Determination of characteristic neutron flux parameters of nuclear reactors for thermal neutron activation analysis

The characteristic neutron spectrum parameters for thermal neutron activation analysis have been determined for the most important irradiation positions of the reactors BR1 and BR2 at Mol (Belgium), HFR at Petten (Netherlands) and FRJ2 at Jülich (Federal Republic of Germany). The method of determination is described.     

Applications of synchrotron radiation in materials analysis

The synchrotron radiation (SR) emitted by circulating high-energy electrons has extraordinary properties: The light is intensive and bright, it is tunable and highly collimated, and finally, it is linearly polarized. These exceptional properties have initiated a unique revival of many spectroscopies using electromagnetic radiation. The techniques of special concern for materials analysis which are treated in this article are: X-ray absorption, reflection, fluorescence, diffraction and topography. A number of examples will be given in order to illustrate the possibilities of these techniques when SR is used.On leave of absence from Institut für Festkörperforschung, KFA Jülich, D-5170 Jülich, Federal Republic of Germany     

Determination of the chain conformation of polypropylene in the crystalline state by neutron scattering

Summary Wide and small angle neutron scattering from melt-crystallised isotactic polypropylene mixtures of deuterated and protonated molecules were measured in aQ range of 0.003 Å^–1 to 0,8 Å^–1. The scattering curves between 0.1 Å^–1 and 0.8 Å^–1 are very sensitive to the amount of folding of the chains within a lamella. Different annealing conditions which influence the degree of crystallinit between 0.39 and 0.67 and the long spacing between 125 Å and 245 Å had an insignificant influence on the scattering in this range. For various arrangements of crystalline sequences scattering functions were calculated. Best agreement with the experimental scattering curves was obtained for a mixture of single and double crystalline sequences of equal proportion. An adjacent reentry folding model for the molecular conformation is not consistent with the experimental data.The neutron scattering experiments have been performed at the Institute Laue-Langevin in Grenoble/France and at the Kernforschungsanlage Jülich/Germany.     

The single-comparator method in thermal neutron activation analysis extended for some (n,p) reactions

From experimental studies of the rate of the reactions⁴⁷Ti(n, p)⁴⁷Sc,⁴⁸Ti(n, p)⁴⁸Sc and⁵⁸Ni(n, p)⁵⁸Co in four nuclear reactors, it is concluded that for the irradiation positions of the light water moderated reactors BR2 (Mol, Belgium) and HFR (Petten, Netherlands) a simple empirical relation exists between the fast neutron flux on the one hand and the thermal and epithermal neutron flux on the other. The graphite moderated reactor BR1 (Mol, Belgium) and the heavy water reactor FRJ2 (Jülich, Federal Republic of Germany), however, have relatively much lower fast fluxes and their irradiation facilities do not obey the empirical relation determined.     

Neutron activation analysis at the research reactor center of IPEN/CNEN-SP- biological and environmental applications

The Research Reactor Center (CRPQ) of IPEN/CNEN-SP operates the IEA-R1 Research Reactor, at a nominal power of 2 MW thermal, on a 64 hour per week continuous cycle. The IEA-R1 is a pool type reactor, moderated and cooled by light water, with graphite as a reflector. One of the main activities of CRPQ is the neutron activation analysis, which is applied to many fields of research, in collaboration with other institutes and universities. The Research Reactor installations are also intensely used for human resources development in the field of radiochemistry and neutron activation analysis, at graduate and post-graduate levels. In the present paper, an overview will be presented of some of the neutron activation analysis research lines that are being developed, comprising environmental and health-related applications. This revised version was published online in August 2006 with corrections to the Cover Date.     

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.     

