Halogen speciation in the rat thyroid: Simultaneous determination of bromine and iodine by short-term INAA

The study describes a mode of non-destructive simultaneous determination of bromine and iodine concentrations, by reactor instrumental neutron activation analysis (INAA) in the regime of short-term activation. Under the conditions of 1-minute activation in the neutron flux of 8.0·10¹³ n·cm⁻²·s⁻¹, it was possible to determine reliably as little as 5·10⁻⁸ g bromine and about 10⁻⁷ g iodine in matrices of a given type and of the mass of about 5 mg dry weight. We applied this method for the determination of Br and I concentrations in the whole rat thyroid gland as well as for the halogen speciation in fractions separated from this organ.     

Determination of trace elements in high purity copper by INAA, GFAAS and ICP/AES

Trace impurity elements in high purity copper metal (4 mine class) put on the market were analyzed by Instrumental Neutron Activation Analysis (INAA) and the results compared with those from Graphite Furnace Atomic Absorption Spectrophotometry (GFAAS) and Inductively Coupled Plasma Atomic Emission Spectrophotometry (ICP-AES). The sample irradiation was done at the irradiation facilities (thermal neutron flux, 5·10¹² n·cm⁻²·s⁻¹) of the TRIGA Mark-III research reactor in the Korea Atomic Energy Research Institute. Four unalloyed copper standards (NIST SRM # 393, 394, 395 and 398) were used to identify the accuracy and precision of the analytical procedure. The homogeneity of samples was assessed by means of the elements such as Ag, As, Co, Sb, Se and Zn. The analytical results of INAA, GFAAS and ICP-AES were in good agreement within expected uncertainties each other and showed the possibility of using them for the analytical quality control.     

Fast-neutron activation analysis with short-lived nuclides

At the GKSS Research Center Geesthacht, a new 14 MeV activation facility—a 5·10¹² n/s neutron generator combined with a fast rabbit system (KORONA)—is being installed. Homogeneous neutron flux at a level of 5·10¹⁰ n·cm⁻²·s⁻¹ and sample transfer times of 140 ms to a 16m distant detector station are characteristic features of the facility described in the paper. With special consideration of short-lived nuclides and including cyclic activation, the analytical prospects with the intense neutron source are discussed, and sensitivities for 78 elements are presented.     

Characterization and use of the new NIST rapid pneumatic tube irradiation facility

Recently a new rapid pneumatic tube facility was inserted into a long unused location in the NIST 20 MW nuclear reactor. This facility was designed and constructed specifically for rapid INAA using short lived activation products. Included is a computer controlled console which uses fast sensors to accurately measure the irradiation capsule flight time, and a loss-free counting system connected to a 32% efficient PHGe detector with a transistor reset preamplifier. Measurement of travel, times from end-of-irradiation to detector were 473±8 ms. Measurement of the thermal neutron fluence rate was 5.0·10¹³ n·cm⁻²·s⁻¹. The other three pneumatic tubes in the NIST reactor have transfer times of 3 to 15 seconds, and no timing capability more accurate than human response. This new facility substantially improves our ability to accurately determine activation products with half-lives from 1 to 100 seconds. Characterization information reported on this new irradiation facility includes absolute fluence measurements, fluence rate variations within the capsule and variations with time, and determination of analytical sensitivities for fluorine-20 selenium-77m, and silver-110g.     

Test-fitting on adsorption isotherms of organic pollutants from waste waters on activated carbon

An alternative method of approach has been developed for the measurement of thermal neutron flux. The method depends only on the activity of the bare foil if the cadmium ratio at the irradiation position is known. The method has been tested on the GHARR-1 facility at the Ghana Atomic Energy Commission using gold and indium foils for the measurement of the thermal neutron flux in the flux range of 10¹⁰–10¹² n·cm⁻²·s⁻¹ and the results compare very well with those obtained using the conventional method (cadmium separation method).     

