Radiochemical and instrumental neutron activation analysis procedures for the determination of low level trace elements in human livers

A comprehensive approach to the analysis of human livers was developed in a pilot program for the National Environmental Specimen Bank that employed a combination of four analytical techniques. Refinements in this approach were needed for improvement in detection limits, more effective sample usage and to reduce the number of analytical steps that were involved. Since neutron activation analysis (NAA) had determined most of the elements, expansion of NAA was chosen to achieve these goals. Modifications in the instrumental NAA procedures, including the use of a Compton Suppressor System, gave increased sensitivity for some low level elements, such as arsenic and chromium. Radiochemical procedures that followed the instrumental counts increased the sensitivity for the elements chromium, selenium, arsenic, molybdenum, silver, antimony, and tin. Results are given for two radiochemical procedures that were applied following the modified procedure, either the use of an inorganic ion exchange column or a liquid/liquid extraction, and these are compared to instrumental results.     

Analytical radiochemistry of neutron activated samples in practice

Analytical radiochemistry of neutron-activated samples, as practiced during past decades at the Jo?ef Stefan Institute Ljubljana, is outlined. The paper reviews achievements made in both elemental analysis and analyses of long-lived radionuclides, in variety of sample types. The presented analytical procedures include application of diverse chemical separations, multiple irradiations of samples, use of various nuclear reactions and detection modes for particular measurands, and determination of elements that are difficult to be determined by neutron activation analysis (NAA). Useful practical applications of neutron-activated tracers for chemical yield determinations, as unique feature of radiochemical NAA in comparison with non-nuclear analytical methods, are also addressed.     

Challenges and successes in the use of neutron activation analysis procedures for value assignment of animal serum and bovine liver Standard Reference Materials

Analyses for value assignment in the renewal Standard Reference Materials^® SRM 1598a Animal Serum and SRM 1577c Bovine Liver included extensive characterization by neutron activation analysis (NAA). Conventional instrumental NAA procedures were complemented by pre-irradiation chemical separations for the determination of Al, V, Mn, and Cu, radiochemical separations for the determination of Ag, As, Cd, Cr, Cu, Mo, Sb, and Se, and the use of (anti-) coincidence gamma-ray spectrometry systems for the instrumental determination of Ag, Cr, and Hg. The previous materials, SRMs 1598, 1577, and 1577b, were analyzed together with the new materials for quality control.     

Fast neutron activation analysis at Texas A&M University

Fast neutron generators are used at Texas A & M University to provide a supply of high energy neutrons for nuclear analytical measurements. A series of neutron activation analysis procedures have been developed for determining various major, minor and trace constituents in a variety of materials. These procedures are primarily developed to compliment our reactor based NAA program, thereby expanding the list of determinable elements to include those difficult or impossible to measure using thermal neutrons. A few typical methods are discussed. The unique implementation of the methodologies at Texas A & M are explained.     

A multiple time-gated system for pulsed digital gamma-ray spectroscopy

Neutron activation analysis (NAA) systems that use pulsed neutron generators (NGs) employ spectrum gating procedures to segregate nuclear processes by acquiring gamma-ray spectra separately when the generator is on (HIGH gate) and off (LOW gate). Often, the actual neutron burst lags the leading edge of the HIGH gate signal by a few μs. Thus, count rates vary not only between the on and off states of the NG, but within them as well. Recent advances in digital gamma-ray spectrometers that allowed the concurrent acquisition of data by sorting events into two separate spectra based on gate status suggested that a time-resolved analysis that further subdivided the neutron pulse cycle could obtain further information to separate gamma-rays produced by different nuclear reactions. In this paper we introduce a gating system for time-resolved NAA that is capable of concurrently acquiring as many as 16 spectra from up to 8 user-defined time intervals during each of the HIGH gate and LOW gate periods, each with all required timing and count rate information. We present the new gating system’s implementation, operation and some first experimental test results.     

