Determination of trace concentration of boron in ADU by the nuclear track technique

A method for the determination of boron concentration in extracted (NH₄)₂ U₂O₇·H₂O (ADU) has been used. One ml of the aqueous solution is irradiated with thermal neutrons from a 10 Ci Am/Be neutron source with a flux of 0.2·10⁵ n·cm^–2·s^–1 and thermal column in the IRT-5000 with a flux of about 10⁷ n·cm^–2·s^–1. The alpha-activity due to the reaction¹⁰B(n, )⁷Li is recorded by a CR-39 alpha track detector. After the exposure, the alpha tracks are made visible in an optical microscope at magnification of 800X by etching the detector in 6N NaOH, and the track density is determined using calibration curves of known concentrations of boron. The boron concentration of the extracted ADU was found to be 5 ppm.     

Determination of boron in glass by alpha-spectrometry

Alpha-spectrometric method has been used for the determination of boron in borosilicate glasses. For irradiation thermal neutrons with a flux of about 10⁵ n·cm^–2·s^–1, produced in a paraffin moderator surrounding a deuteron target of a small neutron generator, were used. Alpha-particles from the reaction¹⁰B(n, ) were detected by a Si solid state detector with a resolution of about 50 keV. The sensitivity of the method is 0.05 wt % boron in glass samples.This work was supported by the Hungarian Research Foundation (Contract No. 1734/91.).     

Multi-element determination in silicate rocks by instrumental neutron activation analysis

Instrumental neutron activation analysis technique was applied for the determination of 20 elements in 54 silicate rock samples which belong to three sedimentary geological formations located in the western desert of Iraq. The samples along with USGS standards were irradiated in an IRT-5000 reactor at a neutron flux of 3.7·10¹³ n·cm^–2·s^–1 The following minor and trace element constituents have been determined: Na, K, Ca, Fe, Sc, Cr, Co, Zr, Ce, La, Nd, Sm, Eu, Tb, Yb, Lu, Hf, Ta, Th and U.     

Measurement of30Si as a tracer by neutron-induced prompt gamma-ray analysis

The application of stable isotope analysis using neutron-induced prompt -ray analysis (PGA) with cold/thermal neutron beams for the tracer study of geological materials are discussed. Silicon has three natural isotopes differing in abundance:²⁸Si (92.23%),²⁹Si (4.67%) and³⁰Si (3.10%). For the purpose of the assessment of Si migration in engineered barrier material, enriched³⁰Si can be used as a tracer due to its nuclear and chemical properties. Isotope analysis of³⁰Si was performed by PGA during the tracer study. Neutron intensity at the sample position was 1.4·10⁸ n¢cm^–2·s^–1, 2.4·10⁷ n·cm^–2·s^–1 for cold and themal neutron guided beams of JRR-3M, respectively. Calibration curves and analytical sensitivity of³⁰Si were determined based on measurement of standard samples. BG and detection limits for³⁰Si analysis were also measured in Japanese bentonite (Kunigel V1 and Kunipia F) and their pore water. Fiffteen elements were determined simultaneously using PGA.     

Determination of Si,Al, Ti,Fe and Zr in glass sand samples by 14 MeV neutron activation analysis

Fast neutron activation analysis technique was applied for the determination of Si, Al, Ti, Fe and Zr in glass sand rock samples. The samples and standards were irradiated with a mono-energetic neutron flux of 10⁸n · cm^– · s^–1. Pneumatic facility was used. The gamma activities from samples and standards were counted using a 30 cm³ Ge(Li) detector, with FWHM of 2.9 keV at 1.332 MeV, coupled to an on-line computer facility.     