Rare-earth elemental analysis of banded iron-formations by instrumental neutron activation analysis

Representative banded iron-formations (BIFs) from various locations of the eastern Indian geological belt were investigated by instrumental neutron activation analysis (INAA). After pre-concentration, irradiation was carried out using a neutron flux of 5.1·10¹⁶ m⁻²·s⁻¹, 1.0·10¹⁵ m⁻²·s⁻¹ and 3.7·10¹⁵ m⁻²s⁻¹, with thermal, epi-thermal and fast neutrons, respectively. The activities in these samples were measured by a HPGe detector. Ten rare-earth elements, such as La, Ce, Nd, Sm, Eu, Tb, Ho, Tm, Yb and Lu, have been qualitatively identified and quantitatively estimated in these samples. The present investigation is an example of employing a pre-concentration method for high iron-containing ores prior to neutron activation analysis.     

Determination of 22 elements in geological samples by instrumental neutron activation analysis

An instrumental neutron activation analysis (INAA) method has been developed for multi-element determination in geological samples. The INAA method consists of irradiation of samples for 90 sec at a flux of 1.0·10¹² n·cm⁻²·sec⁻¹ and determination of 12 elements by using their short-lived nuclides. Samples have been re-irradiated for 3 hrs for measuring concentrations of another 10 elements. Precision and accuracy of the INAA method have been evaluated by analysing samples and USGS standard reference materials. Precision and accuracy are within±15% and ±10%, respectively.     

Alternative chromatographic processes for no-carrier added 177Lu radioisotope separation Part I. Multi-column chromatographic process for clinically applicable

The conventional multi-column solid phase extraction (SPE) chromatography technique using di-(2-ethylhexyl)orthophosphoric acid (HDEHP) impregnated OASIS-HLB sorbent based SPE resins (OASIS-HDEHP) was developed for the separation of no-carrier added (n.c.a) ¹⁷⁷Lu from the bulk quantity of ytterbium target. This technique exploited the large variation of lutetium metal ion distribution coefficients in the varying acidity of the HCl solution-OASIS-HDEHP resin systems for the consecutive loading-eluting cycles performed on different columns. The production batches of several hundred mCi n.c.a ¹⁷⁷Lu radioisotope separated from 50 mg Yb target activated in a nuclear reactor of medium neutron flux (Φ = 5·10¹³ n·cm⁻²·s⁻¹) were successfully performed using the above mentioned separation technique. With the target irradiation in a reactor of thermal neutron flux Φ = 2·10¹⁴ n·cm⁻²·s⁻¹ or the parallel run of several separation units, many Ci-s of n.c.a ¹⁷⁷Lu can be profitably produced. The OASIS-HDEHP resin based multi-column SPE chromatography technique makes the separation process simple and economic and offers an automation capability for operation in highly radioactive hazardous environments.     

Gallium determination in biological samples

A sensitive, simple and time-saving method has been developed for the neutron activation analysis of gallium at concentrations around 10⁻⁴ ppm in biological tissues. After a 24-hour irradiation in a thermal neutron flux of 2.8·10¹³ n·cm⁻²·s⁻¹ and a purification by ion-exchange chromatography to eliminate troublesome elements such as sodium, iron and copper, the⁷²Ga activity is measured with enough accuracy for the method to be applicable in animal physiology and clinical toxicology.     

Determination of phosphorus in polymers by INAA

An INAA technique employing beta spectrometry was developed for the determination of phosphorus in polymers. The (n,γ) reaction on phosphorus produces³²P, half-life 14.3 days, a pure beta emitter with end-point energy 1.71 MeV. Polymer samples in the form of powders, films and pellets are irradiated and then counted with a plastic scintillator. The beta spectrum is corrected for interferences (especially Sb, Zn and Br which are quantified by gamma spectrometry) and for energy loss in the thick sample. Samples must also be analyzed for S and Cl which cause nuclear interferences. With an irradiation time of 4 hours at a neutron flux of 5·10¹¹ n·cm^{−2 s −1}, decay time 10 days and counting time 10 minutes, the sensitivity is 520 counts/μg phosphorus and the detection limit is typically 2μg/g.     

