAA for quantification of aluminium as a part of method validation.     

Moderator for neutron activation with the photoneutrons produced by a LINAC

Using Monte Carlo methods a polyethylene moderator has been designed to induce activation using the photoneutrons field of a 15 MV linear accelerator for radiotherapy. In the calculations the photoneutron spectrum at 1 m from the isocenter was used as a source term and the neutron spectra were calculated in the center of different size cylindrical moderators. The best size was selected defining the thermal-to-fast-neutron ratios as a figure of merit. The moderator was built and its performance was evaluated by inducing the activation of Mn dissolved in water, silver coins and souvenir coin. The thermal neutron fluence rate was determined with the Mn samples being 9.96 × 10⁵ cm^?2 Gy _x ^?1 .     

Applications of EDXRF and INAA techniques for studying impact of industries to the environment

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.     

Applications of k 0 NAA at FRM II with high f values

The research reactor FRM II offers different irradiation facilities with highly thermalized neutron flux. 3 facilities for the k ₀ neutron activation analysis (k ₀ NAA) will be introduced shortly. The influence of flux parameter α on the concentration calculation of samples irradiated in a neutron field with very high ratio of thermal to epi-thermal neutron flux f > 1,000 are here investigated. Even for the most k ₀ isotopes with big Q ₀ values, the uncertainty of a concentration calculation without α correction is <3 %, when the f value larger than 3,000. The uncertainty is about 5 % for the isotope ⁹⁶Zr in this case. The k ₀ library of the computer program MULTINAA is updated. A standard reference material IAEA/soil-7 was analyzed to verify the k ₀ NAA at FRM II.     

A pilot study to measure levels of selected elements in Thai foods by instrumental neutron activation analysis

A pilot study was carried out to evaluate the scope of instrumental neutron activation analysis (INAA) for measuring the levels of selected elements in a few commonly consumed food items in Thailand. Several varieties of rice, beans, aquatic food items, vegetables and soybean products were bought from major distribution centers in Bangkok, Thailand. Samples were prepared according to the protocols prescribed by the nutritionist for food compositional analysis. Levels of As, Br, Ca, Cd, Cl, Cr, Cu, Fe, K, Mg, Mn, and Zn were measured by INAA using the irradiation and counting facilities available at the Thai Research Reactor with the maximum in-core thermal neutron flux of 3 × 10¹³ cm^?2 s^?1 of the Thailand Institute of Nuclear Technology in Bangkok. Selenium was determined by cyclic INAA using the Dalhousie University SLOWPOKE-2 Reactor facilities in Halifax, Canada at a thermal neutron flux of 2.5 × 10¹¹ cm^?2 s^?1. Both cooked and uncooked foods were analyzed. The elemental composition of food products was found to depend significantly on the raw material as well as the preparation technique.     

Enhanced electrochemical performance of straw-based porous carbon fibers for supercapacitor

The efficient utilization of natural biomass as renewable raw materials is of importance. We herein prepared porous carbon fibers (PCFs) by activation of the extracted cellulose microfibers from the agriculture byproduct of corn straw. Different from the porous carbons (PCs) by directly activating straw, the obtained PCFs had typical one-dimensional morphology with high surface area (2013 m² g^?1) and large pore volume (1.27 cm³ g^?1). The influence of the ZnCl₂/cellulose mass ratio on the electrochemical performance was studied, and the optimized PCF(1:1) possessed a much higher specific capacitance than the PC(1:1) sample, which was attributed to the improved specific surface area as well as the fiber-like morphology where it had short ion diffusion route and small interfacial resistance in comparison to PCs. PCFs have a high specific capacitance of 230 F g^?1 at 0.5 A g^?1, and 183 F g^?1 was retained at 20 A g^?1 (79.6%), revealing an excellent rate capability. The assembled symmetrical supercapacitor exhibited a wide potential window of 1.8 V, small electrochemical impedance, and superior cycle performance. Moreover, a high energy density of 16.0 Wh kg^?1 was obtained at a power density of 450.4 W kg^?1, which was preserved of 6.9 Wh kg^?1 at a high power density of 14,194.3 W kg^?1.     

Chemical characterization of graphite by instrumental neutron activation analysis

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.