Synthetic multielement standard samples for serial neutron activation analysis of biological materials

New synthetic standard samples (SSB-1 and SSB-2), produced on the basis of phenol-formaldehyde resin in the shape of tablets are suggested. The samples are intended for INAA of biological materials. SSB-1 and SSB-2 samples contain Se, Cr, Au, Sb, Ag, Rb, Fe, Zn, Co and Ca, Ba, Hg, Sn, Br, Cs, Ni, Sc and Na. The concentrations of these elements are chosen so that the maximum statistical error of -quantum registration by the semiconductor detector should not exceed 3% when irradiating samples in a neutron flux of 10¹³ n·cm^–2·s^–1.     

Elemental analysis in bed sediment samples of Karnafuli estuarine zone in the Bay of Bengal by instrumental neutron activation analysis

The concentration of rare earths and other elements have been determined in the bed sediment samples of Karnafuli estuarine zone in the Bay of Bengal by instrumental neutron activation analysis (INAA). The samples and the standards soil-5, soil-7, coal fly ash and pond sediment were prepared and simultaneously irradiated for short and long time at the TRIGA Mark-II research reactor facility of Atomic Energy Research Establishment, Savar, Dhaka. The maximum themal neutron flux was of the order of 10¹³ n·cm^–2·s^–1. After irradiation the radioactivity of the product nuclides was measured by using a high resolution high purity germanium detector system. Analysis of -ray spectra and quantitative analysis of the elemental concentration were done via the software GANAAS, it has been possible to determine the concentration level of 27 elements including the rare earths La, Ce, Sm, Eu, Tb, Dy and Yb and uranium and thorium.     

Determination of traces of uranium in tungsten and molybdenum by radiochemical neutron activation analysis via the fission product140Ba

A radiochemical separation procedure has been developed to determine traces of uranium in tungsten and molybdenum. In this procedure the fission product¹⁴⁰Ba, as indicator nuclide for uranium, is selectively separated from the matrix activities and from all other long-lived activation and fission products and obtained at high purity. The radionuclide in the final fraction is sufficiently pure so that it can be measured with high counting efficiency by -counting. The separation procedure consists of two steps: a cation-exchange separation to separate barium from the anionic matrix tungste or molybdate, and many other elements. In the second step the Ba-fraction is further purified by precipitation of barium as barium chloride in 8M hydrochloric acid. The precipitate is then dissolved in water for -counting via the Cerenkov effect. The chemical yield for barium is 94.6±2.6%. When samples of 0.1 g, a thermal neutron flux of 2·10¹³ n·cm^–2·s^–1, an irradiation time of 10 hours and a measuring time of 2 hours were applied, then the detection limit of uranium was 4 ng/g.Presented at the 3rd Intern. Conf. on Nuclear and Radiochemistry, Vienna, September 7–11, 1992.     

Neutron activation and radiochemical separation of selenium from environmental and food samples from and around Bombay using ethyl-α-isonitrosoacetoacetate

Neutron activation analysis has been applied for determination of selenium in environmental and food samples. Food and environmental samples from city, industrial and agricultural zones were collected with utmost care. Samples were activated in the flux 1·10¹³ n·cm^–2·s^–1 in the CIRUS reactor of BARC, Bombay, 75-Se was separated from 6.5N HCl solution using ethyl--isonitrosoacetoacetate (HEINA) reagent. The decontamination studies showed the method is very selective. Selenium contents of wheat, rice, vegetables, cereals pulses etc. and of soil, water, and deposits on plants and surface were determined by the procedure developed.     

Extraction and neutron activation analysis of humic substances

Methods are described for the isolation of humaic substances from a soil samples. The produres and based on extractions with sodium hydroxide or sodium pyrophosphate. Four of the humic samples were dried and then analysed by thermal neutron activation analysis. The humic samples along with three standard rocks were irradiated for 15 hours in a flux of 10¹² n·cm^–2·s^–1. Counting was carried out using both a large volume Ge(Li) detector and a high resolution LEP detertor. Quantitative analysis was based on the known element concentrations in the standard rocks. The elements determined were Sc, Cr, Fe, Co, As, Se, Br, Mo, Sb, La, Ce, Eu, Hf, Ta, Th, and U. concentrations ranged from 0.02 ppm (La) to 7900 ppm (Fe).     