Aspects of cleaning environmental materials for multi-element analysis, e.g. plant samples

Summary Cleaning of samples is often the first step in the entire procedure of sample preparation in environmental trace element research. The question must generally be raised of whether cleaning is meaningful before chemical investigations with plant material (e.g. for the determination of transfer factors in the soil/plant system) or not (e.g. for food chain analysis in the plant/animal system). The most varied cleaning procedures for plant samples are currently available ranging from dry and wet wiping of the leaf or needle surface up to the complete removal of the cuticule with the aid of chloroform. There is at present no standardized cleaning procedure for plant samples so that it is frequently not possible to compare analytical data from different working groups studying the same plant species.Modified paper presented at the IAEA training course on Sampling, sample preparation and data evaluation for multielement and radionuclide analysis by nuclear and instrumental methods from November 6th to December 1st 1989 at the Research Centre in Jülich, FRG     

Collection, preparation and characterization of fresh, marine candidate reference materials of the German Environmental Specimen Bank

Summary The Environmental Specimen Bank (ESB) of the Federal Republic of Germany has been collecting and preparing specially selected biological reference materials since 1982 to help to control representative ecosystems. The preparation and homogenization of the sample material is carried out at cryogenic temperatures, below minus 150°C. There is a broad palette of fresh candidate RMs, stored at the ESB Jülich, characterized not only for special trace elements and essential bulk elements but also for polycyclic aromatic hydrocarbons (PAH) and chlorinated hydrocarbons (CHC). Just for organic analysis there is a need of fresh RMs, which can be filled by the ESB reference materials.     

Electrometric determination of the pH of atmospheric precipitation

Summary Reliable pH-determination of rain water represents a difficult task both from the theoretical and practical point of view because the chemical composition and conductivity of rain water samples varies widely. The method for determining the pH is described that was used during our systematic study of the acidity of rain in various regions of the FRG from 1980 to 1985 and the problems encountered are discussed. Potential sources of error are inadequate sampling, sample storage, and electrometrical pH-determination of samples with a very low conductivity. The use of various types of electrodes, their pretreatment, storage and time response as well as the accuracy of the determination are discussed. Examples are given of the application of the method for determining the time dependence of the pH during single rain events in Jülich as well as average monthly pH-values in polluted and nonpolluted regions in the Federal Republic of Germany.

---

Elektrometrische Bestimmung des pH-Wertes von atmosphärischen Niederschlägen

Zusammenfassung Eine zuverlässige Bestimmung des pH-Wertes des Regenwassers ist wegen unterschiedlicher Zusammensetzung und Leitfähigkeit des Regenwassers verschiedener Herkunft mit theoretischen und praktischen Problemen verbunden. Die während einer langzeitigen Meßreihe des pH-Wertes in verschiedenen Regionen der Bundesrepublik in den Jahren 1980–85 angewendete Methode wird beschrieben und die dabei auftretenden Probleme der pH-Bestimmung diskutiert. Die mangelhafte Richtigkeit ist vor allem auf die Probennahme, Probenlagerung und elektrometrische Bestimmung des pH-Wertes bei einer geringen Leitfähigkeit der Probe zurückzuführen. Verwendung verschiedener Elektrodentypen, ihre Vorbehandlung, Lagerung, Einstellungszeit und Genauigkeitsgrenzen des Meßwertes werden erörtert. Als Beispiel der Verwendung der Meßmethode werden Resultate aus der pH- und Leitfähigkeitsbestimmung in einzelnen Regenvorgängen in Jülich und in durchschnittlichen Monatsproben aus verschiedenen belasteten und nicht belasteten Regionen der Bundesrepublik angeführt.

     

Neutron captue prompt gamma-ray activation analysis at the NIST Cold Neutron Research Facility

An instrument for neutron capture prompt gamma-ray activation analysis (PGAA) has been constructed as part of the Cold Neutron Research Facility at the 20 MW National Institute of Standards and Technology Research Reactor. The neutron fluence rate (thermal equivalent) is 1.5·10⁸ n ·cm^–2·s^–1, with negligible fast neutrons and gamma-rays. With compact geometry and hydrogen-free construction, the sensitivity is sevenfold better than an existing thermal instrument. Hydrogen background is thirtyfold lower.     