Nuclear activation methods for the characterization of fossil fuels

A review is presented on the use of neutron activation analysis (NAA) for the analyses of coal, oil shale, tar sands and petroleum. Fast NAA has been widely used for the determination of oxygen, and to a limited extent, of other elements such as nitrogen and silicon. Reactor NAA followed by instrumental counting, and in specific cases, after radiochemical separations is discussed. Thermal and epithermal neutrons are both used. Limited use of the²⁵²Cf source has been made in fuel analysis. A complementary technique to NAA is the photon-activation analysis with linear accelerator. It can determine over thirty elements, many of them not possible to do by NAA. Round-robin analyses of standard coal, fly ash, or oil shale samples indicate nuclear activation methods are comparable in accuracy and precision to X-ray fluorescence or atomic spectrometric methods for most elements.     

Comparison of the role of photon and neutron activation analyses for elemental characterization of geological,biological and environmental materials

The potential of photon activation analysis (PAA) for multielement trace analysis can hardly compare with that of neutron activation analysis (NAA). However, PAA appears superior over NAA for the determination of a number of elements, namely C, N, O, F, Mg, Si, Ca, Ti, Ni, Sr, Y, Zr, Nb, Sn, Tl and Pb in geological, environmental and biological materials. Most of these and other elements can be determined using nondestructive, instrumental PAA (IPAA), especially in geological materials. The possibilities of IPAA for multielement analysis using photoexitation and other photonuclear reactions are reviewed and compared with those of instrumental NAA (INAA), namely for geological materials. The need for and usefulness of radiochemical PAA (RPAA) procedures are also discussed.     

Arsenic speciation: HPLC followed by ICP-MS or INAA

Sensitivities for the measurement of four arsenic species, As^III, As^V, monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA), in environmental waters and rice extracts by a new neutron activation analysis (NAA) method using pre-separation of the species by liquid chromatography were determined. A manual fraction collection was used to isolate the species, followed by instrumental neutron activation analysis procedures. The sensitivities determined for arsenic species in the samples varied from 1.21 to 1.47 ng per vial or about 30 μg·L⁻¹ in sample solutions which translates to about 900 ng arsenic per gram of rice for our HPLC-NAA experiments.     

Inteferences in neutron and photon activation analysis

The effect of following interferences was quantitatively assessed in terms of interference factor by irradiating samples together with highly pure reagents at two reactor sites of diferent neutron spectra and fluxes for neutron activation analysis (NAA) and an electron LINAC for photon activation analysis (PAA). The interfering reactions studied are 91) fast neutron-induced reactions, (2) uranium fission (3) (n,γ) reactions of other target elements in NAA, and (4) reactions induced by secondary neutrons in PAA. Corrections for these interferences were successfully applied to the activation analysis of some geological reference rock samples and biological samples.     

Opportunities for innovation in neutron activation analysis

Neutron activation laboratories worldwide are at a turning point at which new staff has to be found for the retiring pioneers from the 1960s–1970s. A scientific career in a well-understood technique, often characterized as ‘mature’ may only be attractive to young scientists if still challenges for further improvement and inspiring new applications can be offered. The strengths and weaknesses of neutron activation analysis (NAA) are revisited to identify opportunities for innovation. Position-sensitive detection of elements in large samples, Monte Carlo calculations replacing the use of standards, use of scintillator detectors and new deconvolution techniques for increasing the sensitivity are examples of challenging new roads in NAA. Material science provides challenges for the application of NAA in both bulk samples, ultrathin layers and ultrapure materials.     

Forty-five years of neutron activation analysis in Slovenia: achievements towards improved quality of measurements results

Main achievements towards improved quality of measurements results obtained by neutron activation analysis (NAA) at the TRIGA Mark II reactor of the Jožef Stefan Institute during its 45 years of continuous operation are reviewed from a historical perspective; emphasis is on the features specific for NAA. The development of radiochemical neutron activation analysis for characterising reference materials is described in detail in the first part. Several approaches specific for the method such as the determination of long-lived radionuclides, the simultaneous determination of several elements using double irradiation and the internal standard method are presented in more detail. Several interesting approaches such as combination with liquid scintillation counting detection and combination with radiometric measurements are outlined. Then, the development of instrumental neutron activation analysis, specifically the k ₀-NAA based method is discussed. The contribution towards methodological development of uncertainty assessment is outlined, and the importance of the nuclide-specific and neutron fluence-specific approach is emphasised. Throughout the paper, the importance of neutron activation analysis and contributions of measurements results obtained by this method to characterising (candidate) reference materials is shown.     

