Utilization of cyclotron produced fast neutrons in the activation analysis for oxygen

The possible application of cyclotron-produced fast neutrons to activation analysis for oxygen based on the¹⁶O(n, p)¹⁶N reaction has been investigated. Neutrons were produced by bombarding a thick beryllium target with 22 to 45 MeV deuterons. It was found that the sensitivity increases rapidly with the energy of the deuterons. Using 45 MeV deuterons and a 10 μA beam current a sensitivity of about 20 counts per 1 μg oxigen could be achieved, enabling the determination of less than 1 μg oxigen. In a direct comparison it was experimentally established that the sensitivity for cyclotron-produced neutrons assuming a deuteron beam of about 10 μA, is up to two orders of magnitude higher than that achievable for 14 MeV neutrons with a flux of about 10¹⁰ n/s. The interference of fluorine is at about the same level for both the cyclotron-produced and 14 MeV neutrons. Using cyclotron-produced fast neutrons in the investigated energy range, sodium and magnesium can also interfere, but only to a very much lower extent.     

Estimation of the possibilities of a neutron generator-based source of thermalized neutrons for activation analysis

Characteristics of a source of thermal neutrons based on an evacuated NG-400 neutron generator with the maximum flux (Φ_f) 2 × 10¹¹ neutron/s for 14 MeV neutrons and 2 × 10⁹ neutrons/s for 3 meV neutrons have been investigated. The possibilities of its application for neutron activation analysis have been estimated. The distribution, composition, and density (φ_T) values of the thermal neutron flux have been measured in the inner cavity of the moderator using activation detectors. φ_T was 2 × 10⁸ and 2 × 10⁶ neutrons/cm² s for thermalized neutrons with energies of 14 and 3 MeV, respectively. The possibilities of the apparatus have been estimated theoretically and experimentally for the cases of thermalized neutrons of 14 MeV and 3 MeV.     

Contribution a l’etude du dosage par radioactivation du soufre et du phosphore en tres faibles concentrations dans les metaux de tres haute purete (Aluminium,magnesium, cuivre,fer, nickel)

The analytical procedure for the determination of sulfur in copper by activation with thermal neutrons is given. The purifications necessary to obtain a radiochemically pure precipitate of baryum sulphate are described. The occurrence of some discrepant values in the determinations led to the observation, for the first time, of abnormally high contents of³⁵S^* at a relatively important depth in the samples of irradiated copper (as deep as about 300 μ). Therefore it is necessary to etch the samples to a depth of 300 μ at least on each surface, before doing the chemical separations. Owing to the great influence of the reaction³⁵Cl(n,p)³⁵S^*, the determination of sulfur by thermal neutrons is only possible at contents higher than 10⁻⁶, even if the chlorine concentration is very low (2·10⁻⁸ Cl introduces a correction in terms of sulfur of the order of 10⁻⁶). For sulfur contents lower than 10⁻⁶, the determination is made by irradiation in fast neutrons. The analytical procedure is described and the corrections in the presence of phosphorus and chlorine are discussed. At contents of the order of 10⁻⁸, the corrections are very small and the determination of some 10⁻⁷ of sulfur is easy. Finally, the determination of phosphorus in copper by activation in thermal neutrons is given. The chemical separations are the same as in the preceding case. Contents of the order of 10⁻⁸ phosphorus are determined without difficulty. The results of the determination of sulfur and phosphorus in many samples of copper are indicated: OFHC copper, High Purity copper (99.999%) and different samples of zone refined copper prepared at the Vitry’s Laboratory.      