Neutron damage of hexagonal boron nitride: h-BN

Hexagonal boron nitride (h-BN) was neutron damaged at an integral flux of 2.40 × 10¹² n cm⁻² s⁻¹ for 1, 2, 3 and 4 h. The h-BN samples undergo a transition from sp² to sp³ hybridization as a consequence of the neutron induced damage with the formation of cubic boron nitride (c-BN) spots, as suggested both by FT–IR and Raman spectroscopy. In addition to c-BN, also a certain degree of amorphization is achieved by h-BN already at the lowest neutron fluence of 8.64 × 10¹⁵ n cm⁻² as clearly evidenced by Raman spectroscopy. The Wigner or stored energy to the radiation-damaged h-BN samples was studied by DSC and also in this case there was a clear evidence that the neutron damage was partly irreversible and insensitive to the thermal annealing up to 630 °C. Electron spin resonance (ESR) was employed to further study the structural defects induced by the neutron bombardment of h-BN. Two kinds of paramagnetic defective structures centered on ¹¹B atoms were identified.

     

Rapid separation of mercury,arsenic, thallium and chromium species

Radiochemical neutron activation analysis is the only method to determine the galactic cosmic ray (GCR) produced radionuclide⁵³Mn (T=3.8·10⁶) in small meteorite samples. A large number of such samples was analyzed using extremely thermalized neutrons of the DIDO reactor at the KFA Jülich. The detection limit of 10^–14 g/g was recently achieved in our laboratory through the improvement of pre- and postirradiation chemistry. The main purpose of our studies of meteorite finds from Antarctica and the Southwestern United States is to establish their exposure ages up to 12·10⁶ a by means of⁵³Mn. Especially in the case of Antarctic meteorites terrestrial ages up to several 10⁵ years have been observed by combining⁵³Mn and²⁶Al (T=7.2·10⁵ a) measurements.     

Direct determination of atmospheric lead by Zeeman solid sampling graphite furnace atomic absorption spectrometry (GFAAS)

Summary Atmospheric lead was collected by membrane filters using two low volume air samplers at Jülich, Stolberg, and Wetzlar, Federal Republic of Germany. Sampling times varied from 2 to 8 h. After sampling, each filter was subsampled in two cross-sections using a clean stainless steel punch (diameter 5 mm). The lead content of each subsample disc was determined directly by Zeeman GFAAS, calibrated with aqueous standard solutions and supported by solid reference materials. The distribution of lead between the subsamples was generally homogeneous, with standard deviations ranging from 11 to 37%, but typically <15% for samples with 8 h sampling time. The analysis of each filter usually took about 30 min. The differences in air quality between the three sampling locations, as measured by the lead concentrations, are discussed. In general, Stolberg appears to have the highest lead concentrations. The mass particle-size distribution of lead in the aerosol samples collected by membrane filters using a cascade impactor at Stolberg was also investigated with the same analytical technique. Using graphite platform boats as direct samplers, it is possible for the dry deposition flux of lead to be estimated. This provides a quick means of assessing the levels of lead pollution in the atmospheric environment. With lead concentrations measured in parallel, the dry deposition velocities of lead can be estimated under various meteorological conditions. Application of similar sampling and analytical techniques to other atmospheric trace metals may be possible.     

Reference materials for chemical analysis. Highlights on the activity of JRC-Ispra laboratories

Summary Within the framework of a program of the Community Bureau of Reference concerning the preparation of compositional reference materials, examples are given of the activities of the Chemistry Division of the Joint Research Centre — Ispra Establishment, relating to the homogeneity verification, the analytical characterization and the derivation of consensus values of various constituents of different reference materials.

---

Referenzmaterialien für die chemische Analyse. Besondere Aktivitäten der JRC-Laboratorien, Ispra

Zusammenfassung Beispiele werden gegeben zu den Aktivitäten der chemischen Abteilung des Forschungszentrums Ispra, die im Rahmen eines Programms des Europäischen Büros für Referenzmaterialien Arbeiten zur Herstellung solcher zusammengesetzter Materialien durchführt. Diese beziehen sich auf die Homogenitätsprüfung, sowie die analytische Charakterisierung und Ableitung des maßgebenden Wertes für verschiedene Bestandteile unterschiedlicher Referenzmaterialien.