INAA of trace impurities in aluminium clads

As a contribution to nondestructive neutron assay of reactor grade aluminium, a number of elements have been investigated qualitatively and quantiatively using a vertical channel in the IRT-5000 reactor with a thermal neutron flux of 7.6·10¹²n·cm^–2·s^–1. The -ray spectra of irradiated samples were analysed with a 30 cm³ Ge(Li) detector connected to an HP-computer and a 4096 channel analyser. The following impurities have been determined: Sc, Ca, Cr, Fe, Ni, Co, Zn, As, Sb, W, Au, Th and U, while Lu and Hf have been determined qualitatively only.     

Neutron activation analysis of low level lithium in water samples

For determining low level lithium concentrations in water, a neutron activation method based on the measurement of tritium radioactivity produced by⁶Li(n,)³H reaction has been developed. This method is specific and free from interference by other chemical elements. Using a low background liquid scintillation counter for tritium measurement, the detection limit is approximately 0.3 ppm during irradiation at a thermal neutron flux density of 1.1·10⁷n·cm^–2·s^–1 for 6 hours by a small nuclear reactor and liquid scintillation counting for 2000 minutes     

Determination of traces of phosphorus in gallium arsenide by radiochemical neutron activation analysis

A radiochemical separation procedure has been developed to determine traces of phosphorus in gallium arsenide. In this procedure the indicator nuclide³²P is separated from all other long-lived activation products in high purity. The resulting eluate is sufficiently pure to allow -counting. Because of the high -energy of³²P (1710 keV) the activity can be measured via the Cerenkov effect, whereas most radionuclides, because they have essentially lower -energies, are discriminated by this technique, so that the selectivity of the measurement of³²P is improved considerably. A detection limit of 1 ng/g was achieved when using samples of 50 mg, a thermal neutron flux of _th=1·10¹³n·cm^–2·s^–1, an irradiation time of 36 hours and a measuring time of 1 hour.     

Elemental composition studies of fugitive and ambient air dust particulates from a thermal power station by instrumental neutron activation analysis

In order to assess the source of pollutants and the atmosphere quality in and around a thermal power plant, fugitive dust particulates from seven different locations and ambient air dust from six locations have been analyzed for 32 elements (As, Au, Ba, Br, Ce, Cl, Co, Cr, Cs, Cu, Eu, Fe, Ga, Hg, Hf, K, La, Lu, Mg, Mn, Na, P, Rb, Sb, Sc, Se, Ta, Tb, Te, Th, W and Yb) by employing instrumental neutron activation analysis (INAA). The method involves the irradiation of samples and comparator standards in a thermal neutron flux range of 10¹²–10¹³ n·cm^–2·s^–1 in a nuclear reactor for 10 min and 1 day followed by high resolution -spectrometry. Wide differences have been observed in the mean elemental concentrations of Fe, Co, Br, Mn, As, P. Ba and Cu in fugitive and ambient dust particulates coliected from these different locations. Further, a comparison of the elemental contents of the dust particulates from the plant with environmental standards (Urban Particulate Matter, Coal Fly Ash, Vehicle Exhaust and Coal) show significantly lower or comparable amounts of toxic and pollutant elements in the environmental samples.     

Interference by neutron induced second order nuclear reaction in activation analysis of platinum group elements after a nickel sulphide fire assay preconcentration

In determining the trace platinum group elements and gold in rocks and ores by the neutron activation analysis after a nickel sulphide fire assay preconcentration, there are interferences due to nuclides produced from second order nuclear reactions. This paper presents the degree of interference calculated over the ranges of long irradiation times and of reactor neutron flux from 1·10¹³ to 1·10¹⁵ n·cm^–2·s^–1. According to the results of these calculations, every one of the second order interfering reactions on the PGE+Au, except the¹⁹⁷Au(n, )¹⁹⁸Au(n, )¹⁹⁹Au reaction, can be neglected under the long irradiation time or high reactor neutron flux. Special attention is given to the interference from gold in the determining platinum.     