A study of the elemental composition of diabases by instrumental neutron activation and X-ray fluorescence analysis

The distribution of the elemental composition was studied mainly for microelements in the diabases of the Pechenga suite subjected to various changes. Investigations were conducted by a combination of instrumental neutron activation INAA and X-ray fluoresence XRFA analyses. The INAA was conducted with sample weights of 20–100 mg exposed to irradiation in a nuclear reactor by a flux of neutrons ≈10¹³ n·cm⁻²·s⁻¹. Measurements were carried out by means of a semi-conductor gamma-spectrometer with a Ge(Li) detector. The determination of Al, Mn, Mg, Ti, V, Ca was conducted by short-lived isotopes, while the determination of Na, Sc, Fe, Co, Cr, Hf, Th, La, Ce, Sm, Eu, Yb, Lu by longlived ones. For XRFA samples weighing up to 2 g were irradiated by means of an¹⁰⁹Cd isotope source and were measured by a spectrometer with a Si(Li) detector and beryllium window. By this method we determined the Sr, Zr an Nb contents. Continuous distribution histograms were plotted for the concentration of 22 elements and some of their ratios. Considerable variations in microelemental composition observed in a number of cases make it possible to assess the character of past processes of diabasic change.     

Analytical use of neutron-capture gamma-rays

Certain elements which are not possible to detect with conventional neutron activation analysis can be measured using thermal neutron-capture gamma-ray analysis. The use of a curved neutron guide at the High Flux Reactor, Grenoble, with a thermal neutron flux of 1.5·10¹⁰n·cm⁻²·sec⁻¹ and the advantage of a low-background counting system (Ge(Li) detector) far from the reactor core are described. Experimental detection limits of a number of elements are given for the low-energy and the high-energy regions. Some applications of the capture gamma-ray method in the whole energy range are studied and are briefly discussed.     

Characterization of trace elements in medicinal herbs by instrumental neutron activation analysis

Medicinal herbs are often used as alternative medicines for healing and controlling some diseases in the world. This study focuses on the content of heavy and trace elements of some widely consumed herbs in Libya. Nine most popular herbs were analyzed by k ₀-instrumental neutron activation analysis. All the samples, SRM and flux monitors were irradiated for 7 and 10 hours under thermal neutron flux of 1.3·10¹³ cm⁻²·s⁻¹ at Tajoura nuclear reactor. In total, 33 elements were analyzed in different herbs. The variations in the concentration of the elements are attributed to soil composition and the climate in which the plant grows. The study showed that the toxic elements found in the samples were below the levels prescribed by health regulations. The precision and the accuracy of the results were evaluated by analyzing the reference materials Pine Needles SRM 1575 and Citrus Leaves SRM1572.     

Design and construction of a facility for neutron activation analysis using the 14 MeV neutron generator at HMS Sultan

The potential for using a small, sealed tube, DT neutron generator for neutron activation analysis has been well documented but not well demonstrated, except for 14 MeV activation analysis. This paper describes the design, construction and characterization of a neutron irradiation facility incorporating a small sealed tube DT neutron generator producing 14 MeV neutrons with fluence rates of 2·10⁸ s⁻¹ in 4π (steady state) and 10¹¹ s⁻¹ in 4π (pulsed). Monte Carlo modeling using MCNP4c and McBend9 has been used to optimize the design of this facility, including the location of a thermal irradiation facility for conventional neutron activation analysis. A significant factor in designing the facility has been the requirement to conform with Ionising Radiation Regulations and the design has been optimized to keep potential radiation doses to less that 1 μSv/h at the external walls of the facility. Activation of gold foils has been used for flux characterization and the experimental results agree well with the modeling.     

Ultra-sensitive determination of K, Th, U and other trace impurities in liquid organic scintillators by NAA

We present a NAA method to determine ultratraces of K, Th, U and other trace impurities in liquid organic scintillators, which are known as ultrapure detector materials for neutrino or dark matter experiments. A combined optimization of relevant factors for sensitive NAA has been realized, leading to a sensitivity for U down to 10⁻¹⁶g/g. Samples of 250 ml have been irradiated up to 120 h at a thermal neutron flux of 5–8·10¹²·n·cm⁻²·s⁻¹. Acidic extraction, wet ashing and TBP-extraction are used for radiochemical separations. Finally, coincidence techniques are applied for increased sensitivity.     

