Gamma ray spectra and sensitivities for 14 MeV neutron activation analysis

The purpose of this study was to define experimentally the sensitivity of determination for 63 different elements by 14 MeV neutron activation, with a 150 kV Cockroft-Walton accelerator at a neutron flux of 2·10⁸ n·cm⁻²·sec⁻¹ on the sample. The obtained gamma ray spectra are given, and the origin of the photopeaks observed are explained. A maximum irradiation time of five minutes was used as a convenient experimental limit to obtain the maximum sensitivity, considering, however, that the tritium target life is limited, and that the time to perform an analysis has to be reasonable. The practical use of 14 MeV neutron activation analysis is demonstrated by the detection limits obtained.     

Determination de quelques elements traces dans le charbon,d'une maniere non destructive,par photoactivation nucleaire

Photonuclear activation and high resolution gamma spectrometry have been used to determine nondestructively 28 trace elements in coal. The samples and synthetic multielement standards were simultaneously irradiated in the bremsstrahlung beam at 18 and 30 MeV maximum energies. Taking into account the contribution of the main possible interferences, limits of detection between 0.2 and 125 μg·g⁻¹ were obtained.

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Stagiaire Etranger au C. E. A.     

The determination of carbon,nitrogen and oxygen in gases by neutron time-of-flight spectrometry

Carbon, nitrogen and oxygen were determined in gases by time-of-flight spectrometry of prompt neutrons from the respective reactions¹²C(d, n)¹³N,¹⁴N(d, n)¹⁵O and¹⁶O(d, n)¹⁷F, produced by a pulsed beam of deuterons of 2 MeV (for nitrogen) or 3 MeV. The analysis is non-destructive and requires about 15 min. per sample. The relative standard deviation for all three elements was about ±3%. Detection limits, using a total irradiation current of 20 millicoulombs, for carbon, nitrogen and oxygen, respectively, were 6·10⁻⁸ g, 2·10⁻⁷ g and 1.7·10⁻⁷ g per cm² cross-sectional area of irradiating beam.     

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%.     

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.     

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.     

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.     

Neutron beam preparation with Am–Be source for analysis of biological samples with PGNAA method

Material analysis with prompt gamma neutron activation analysis (PGNAA) requires a proper geometrical arrangement for equipments in laboratory. Application of PGNAA in analysis of biological samples, due to small size of sample, needs attention to the dimension of neutron beam. In our work, neutron source has been made of ²⁴¹Am–Be type. Activity of ²⁴¹Am was 20 Ci which lead to neutron source strength of 4.4 × 10⁷ neutrons per second. Water has been considered as the basic shielding material for the neutron source. The effect of various concentration of boric acid in the reduction of intensity of fast and thermal components of the neutron beam and gamma ray has been investigated. Gamma ray is produced by (α, n) reaction in Am–Be source (4.483 MeV), neutron capture by hydrogen (2.224 MeV), and neutron capture by boron (0.483 MeV). Various types of neutron and gamma ray dosimeters have been employed including BF₃ and NE-213 detectors to detect fast and thermal neutrons. BGO scintillation detector has been used for gamma ray spectroscopy. It is shown that the gamma and neutron radiation dose due to direct beam is of the same magnitude as the dose due to radiation scattered in the laboratory ambient. It is concluded that 14 kg boric acid dissolved in 1,000 kg water is the optimum solution to surround the neutron source. The experimental results have been compared with Monte Carlo simulation.     

Determination of chromium in blood by neutron activation analysis

A procedure for the determination of chromium in blood has been developed with a sensitivity of 5×10⁻³ μg Cr. Dried blood was irradiated with a neutron flux of 10¹² n·cm⁻²·sec⁻¹ in the VVRS reactor for 4 weeks, then the sample was mineralized and the chromium isolated by extraction as perchromic acid. The determination of the chromium content was accomplished by measuring the 0.32 MeV gamma energy of⁵¹Cr. In order to make correction for the interfering reaction⁵⁴Fe(n,α)⁵¹Cr, the formation of chromium from high-purity iron was investigated. The chromium content of the blood samples was between 1.03×10⁻² and 5.2×10⁻² ppm Cr.     

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.     

Trace determination of boron,silicon and sulfur with oxygen-18 ion bombardment

In order to determine traces of boron, silicon and sulfur, B(¹⁸O, x)²⁷Mg, Si(¹⁸O, x)⁴³Sc and S(¹⁸O, x)⁴⁷V reactions have been investigated between 15 and 44MeV. At 34 MeV, only a few of the systematically identified nuclear interferences produce²⁷Mg and the detection limit is 30ng boron for a 10 minute irradiation with a 0.3μA·cm⁻² oxygen-18 beam. Silicon analysis has shown nuclear interferences from Al, P and K; interference-free detection limit is 80 ng silicon for an hour irradiation with a 0.4 μA·cm⁻² beam at 39 MeV. There is no nuclear interference for the sulfur determination and the detection limit is 5 ng sulfur for a 30 minutes irradiation with a 0.5 μA·cm⁻² beam at 39 MeV. Thus a selective and sensitive sulfur determination can be achieved.     

