A study of flux monitoring for instrumental neutron activation analysis

The accuracy of instrumental neutron activation analysis is dependent upon measurement of the neutron flux to which samples are submitted. Flux monitoring techniques described and evaluated include: target cooling water activity, BFa counters, plastic scintillators, and a simple reference sample system. Evaluation is made on the basis of results obtained for oxygen analysis using primary standard materials. The superiority of the reference sample system for flux measurement during irregular neutron flux production is shown.     

Some aspects of quality assessment of the k0-based method of NAA

Neutron activation analysis is one of the analytical techniques often used for certification of reference materials. The k₀-based method of instrumental neutron activation analysis can also be applied in intercomparison runs in the certification process and therefore it is desirable to know its accuracy in advance. Possible systematic errors related to the application of nuclear data at given neutron flux rate parameters, that can affect the uncertainties of the results obtained by this specific method, are elucidated and error propagation factors calculated for a typical irradiation position in the TRIGA Mark II reactor of the Jozef Stefan Institute. It was found that these uncertainties are at the level of 1–2% on the average.     

BEAMGAA: A chance for high precision analysis of big samples

Summary In activation analysis of traces in small samples, the non-equivalence of the activating radiation doses of sample and calibration material gives rise to sometimes tolerable systematic errors. Conversely, analysis of major components usually demands high trueness and precision. To meet this, beam geometry activation analysis (BEAMGAA) procedures have been developed for instrumental photon (IPAA) and neutron activation analysis (INAA) in which the activating neutron/photon beam exhibits broad, flat-topped characteristics. This results in a very low lateral activating flux gradient compared to known radiation facilities, however, at significantly lower flux density. The axial flux gradient can be accounted for by a monitor-sample-monitor assembly. As a first approach, major components were determined in high purity substances as well as selenium in a cattle fodder additive.     

Investigation of gamma-spectra of biological materials irradiated in the epithermal range of the reactor neutron spectrum

Irradiation of various biological materials in the nuclear reactor neutron epithermal flux allows the increase of the selectivity of the pure instrumental method of activation analysis for the definite set of tracers either not determined instrumentally during sample irradiation by the thermal neutron flux or determined with low sensitivity. The given paper describes a method of increasing the sensitivity of the instrumental neutron activation determination of As, Br, Mo, Cd, Sb, W and Au in biological materials at the level of the whole blood, tissue and subcellular components.     

Neutron spectral measurement of the Ohio state research reactor pneumatic tube

Pneumatic irradiation facilities are used for neutron activation analysis, materials testing, electronics hardening, and radioisotope production. The application of these facilities can benefit from a greater understanding of the neutron energy profile inside the irradiation cavities as often only the cadmium ratio is known. A program to measure the energy-dependent neutron fields inside the pneumatic tube at the Ohio State University Research Reactor was undertaken using wires consisting of thermal activation materials and threshold reaction materials with and without thermal and resonance absorbers surrounding them. The measured activities were unfolded using the MAXED unfolding code to reconstruct the neutron energy spectra and compared to the MCNP-calculated flux.     

Prompt determination of evacuee radiation dose from a nuclear event

In anticipation of a nuclear detonation, techniques to quickly assess the radiation exposure of evacuees should be developed. Based on experience relating neutron radiation exposures to activation products, measurement of activation products can be performed in a few minutes. Personal items exposed to significant levels of radiation allows neutron dose assessment via the activation products. This approach allows prompt collection of important data on human exposure following a nuclear attack. Data collected will facilitate triage decisions for emergency medical treatment to ameliorate the radiation effects on exposed individuals. Activation experiments with everyday items exposed to a neutron source are presented.     

Monte Carlo simulation of PGNAA system for determining element content in the rock sample

The element content in rock sample can be determined by prompt gamma ray activation analysis technology. The neutron distributions under the conditions with different moderating materials, moderator size and distance from neutron source to lead-out hole were simulated using Monte Carlo method, and then the optimal structure parameters to get the highest thermal neutron flux was obtained. The PGNAA system with optimal parameters based on ²⁵²Cf neutron source was founded. In addition, the rock and element standard samples were irradiated by thermal neutron in this system. Moreover, the element content was calculated by processing gamma ray spectroscopy recorded, and it is in agreement with result of XRF method.     

Improved ease of operation in epithermal NAA by irradiation in plastic capsules and use of well-type Ge-spectrometry: A feasibility study

An epithermal neutron activation analysis (ENAA) procedure has been evaluated in which samples packed in polyethylene capsules are irradiated during 15 minutes only, and induced activities are counted using well-type Ge-spectrometry. The evaluation was carried out in order to improve on ease of operation in ENAA. Biological and sediment reference materials have been analyzed. Compared to routine INAA, an improvement in detection limits was observed for As, Au, Cd, Mo, Ni, Sb, Sm, Sr, Ta, U, W and Zn. By Au–Zr neutron flux monitors, epithermal flux gradients have been determined. Concentrations found in the reference materials were generally in agreement with certified and consensus values.     