Errors in activation analysis by nuclear recoil

The recoil energies of up to several MeV developed during nuclear reactions involving particle emission lead to the radionuclides used in the analysis being redistributed between adjacent materials. In aluminum irradiated by reactor neutrons,²⁴Na losses were observed up to a depth of 8·10⁻⁶ m; in the adjacent silicon, a²⁴Na penetration depth was observed up to 4·10⁻⁶ m. Similar results were obtained from reaction products deriving from irradiation of Ti, Ni, N, S and Cl. This means that the results of activation analysis investigations performed for the purpose of evaluating this type of reaction might contain significant errors if thin layers, boundary zones of very small sample volumes are examined. In the analysis of surface layers on silicon devices, completely erroneous results have been obtained in some cases due to the recoil phenomena described.     

Evaluation of stray neutron distribution in medical cyclotron vault room by neutron activation analysis approach

Stray neutron distribution in a medical cyclotron vault room was evaluated by neutron activation analysis (NAA). Neutrons were generated in the production of radioactive nuclides, such as ¹⁸F, ¹¹C, ¹³N and ¹⁵O, for diagnostic usage. Indium foil was adopted to evaluate the stray fast and thermal neutron intensity based on ¹¹⁵In(n_f, n′)^115mIn and ¹¹⁵In(n_th, γ)^116m1In reactions, respectively. The indium foils were weighed, sealed and placed at 62 points around the 6.7×8.2 m² cyclotron room. Additionally, each indium foil was exposed for over 80 minutes during cyclotron operation and γ-peaks were analyzed using an HPGe detector to evaluate the number of stray fast (Φ _f) or thermal (Φ _th) neutrons. The minimum to maximum numbers of fast and thermal neutrons were (3.47±0.11)×10³ to (1.06±0.21)×10⁴ n·cm⁻²·s⁻¹ and 9 to 965 n·cm⁻²·s⁻¹, respectively. The minimum detectable limit for stray neutrons was included herein to demonstrate the reliability. Accordingly, 60 and two points, respectively, the confidence level associated with the reported intensities of fast and thermal neutrons reached 95%. The low qualified ratio in the evaluation of stray thermal neutrons might have been caused by either the high Compton scattering plateau or the low intensity of the gamma-ray peak in the relevant spectrum.     

Fast neutron activation analysis of silicon in aluminum alloys

The silicon content in an aluminum-silicon alloy was measured by nondestructive fast neutron activation analysis with fission spectrum neutrons. A boron nitride irradiation container reduced the flux of thermal and epithermal neutrons at the sample position, enhancing the²⁹Si (n, p)²⁹Al reaction. A detection limit of 0.4% silicon in a 0.5 g alloy sample was obtained.     

Gaseous sample introduction for the determination of silicon by ICP-AES

The generation of volatile species of silicon as a means to introduce silicon into an inductively coupled plasma has been studied. It is based on the reaction between silicon and fluoride ions in sulfuric acid media and it was carried out using different flow injection mountings. The first mounting works with an injection of 100 μL concentrated sulfuric acid and 150 μL silicon standard solution in a continuous 0.05 mol L^–1 NaF solution flow. The method shows a linear response between the intensity of emission at 251.611 nm line and the silicon concentration from 0.1 to 200 μg mL^–1, with a reproducibility of 2% and a detection limit of 0.004 μg mL^–1. The second mounting produces the volatile species by the reaction between two opposed aerosol flows in a home-made nebulization chamber. This chamber has a Cross-Flow and a Meinhard nebulizer at either end. A linear response ranging from 0.1 to 1000 μg mL^–1 of silicon solution is obtained and the reproducibility rises to 8%.The detection limit reached is 0.02 μg mL^–1. The silicon content in real water samples was determined by applying both the above-mentioned methods and a third method for reference. Received: 6 November 1996 / Revised: 19 December 1996 / Accepted: 3 January 1997     

Heterogeneous exchange reactions of unstable simple systems

The analysis of less than 10⁻⁹ g of the isotope²⁰⁴Pb in lunar samples was carried out by an (n, 2n) activation using high energy (>8. 8 MeV) neutrons. A procedure of using the neutrons produced by bombardment of a specially designed Be sample holder with deuterons in a cyclotron was developed and compared to irradiation carried out in the core of a nuclear reactor, Radiochemical separations and X ray-γ ray coincidence counting techniques are necessary to achieve the required sensitivity. Although the flux of neutrons of sufficient energy from the cyclotron procedure is somewhat lower can be obtained in the best reactor irradiations, the high radioactivity due to other elements produced by the (n, γ) reactions in the reactor is eliminated. Radiochemical procedures for the analysis of Bi, Tl, Zn in the same samples are also described.     