Natural radioactivity and indoor radiation measurements in buildings and building materials in Gobichettipalayam town

Samples of natural and manufactured building materials used by the people of Gobichettipalayam town have been analyzed for ²²⁶Ra, ²³²Th and ⁴⁰K using gamma-ray spectrometry. Radium equivalent activity of the materials has been measured using the formula given by OECD and the geometric mean value of sand, clay and cements are found to be 53.53 Bq·kg⁻¹, 89.09 Bq·kg⁻¹ and 72.25 Bq·kg⁻¹, respectively. The radium equivalent activities obtained in the building materials are all well below the acceptable limit. The indoor gamma-dose has been measured using thermoluminescence dosimeters and it was found in the range of 1051.2–3946.0 μGy/year. The annual effective indoor gamma radiation dose to the people of Gobichettipalayam town has been found to be 0.8 mSv/y.     

Analyse multielementaire des cheveux par photoactivation nucleaire

Photonuclear activation with 18 and 35 MeV bremsstrahlung beams and gamma ray spectrometry has been used to determine the concentrations of 14 elements in human hair. A careful study of interferences made possible a nondestructive analysis with practical limits of detection between 0.1 and 100 μg·g.      

In vitro activation of bone with 14 MeV neutrons

Samples of compact bone, bone marrow and spongiosa of cow femur have been irradiated in vitro with 14 MeV neutrons. The Ca/P ratio for compact bone was found to be 2.16±0.24. The suitability of using 14 MeV neutrons and the³¹P(n, α)²⁸Al reaction for studying the bone mineral composition in vitro is discussed.     

Simultaneous oxygen,carbon, nitrogen,sulfur and silicon determination in coal by proton induced gamma-ray analysis

The technique of gamma-ray analysis of light elements (GRALE) is extended to measure the concentration of carbon, nitrogen, oxygen, sulfur and silicon in coal samples. The composition of the sample is determined by analyzing the spectrum of gamma rays emitted following inelastic scattering of protons bombarding the target. A large volume lithium drifted germanium detector is used as a gamma-ray detector in this work. Coal samples are irradiated with 9.5 MeV protons in a helium atmosphere for 1000 sec. Results with standard coal samples indicate that the method has an accuracy of ∼5% of the concentration of each element and a precision of ∼4% for elements constituting at least 1% of the coal by weight.     

Investigation of the interaction of Greek dolomitic marble with metal aqueous solutions using rutherford backscattering and X-ray photoelectron spectroscopy

To enhance the applicability of the nuclear analytical technique in the field of industry and the environment, the inorganic elemental content of the bottom ash from a municipal solid waste incinerator was determined by instrumental neutron activation analysis. Bottom ash samples were monthly collected from an incinerator located at a metropolitan city in Korea, strained through a 5 mm sieve, dried by an oven and pulverized by an agate mortar. The samples were irradiated at the NAA #1 irradiation hole (thermal neutron flux: 2.92·10¹³ n·cm⁻²·s⁻¹) in the HANARO research reactor of the Korea Atomic Energy Research Institute and the irradiated samples were measured by a HP Ge gamma-ray spectrometer. Thirty-three elements including As, Cr, Cu, Fe, Mn, Sb and Zn were analyzed by an absolute method. The quality control was conducted by a simultaneous analysis with NIST standard reference materials. The average concentrations of the major elements such as Ca, Fe, Al, Na, Mg, K and Ti measured in the sample were 19.9%, 4.85%, 3.79%, 2.11%, 1.84%, 1.22% and 1.02%, respectively. In addition, the concentrations of the hazardous metals like Zn, Cu, Cr, Sb and As were 0.77%, 0.31%, 729 mg·kg⁻¹, 116 mg·kg⁻¹ and 22.2 mg·kg⁻¹, respectively.     

Determination of nitrogen in steels by alpha-induced prompt gamma-ray spectrometry

The prompt gamma-ray of 871 keV emitted during the bombardment of steels by 5 MeV alpha particles were used to determine nitrogen by means of the reaction¹⁴N(α, pγ)¹⁷O. The method is non-destructive, rapid and experimentally simple. It has a sensitivity of about 7 μg·g⁻¹. In the nitrogen concentration range of 10¹–10² μg·g⁻¹ the relative precision of the method is about 3%. The accuracy of the method compares with that of other nuclear methods. Presented at the 5th Symposium on Recent Developments in Activation Analysis, Oxford, 17–21 July, 1978.     

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.     

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.     

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.