Determination of rare earth elements in rice by INAA and ICP-MS

In order to improve the accuracy of reactor neutron activation analysis, flux gradients and spectrum changes in the irradiation capsule have been studied at the Kyoto University Reactor (KUR). The flux and spectrum monitoring samples of Fe, Co, Au, Sb, U and Ni were placed at several positions in a polyethylene irradiation capsule of 24 mm inner diameter and 98 mm length, and were irradiated in a pneumatic irradiation facility (Pn-2). The flux gradients were found to be rather negligible in the vertical (axial) direction while they were considerable in the radial one. The flux gradient was around 5%/cm for thermal neutrons and 10%/cm for epithermal and fast neutrons. The spectrum changes were dependent on the materials (polyethylene and silica) filled in the capsule. Based on these observations, the effect of the flux gradients and spectrum changes on the accuracy of reactor neutron activation analysis was discussed.     

Design considerations for a neutron generator-based total-body irradiator

Summary The prompt- and delayed-gamma neutron activation techniques have been used for the non-invasive measurement of human body composition. In recent years, neutron irradiators have used only transuranic isotopic sources (^{238PuBe, 241}AmBe, ²⁵²Cf). However, in today’s security-minded environment, the use of alternate neutron sources may provide some advantages. We have examined several designs for an irradiator that would use a high-output, miniature D-T neutron generator (MF Physics). The use of this type of neutron source will lessen the storage, security, and transport issues associated with continuous-output isotopic neutron sources. To determine the scientific impact of this decision, we have performed Monte Carlo simulations (MCNP-4B2; Los Alamos National Laboratory) to aid in the design of the irradiator system, evaluating shielding materials, collimation, and source-to-subject distance, for the measurement of total body nitrogen (TBN). Based on internal flux distributions within the simulated body region of a subject, several design options were identified. The final design will be selected based on the optimization of precision, dose, and exposure time.     

Determination of the trace element levels in atmospheric pollutants by neutron activation analysis

An investigation of the potentials of neutron activation analysis for the routine analysis of trace elements present in atmospheric pollutants is discussed. Various techniques including sequential air sampling, multiple neutron irradiation, high resolution γ-ray spectrometry, chemical isolation, high flux neutron irradiation and X-ray spectrometry have been employed to determine the levels of Pb, Al, V, I, Cl, Mn, Cu, Br, Na, La, Mo, Au, Cr, Fe, Ni, Se, Zn, Ag and Co in atmospheric pollutants. The results of the analysis of nearly two hundred samples collected from the Buffalo New York area during 1968–1969 are reported. Presented at the Fourth Annual Conference on Trace Substances in Environmental Health, University of Missouri, Columbia Missouri, USA (June, 1970).     

Application of CR-39™ SSNTD with a boron converter for the characterization of the external neutron beam of a powder diffractometer

In this work, the solid state nuclear track detector (SSNTD) CR-39? has been used in combination with a boron converter screen for the characterization of the neutron distribution in the neutron powder diffractometer of the Es-Salam research reactor. A relationship between the track density in the CR-39? and the neutron flux distribution has been established by a mathematical development. Good agreement was found between the distribution of the thermal neutron flux determined by CR-39? detector and the distribution measured by the activation of Dysprosium foils. On the other hand, the degree of homogeneity of the neutron beam has been determined by the SSNTD and direct neutron radiography techniques. The results obtained by both techniques showed a depression of the flux at the left bottom region of the beam.     

Non-destructive determination of zinc in biological certified reference materials

Non-destructive neutron activation analysis was employed to determine zinc in ten biological standard reference materials from the National Bureau of Standards and the National Research Council of Canada. The use of a 4 h. irradiation at a medium neutron flux allows excellent accuracies, precision and sensitivities to be attained for all the samples analyzed. It is suggested that neutron activation analysis be one of the benchmark methods for the determination of zinc in biological reference materials for concentrations as low as the one part per million level.     

Performance of NAA Methods in an International Interlaboratory Reference Material Characterization Campaign

An extensive database of analytical results from a recent biological matrix Reference Material Characterization Campaign permitted an intercomparison of the performances of various methods among each other and with "true" best estimate concentration values established for these materials. Six different variants of neutron activation analysis (NAA) methods were employed including: instrumental neutron activation analysis, instrumental neutron activation analysis with acid digestion, neutron activation analysis with radiochemical separation, neutron capture prompt gamma activation analysis, epithermal instrumental neutron activation analysis, and neutron activation analysis with preconcentration. The precision and accuracy performance of NAA-based analytical methods are compared with three other major techniques, atomic absorption spectrometry (AAS), atomic emission spectrometry (AES) and mass spectrometry (MS) for 28 elements in 10 natural matrix materials.     