Fluorine analysis by activation with an isotopic fast-neutron source and counting Nitrogen-16

A rapid, nondestructive method has been developed for determination of fluorine by activation with fast neutrons from a²⁴¹Am-²⁴²Cm-Be source and counting the 6–7 MeV γ rays of the product nitrogen-16. The total neutron output of the source is 4.8·10⁹ unmoderated neutrons per second and the flux is 1.4·10⁸ fast n·cm⁻²· sec⁻¹. The γ-ray detectors consist of two opposing, matched cylindrical NaI(Tl) crystals 10 cm long and 10 cm in diameter. The sample is irradiated for 30 seconds, cooled for 4 seconds, and then counted for 30 seconds. The sensitivity is 4.8·10⁴ counts nitrogen-16 per gram fluorine, and the limit of detection is 0.4 mg fluorine in a 10-gram sample. A reproducibility of 0.24% is achieved. The relative standard deviation of the specific count rate of nitrogen-16 for 11 fluorine compounds is 1.31%.     

Silicon determination in mine flue-dust by 14 MeV neutron activation analysis

The Si-contents of flue-dust and sedimented dust from Czechoslovak mines were determined by instrumental activation analysis with 14 MeV neutrons using a flux of 10⁷ cm⁻²·s⁻¹. The amounts determined range from 3 to 30 mg.     

Performance comparison of 2.8 MeV and <Superscript>241</Superscript>Am-Be neutrons based moisture measurement setups

Performance of a ²⁴¹Am-Be neutron source-based and 2.8 MeV neutrons-based moisture measurement setups have been compared using Monte Carlo simulation. In the setup fast neutrons transmitted through the sample were detected by a fast neutron detector, which was placed behind a massive long double truncated collimator. The setup geometry was optimized to detect maximum effect of 1–7 wt.% moisture on the neutron intensity transmitted through the sample. The yield of neutrons transmitted through concrete, coal, wood and soil samples containing 1–7 wt.% moisture was calculated for 2.8 MeV neutrons and neutrons from an ²⁴¹Am-Be source. The slopes of the fast neutron intensities transmitted through the samples vs. their moisture contents are very sensitive to the neutron energy and the sample composition. Higher slopes have been observed for the samples with larger bulk density. The slopes of fast neutron yield show dependence on the incident neutron energy. Larger slopes have been observed for neutrons with samller energy. Due to the overall large slopes of the transmitted intensity data of the samples for 2.8 MeV neutrons, it is expected to achieve better sensitivity in moisture measurements for a 2.8 MeV neutrons based moisture setup.     

Gamma-ray spectra and sensitivities for 2.8 MeV neutron activation analysis

The use of 2.8 MeV neutrons produced by the D(d, n)³He reaction should be taken into consideration in some applications of radioactivation analysis. The low number of elements activable by these neutrons makes possible to minimize the matrix interference and the background below the characteristic photopeaks. The very low dead-time of the spectrometric measurements permits the use of the maximum neutron flux available now and in the future. The purpose of this paper is to define experimentally the sensitivity of determination for the 16 main elements activable with a 400 keV Van de Graaff accelerator at a 2.8 MeV neutron flux of 2·10⁶ n·cm⁻²·sec⁻¹ on the sample.     