Advances in Radiogeochemistry

The applications of reactor thermal and epithermal neutron activation analysis (NAA) to geological materials are reviewed. These include the historical development of radiochemical (destructive) (RNAA) and instrumental (non-destructive) (INAA) methods, the counting systems, epithermal neutron activation. Special attention is given to reference materials and the place of NAA in the firmament of geoanalytical techniques for their certification and characterization. Literature references useful in NAA of geological materials are listed.     

Application of different activation analysis techniques for determination of trace elements in human blood

One of the requirements of stable isotope tracer technique is detection of two isotopes of same element. It is preferable to use instrumental techniques in order not to contaminate the samples. Different instrumental nuclear techniques namely neutron activation analysis (NAA), photon activation analysis (IPAA), and prompt gamma ray activation analysis (PGAA) were tried on human blood samples. The techniques were found to be complementary to each other, NAA being the most sensitive of the three. Zinc is choosen for validation work among the three feasible elements (Zn, Cr, Se) for stable isotope tracer technique. As NAA was not sufficient to detect two isotopes of Zn, a radiochemical separation scheme was developed later.     

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.     

Determination of cadmium in Arctic air filters by epithermal neutron activation analysis and Compton suppression

Arctic pollution is a problem of great concern, because its characteristics (transportation, assimilation into the environment, etc.) are complex and not fully understood. Detection of elemental constituents has been undertaken through the use of neutron activation analysis and Compton suppression (to lower the detection limits for radionuclides characteristic of mainly single gamma-ray emission) to discover possible pollutant sources. The goal of this project was to perform a feasibility study to determine the suitability of neutron activation analysis (NAA) to evaluate cadmium concentrations on air filters collected in the Arctic.     

Nuclear-related analytical techniques: Literature retrieval from the INIS database

The applicability of the INIS database for literature retrieval on nuclear-related analytical techniques [e.g. neutron activation analysis (NAA), X-ray fluorescence (XRF), particle-induced X-ray emission (PIXE)] has been studied. There exist about 9700 documents on NAA and other forms of activation analysis, about 3500 documents on XRF and about 1200 documents on PIXE in the database collected from 1976 until July 1988. They cover a variety of elements and matrices in the fields of biology, geochemistry and the physical sciences. Some technical notes and comments on the practical use of this database are also included.     

Optimization of Linac-based neutron source for thermal neutron activation analysis

Journal of Radioanalytical and Nuclear Chemistry - A 20 MeV electron Linac based neutron beam has been shaped for neutron activation analysis (NAA) technique. A beam shaping assembly (BSA)...     

Utilization of pneumatic carrier facility of Dhruva reactor for trace element determination by neutron activation analysis

The pneumatic carrier facility (PCF) of Dhruva reactor is being extensively used for neutron activation analysis (NAA) studies pertaining to research work as well as routine sample analysis. It is useful for the determination of trace elements using short and medium half-lives radioisotopes produced in neutron activation with available higher neutron flux (~5 × 10¹³ cm^?1 s^?1). Solid samples placed in high density polypropylene capsule, are irradiated for 1 min duration and radioactive assay is carried out by high resolution gamma ray spectrometry. Design aspects of PCF and various applications to samples of diverse matrices using NAA are presented.     

An automated facility for neutron activation analysis

A fully automated neutron activation analysis (NAA) facility has been constructed at the Whiteshell Nuclear Research Establishment. This high-capacity facility has been designed for use with a wide variety of neutron sources, including Canada's SLOWPOKE II and MAPLE research reactors. Its pneumatic transfer system is driven by a Square-D Model 500 programmable controller, linked in turn to a Nuclear Data ND6700 computer/spectrometer. Custom software for data entry and system control has been combined with Nuclear Data software for gamma-spectrum acquisition and processing to create a flexible, easy-to-use facility for NAA. Its design and performance are discussed.