Evaluation of measurement uncertainty components associated with results of radiochemical neutron activation analysis for determination of uranium traces

Being aware of the importance to consider every step in the evaluation of the combined measurement uncertainty of the result, the purpose of this work was to evaluate the contribution of the radial thermal neutron flux gradient to the uncertainty budget for trace level uranium determination in biological materials by a radiochemical neutron activation analysis (RNAA). Determination of uranium via the short-lived nuclide ²³⁹U was based on solvent extraction with TBP and measurement of the chemical yield from the gamma-ray spectrum of the isolated fraction via ²³⁵U. It has been shown previously, that radial neutron flux gradient, could have a relevant effect on the final result obtained by RNAA. In the present work, radial neutron flux gradient within the irradiation assembly generally accepted in our lab (standards tapped beside the sample), varied between 93 and 108% around the mean value and contributes approximately 20% to the combined measurement uncertainty of the result.     

Flux calculation in LSNAA using an <Superscript>241</Superscript>Am-Be source

The CITATION code based on neutron diffusion theory is used for flux calculation inside voluminous sample in prompt gamma activation analysis with an isotopic neutron source (²⁴¹Am-Be). The code used the specific parameters related to energy spectrum source, irradiation system materials (shielding, reflector, etc.), geometry and elemental composition of the sample. The flux distribution (thermal and fast) was calculated on three-dimensional geometry for the system: source, air, and polyethylene and water cylindrical sample of 125 liters. The thermal flux was calculated in series of points inside the sample, and agreed with the results obtained by measurements with good statistical uncertainty. The maximum thermal flux was measured at distance of 4.1 cm and calculated at 4.3 cm by the CITATION code. Beyond a depth of 7.2 cm, the ratio of thermal flux to fast flux increases up to twice and allows us the optimization of the detection system in the scope of in-situ PGNAA.     

Evaluation of high purity graphite sample containers for use with rapid instrumental epithermal neutron activation analysis

The suitability of graphite of spectral quality as a sample container in short irradiations for neutron activation analysis has been investigated. The material is found to be a viable alternative to polyethylene containers especially in high flux irradiation positions where the properties of the latter deteriorate as a result of high neutron and gamma dose rates. Examples of application are demonstrated in epithermal neutron irradiations of biological materials and the accuracy and precision of the determinations were assessed.     

Intercomparison and determination of environmental standard samples by instrumental neutron activation analysis

To identify and improve the analytical technique for air pollution research, four kinds of environmental standard samples, i.e., airbome particulate matter, coal flyash, soil and pine needle supplied from the NIST and the IAEA were analyzed using thermal and epithermal neutron activation techniques. Sample irradiation was done at the irradiation facilities (neutron flux, 1 · 10¹³ n·cm^–2·s^–1) of the TRIGA MARK-III Research Reactor in the Korea Atomic Energy Research Institute. The accuracy and precision for the analysis of 40 trace and toxic elements in the samples were compared with the certified and reported values, respectively. In the analytical results of all standard reference materials, the relative standard deviation were within the 15% except for 11 elements and the relative error were agreed within the 10–20% except for 13 elements. The benefit of epithermal activation was investigated and the optimum analytical condition is reported.     

Analysis of selenium in environmental and biological samples by neutron activation

This paper presents the results of the application of a fast rabbit system and a high thermal neutron flux to neutron activation analysis of selenium in environmental samples. The short-lived radionuclide^77mSe, (17.5s) is used for analysis. Results are presented for selenium in sea-water and rain-water, in biological reference materials, in food-stuffs and milk powder, in human hair and human blood-serum.     

A new approach to single-comparator instrumental neutron activation analysis

A new parametric approach to single-comparator instrumental neutron activation analysis (INAA) at the University of Missouri Research Reactor (MURR) was investigated. A detailed MCNP steady-state model of the MURR core was developed using the latest neutron data libraries to compute the continuous-energy neutron flux distribution. Intrinsic reaction rates were predicted by coupling the computed local flux distribution to the isotopic (n, γ) excitation functions for a range of elements present in standard reference materials (SRM). Using the predicted (n, γ) reaction-rates, the concentrations for the various elements were determined. The method worked well for all nuclides tested, including those with cross sections that are not proportional to 1/v such as Lu and Eu with agreements for most elements within 5% of the reference value.