Presented at Euroanalysis III conference, Dublin, 20–25 August, 1978     

Quantitative electron probe microanalysis for the characterization of thin carbon-boron layers in fusion devices

Summary The first wall of the fusion device TEXTOR at the Forschungszentrum Jülich has been coated in situ with an amorphous hydrogen rich carbon/boron film (a-C/B:H) which reduces plasma impurities caused by the plasma surface interaction. The results of the coating process of the 35 m² large inner wall surface have been controlled by a recently developed modification of the quantitative electron probe microanalysis, which has been applied to 12 samples from specified positions inside the tokamak. The quantification itself is based on a Monte Carlo simulation of electron trajectories providing very accurate results for X-ray intensities emitted by elements present in the electron bombarded sample. The Monte Carlo results are used in the present work to calibrate the measured X-ray intensities emitted by boron and carbon from the a-C/B:H layers deposited on pure silicon substrates. As a result the total deposited mass of the layer per area unit as well as the composition of the layers (except hydrogen) could be determined very accurately. The relative errors were less than 7%. The limit of detectability were found to be in the range of one monolayer for boron as well as for carbon.     

Direct solid vs. slurry analysis of tobacco leaves for some trace metals by graphite furnace AAS

Summary Graphite furnace atomic absorption spectrometry (GFAAS) is used to determine cadmium, lead, nickel and cobalt in two samples of tobacco leaves (candidate reference materials). Two techniques for the direct determination of these elements are investigated — direct solid sampling into a ring chamber tube specially designed for the Zeiss AAS-3 spectrometer and slurry sampling. For both investigated sampling methods the optimum parameters of temperature-time programs, influence of Pd modifier and calibration methods are discussed. There is acceptable agreement between the results obtained from direct solid, slurry and solution (after wet decomposition) sampling.Presented at the 4th International Colloquium on Solid Sampling with Atomic Spectroscopy, October 8–10, 1990; Jülich, Federal Republic of Germany     

Trace analysis by intermediate trapping with a modified programmable temperature vaporizer

Summary A system for quantitative transfer of thermally desorbed substances onto capillary columns is described. During desorption substances are intermediately trapped in a programmable temperature vaporizer (PTV) cooled to –150°C. After condensation the injector is heated to a preset temeprature in a few seconds. Various applications are mentioned.Extract from planned Thesis of E. Jülich with authorization of the Faculty     

Neutron activation analysis without multielement standards

A physical approach is described for instrumental multielement activation analysis with whole neutron spectrum (without Cd-cover) using the monostandard (single comparator) method. To test the capabiliteries of this method, 15 samples representing different Egyptian granite rocks were analyzed. As many as 21 trace elements beside Fe, K and Na were determined. Calculation of the experimental data has been done using the Gamma-Monostandard Analysis program with the Commodore Computer available at the Institute of Radiochemistry at Garching near München. The accuracy of the method for nondestructive multielement analysis agrees within 3% with the relative method using multielement standards.     

Design Features of a Prompt Gamma Neutron Activation Analysis System at HANARO

The design features are described of a prompt gamma neutron activation analysis system at HANARO, a 30 MW research reactor in the Korea Atomic Energy Research Institute. The beam consists of polychromatic thermal neutrons diffracted by a set of pyrolytic graphite crystals at orders n in the range 1n6 at a Bragg angle of 45° on a horizontal beam line. A neutron flux of 1.0·10⁸ n·cm^–2·s^–1 is calculated at the sample position from the reflectivity of the crystal which has been confirmed in a measurement of a diffracted neutron spectrum using a time-of-flight spectrometer and gold-wire activation. The fast neutron and gamma backgrounds will be low due to the use of a diffracted beam and a tapered collimator. The detection system comprises a 30% n-type HPGe detector, signal electronics and a fast ADC. The first application of this system will be the analysis of boron concentration in biological samples for neutron capture therapy. Construction of the beam line and the arrangement of the detection system is proceeding.     

The Role of Neutron Activation Analysis at The Dow Chemical Company

The role of neutron activation analysis (NAA) at The Dow Chemical Company has not changed significantly since the first operations, which were conducted in July, 1967. That role is threefold; provide results with appropriate precision, accuracy and sensitivity; provide results in a timely manner; and provide results for a reasonable cost. What has changed, are the requirements for satisfying each of the three components of the role. In a business-focused environment, analyses need to be performed faster with better sensitivity and/or precision and be more cost efficient. In order to meet these requirements, operations at The Dow TRIGA Research Reactor are devoted to NAA activities.