Separation of fluoride ion by extraction with triphenyltin chloride. Application for NAA of fluorine by means of 14-MeV neutrons

The separation of fluoride by extraction with toluene solution of triphenyltin chloride has been studied. Quantitative isolation of fluoride from solutions with a wide acidity range (pH 4.0–11.5) has been established. It is suggested that interferences by Ca, Mg, Fe, and Al can be avoided by masking these elements using sulfate and hydroxyde ions. Interference by phosphate ions can be overcome in a similar fashion. The halogenated species can be masked by mercury nitrate. Detection limit for fluorine determination is about 3 g for a neutron generator flux of 2·11¹¹ n·cm^–1·s^–1. A method for fluorine assay in water using a neutron generator with a detection limit of 1 ppm has been developed.     

Chlorine loss from polyvinylchloride under neutron irradiation

PVC samples were irradiated for 1 hour with a thermal neutron flux of _th =4.71·10¹¹n·cm^–2·s^–1 and the chlorine lost during irradiation was measured by -ray spectrometry. About 15% of loss of chlorine has been observed for untreated samples while samples heated to temperatures of 60 and 80°C for one minute before irradiation have been found to loose about 8% and 3%, respectively. The results indicate an influence of the polymer structure on the release of chlorine.     

Analytical possibilities of the BOR 60 reactor

The analytical potential of a fast neutron reactor has been studied. The maximum density of the neutron flux is 2.5·10¹⁵ cm^–2·s^–1 at a maximum energy of 450 keV. The determining reaction for activation analysis at this reactor is an (n, n) reaction. The possibility of selectively determining Pb, Hg, Cd, Au, Ag and other elements at a level of 10^–5–10^–8% is demonstrated. This activation technique allows rapid determination of these elements.     

Multielemental analysis of IAEA intercomparison standard Hay Powder,V-10 and some edible plant leaves by neutron activation

Instrumental Neutron Activation Analysis (INAA) has been employed for the multielemental determination of an IAEA intercomparison standard Hay Powder, V-10 and some edible plant leaves consumed in India. The samples were irradiated with thermal neutrons at a flux 10¹² n·cm^–2·s^–1 in a reactor for 5 minutes, 1, 2, 5, 10 and 15 hours and counted by high resolution -ray spectrometry. Nearly 18 elements have been determined. Good agreement is observed for most of the elements in several NBS standards and the proposed CRM V-10. Some edible vegetable plant leaves have also been analyzed.Partly presented at the 7th International Conference on Modern Trends in Activation Analysis, June 23–27, 1986, Copenhagen, Denmark, MTAA-7169.     

Neutron activation analysis of major and trace elements in crude petroleum

We have determined the concentration of 25 trace elements in crude petroleum from seven Libyan oil fields by instrumental neutron activation analysis. Crude oil samples were irradiated with a thermal neutron dose rate of 10¹² and 10¹³ n·cm^–2·s^–1 in the Tajoura research reactor. The concentration of U, Br, Mg, Cu, Na, V, Cl, Al, Mn and Ca is in a range of 0.015 to 84 ppm and that of sulphur of 0.12 to 1.8%. The elements Sc, Cr, Ni, Fe, Co, Zn, Ag, Se, Sb, Ba, Cs, Yb, Hf and Hg have a concentration range of 0.009 to 8747 ppb. The coefficients of variation are within 10%. The elements V and Ni occur as both porphyrin and non-porphyrin and the ratio of these two forms varies over a wide range. The V/Ni ratios are located between 0.17 and 6.67, which are comparable to the reported values for the crude oils from other countries.