Instrumental neutron activation analysis of monomineral fractions of sulfide minerals and quartzes

A method has been worked out of multi-elemental instrumental neutron-activation analysis INAA of small weights some mg of monomineral fractions of sulfide minerals pyrites, galenites, chalcopyrites, arsenopyrites, bornites, chalcosines and quartzes. The samples were irradiated in a nuclear reactor under a flux of 1.3·10¹³ n·cm⁻²·s⁻¹. For measuring the gamma radiation of the exposed samples Ge(Li) gamma-spectrometers with semiconductor detectors were used. Determined in sulfide monofractions were the elements: Co, Sc, Ag, Se, Sb, Cr, Fe, Zr; rare-earth elements: Ce, Sm, Eu and others at content levels of 10⁻¹−10⁻⁴%. In quartzes they were: Mn, Na, Sb, Cr, Sc, Fe, Co at content levels of 10⁻⁵−10⁻⁷% and Au to n×10⁻⁹%. A special method has been worked out for the determination of In in sulfides with the irradiation of samples in a cadmium screen. An example is cited of using the method for studying some peculiar features of the genetics of copper pyrite deposits. The data on the distribution of admixture elements in sulfide monofractions produced in this work made it possible to conclude that the oreformation in the deposits has a stage-by-stage character.     

Commercial grade aluminium: A versatile reactor flux monitor

With the advent of Ge(Li) spectrometry, a high standard of purity for neutron flux monitors no longer remains an imperative “must” and becomes rather superfluous. From this standpoint, commercial grade Al was investigated for its suitability as a reactor flux monitor and was found to have a much greater practical utility than most of the monitors reported. Three Al foils and one wire were randomly selected from four different commercial sources, and analysed for their Fe, Ga, Mn and Na contents by neutron activation and high-resolution gamma-spectrometry. While Na was found to have a very heterogeneous distribution, Fe, Mn and Ga concentrations in different splits of each type of Al were consistently uniform within ±2–3%. Eight possible monitor reactions on Al, Mn, Fe and Ga have been recommended as neutron flux integrators for all the 3 components of a reactor spectrum, viz. thermal, epithermal and fast, covering a wide range of flux levels from 10⁷ to 10¹⁴n·cm⁻²·sec⁻¹. The advantages and versatility of commercial grade Al as a pile neutron dosimeter are discussed.     

The role of NAA in nuclear chemistry education

One of the missions of our Institute is the promotion of basic nuclear teaching for students as well as professional teaching for workers in nuclear industry and research. For nuclear chemistry education, we present here a one day teaching course on radioactive decay and nuclear reactions, and a two or three days course based on reactor irradiation of uranium oxide, instrumental and radiochemical analysis of fission products. In the first experiment, the neutron capture is presented as an example of nuclear reaction; the neutron activation of a silver coin with a Am-Be neutron source, followed by γ-ray spectrometry, is used to identify three radionuclides of silver and to calculate their half-lives. In the second experiment, our teaching reactor is used as a neutron source with a flux about 10¹⁰ n·cm⁻²·s⁻¹ at a low thermal power (10 kW). This low flux allows us to irradiate a small uranium sample which is usable for spectrometry after a short cooling time of about two hours. The first day is reserved for instrumental analysis of the fission products and a second day for the radiochemical separation of a fission radionuclides. With these experimental results, the students have to calculate the number of fissions in the irradiated sample. On optional third day for postgraduate students is devoted to the presentation of NAA and some applications as uranium determination by the fission product spectrometry.     

Trace element content of medicinal plants from Algeria

Neutron activation analysis (INAA) has been applied to multielemental determination of eleven medicinal plants used to cure the urinary tract diseases observed in Algeria. These plants include Androgena Citratus, Ceratonia Siliquata, Punica Granatum, Glyryrrhiza Glabra, Lausaunia Alba, Fragaria Vesca, Arbutus Unedol, Hordeum Vulgaris, Papieteria Officinalis, Zea Mays L, and Davallia Seae. Concentrations of twenty elements Ba, Br, Ca, Cl, Co, Cu, Cr, Fe, I, Mn, Na, Mg, Rb, Sb, Se, Sc, Sr, Ti, V, and Zn have been determined by short, and long irradiation times with a thermal and epithermal flux of 1.4·10¹² n·cm⁻²·s⁻¹ and 1.4·10¹¹ n·cm⁻²·s⁻¹, respectively. These analyses were performed in conjunction with Compton suppression. In almost herbs studied the Co, Cr, Cu, Rb, Sb, Sc, Se and V are found to be present at trace levels, Br, Mn, and Zn at the minor level, and Ca, Cl, Fe, Mg and Na are generally at the major level. The accuracy of the measurements has been evaluated by analyzing NIST-botanical references materials.