Determination of noble metals by resonance neutron activation technique

Rhodium, palladium, platinum and iridium have been determined in silver matrix by nondestructive activation analysis upon activation with cadmium- and silver-filtered resonance neutrons. Experiments with different types of filter combinations are reported. The sensitivity of the method is 5·10⁻³% for rhodium, 5·10⁻³% for palladium, 3·10⁻²% for platinum and 5·10⁻³% for iridium.     

Neutron activation analysis of zeolite catalysts

A new method for the determination of aluminum and silicon has been developed for zeolite catalysts. In contrast to previous methods, thermal neutrons are used for the analysis of both elements, and cadmium absorbers are not needed. The silicon determination utilizes a one-hour irradiation to observe the³¹Si produced by the (n, ) reaction of³⁰Si. A 15-second irradiation is used for the²⁷Al(n, )²⁸Al reaction. The²⁸Al activity is corrected for the contribution from the²⁸Si(n,p)²⁸Al reaction by using the analyzed weight of silicon in the sample and the data for a silicon standard irradiated simultaneously with the zeolite and the aluminum standard. The quantitation limits are 0.012 g for silicon and 3.3×10^–5 g for aluminum. Sodium presents a significant interference, but this element can be removed by taking advantage of the ion exchange properties of these materials.     

Determination of boron in iron-based metallic glasses by neutron irradiation and alpha-particle track recording in cellulose nitrate

A method for determination of the boron concentration in Fe−Ni−B metallic glasses has been developed. A solution of the alloy is irradiated with neutrons from a 10 μg²⁵²Cf neutron source and the alpha-activity due to the reaction¹⁰B(n, α)⁷Li is recorded by a cellulose nitrate alpha-track detector immersed in the solution. After the exposure the alpha-tracks are made visible in a microscope by etching the cellulose nitrate film in hot NaOH and the track density is determined.     

A compilation of charged particle production cross-sections by 14 MeV neutrons for Nb and Mo isotopes

A compilation of the cross sections (n, p), (n, n′ p), (n, α) (n, n′ α) and (n,³He) for⁹³Nb,^{92,95,96,97,98,100}Mo by 14 MeV neutrons is presented in the form of a table containing the results of nearly 70 different measurements, mainly obtained by activation analysis. Brief assessments of the experimental methods and the data status are given.     

Determination of oxygen with reactor neutrons

Oxygen in silicon was determined by the secondary nuclear reactions of⁶Li(n, α)T and¹⁶O(t, n)¹⁸F. Lithium fluoride was deposited in vacuum on fused quartz, covered with the sample and irradiated in a nuclear reactor. The depth profiles of¹⁸F in fused quartz and in silicon were observed, and enough depth to eliminate surface oxygen was estimated. On the basis of these results, oxygen was determined by the average cross-section method. Oxygen concentration in CZ silicon with various growing condition was 5–26 ppm and was consistent with those determined by the infrared absorption method. The detection limit of oxygen in silicon is 5 ppm.     

Determination de L’oxygene et du fluor au moyen de l’activation par les photons γ et le comptage des neutrons retardes emis par17N

The activation of¹⁸O and¹⁹F by the reactions¹⁸O(γ, p)¹⁷N and¹⁹F(γ, 2p)¹⁷N was determined as a function of the maximum energy of the bremsstrahlung beam. By the use of this method it is possible to measure oxygen or fluorine by counting the delayed neutrons emitted by¹⁷N with a half-life of 4.2 sec.      

Thermal neutron activation analysis of hafnium in zircaloy with a Van de Graaff accelerator

Thermal neutron activation analysis of hafnium in zircaloy was investigated with a Van de Graaff accelerator. Thermal neutrons were obtained by moderating Be−D fast neutrons with paraffin blocks.^179mHf isotope with a half-life of 18.6 s, produced by¹⁷⁸Hf(n, γ)^179mHf reaction, was utilized in the present analysis. This method made it possible to analyze hafnium rapidly and non-destructively by using scandium as an internal standard material. Several tens to hundreds of ppm of hafnium in zircaloy samples were determined within 2 minutes with a precision of about ±1%.