Applications of nuclear analytical techniques in human nutrition research as exemplified by research programmes of the international atomic energy agency

In human nutrition research, nuclear analytical techniques, particularly neutron activation analysis (NAA), are used mainly for thein vitro study of trace elements. According to work sponsored by the IAEA, up to 15 trace elements and 5 minor elements of nutritional interest may be determined in biological materials by NAA with good accuracy and precision. A programme is described in which NAA was used for the determination of 14 trace elements and one minor element in human milk. NAA also plays an important role in the certification of reference materials for nutritional studies.     

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.     

On the role of neutron activation analysis in the certification of a new reference material for trace-element studies,mixed human diet,H-9

A new biological reference material, which is representative of diets consumed in Finland, has been characterized by means of an intercomparison exercise conducted by the IAEA in the second half of 1985 and in 1986. Results for 35 elements received from 79 participants in 33 countries have been evaluated. A certificate of analysis has been issued with provisional certified values for 22 elements and information values for 2 elements. Neutron activation analysis (NAA) provided approximately one third of all the results reported. Instrumental NAA was used approximately 5 times as frequently as radiochemical NAA. Overall, NAA played an important role in providing useful data for the following 20 elements: Al, As, Br, Cl, Co, Cr, Cs, F, Fe, Hg, I, K, Mn, Mo, Na, Rb, Sb, Sc, Se and Zn. In comparison with the main competing non-nuclear method (usually atomic absorption spectrometry), NAA showed a larger dispersion of results for Cd, Cu, K, and Mg, and a smaller degree of dispersion for Co, Cr, Hg, and Se.     

Elemental analysis of a single-wall carbon nanotube candidate reference material

A material containing single-wall carbon nanotubes (SWCNTs) with other carbon species, catalyst residues, and trace element contaminants has been prepared by the National Institute of Standards and Technology for characterization and distribution as Standard Reference Material SRM 2483 Carbon Nanotube Soot. Neutron activation analysis (NAA) and inductively coupled plasma mass spectrometry (ICP–MS) were selected to characterize the elemental composition. Catalyst residues at percentage mass fraction level were determined with independent NAA procedures and a number of trace elements, including selected rare earth elements, were determined with NAA and ICP–MS procedures. The results of the investigated materials agreed well among the NAA and ICP–MS procedures and good agreement of measured values with certified values was found in selected SRMs included in the analyses. Based on this work mass fraction values for catalyst and trace elements were assigned to the candidate SRM.     

Analysis of the Arctic aerosol for a ten year period using various neutron activation analysis methods

During the past decade we have determined the concentrations of a variety of trace elements in the Arctic aerosol by using themal and epithemal neutron activation analysis (NAA). More recently we have employed Compton suppression NAA to lower the detection limits for radionuclides that are characteristic of single or mainly single gamma-ray emission. Using these various methods, we have been able to use elements such as indium and silicon. Furthermore we have achieved extremely low detection limits for iodine, arsenic and antimony. The usefulness of these NAA methods are discussed in a large sampling program that incorporates more than one thousand samples.     

Characterization of simulated vitrified highly active waste and its leachates by neutron activation

Neutron activation analysis (NAA) methods have been developed for the simultaneous determinations of multielement concentrations in various types of glass and their leachates. The epithermal instrumental NAA (EINAA) method involves the irradiation of samples in a Cd-shielded site for 2–5 min in order to determine levels of of up to 13 elements through their short-lived nuclides. Another 15 elements can be measured via their long-lived nuclides using conventional instrumental NAA (INAA). Accuracy of the methods have been evaluated by analyzing certified reference materials. The limits of detection for all elements are reported. The methods have been applied to sodium borosilicate and sodium calcium aluminosilicate glass samples in order evaluate their suitability as a host matrix for immobilizing high level radioactive waste.     

Application of the radioreagent method for yield determination in neutron activation analysis

A very convenient method for yield determination in NAA is the use of isotopic radiotracers. But for the majority of elements determinable by NAA no suitable isotopic radiotracers exist. For some of these elements the radioreagent methodoffers afvourable opportunity to use also non-isotopic radiotracers. An activation analytical copper determination method is described using a radioactively labelled reagent for correction of separation losses. Results of copper determinations in 8 international standard reference materials are given.     

Comparative analysis of ancient ceramics by neutron activation analysis,inductively coupled plasma-optical-emission spectrometry,inductively coupled plasma-mass spectrometry,and X-ray fluorescence

The accurate measurement of the maximum possible number of elements in ancient ceramic samples is the main requirement in provenance studies. For this reason neutron activation analysis (NAA) and X-ray fluorescence (XRF) have been successfully used for most of the studies. In this work the analytical performance of inductively coupled plasma-optical-emission spectrometry (ICP-OES) and inductively coupled plasma-mass spectrometry (ICP-MS) has been compared with that of XRF and NAA for the chemical characterization of archaeological pottery. Correlation coefficients between ICP techniques and XRF or NAA data were generally better than 0.90. The reproducibility of data calculated on a sample prepared and analysed independently ten times was approximately 5% for most of the elements. Results from the ICP techniques were finally evaluated for their capacity to identify the same compositional pottery groups as results from XRF and NAA analysis, by use of multivariate statistics.     

Adsorption of cobalt on some natural zeolites occurring in ČSFR

Neutron activation analysis is one of many analytical techniques used at the National Institute of Standards and Technology (NIST) for the certification of NIST Standard Reference Materials (SRMs). NAA competes favorably with all other techniques because of it's unique capabilities for high accuracy even at very low concentrations for many elements. In this paper, instrumental and radiochemical NAA results are described for 25 elements in two new NIST SRMs, SRM 1515 (Apple Leaves) and SRM 1547 (Peach Leaves), and are compared to the certified values for 19 elements in these two new botanical reference materials.     

Comparison of neutron activation analysis with other analytical techniques for the determination of inorganic constituents of milk powder

The contribution of different analytical techniques to the results of a recent IAEA intercomparison (A-11) of the determination of the inorganic constituents of a milk powder sample is discussed. In all, 43 laboratories from 24 countries reported results on 40 elements, “recommended” concentrations for 14 elements were established. NAA was the most important of the 9 techniques used in this run, it contributed 40% of all the results and all the results for 7 elements. Accuracy and precision of NAA proved to be good compared to those of other methods.     

Preliminary homogeneity study of in-house reference material using neutron activation analysis and X-ray fluorescence

Summary Although many biological reference materials for quality control of trace element analysis are commercially available, there is still a need for additional local materials for special matrices. In the Latin American region a preliminary study has been commenced involving analytical strategies for the characterization of in-house reference material. A biological sample, prepared in Brazil, constitutes the first regional attempt to prepare reference material. It was analyzed by neutron activation analysis (NAA) and X-ray fluorescence (XRF) to verify its homogeneity. The determination of the trace elements and certain major elements was carried out by instrumental NAA. Trace elements such as Cd, Mn, Mo and Cu were determined using NAA with radiochemical separations to improve the sensitivity and precision. XRF was applied only to major constituents and some trace elements with concentration of more than 10 g/g. From a total of 18 elements analyzed, only Fe, Cr and Sc were not homogeneously distributed.     

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.     

Different methodologies in neutron activation to approach the full analysis of environmental and nutritional samples

Different methodologies of neutron activation analysis (NAA) are now available at the Technological and Nuclear Institute (Sacavém, Portugal), namely Compton suppression, epithermal activation, replicate and cyclic activation, and low energy photon measurement. Prompt gamma activation analysis (PGAA) will be implemented soon. Results by instrumental NAA and PGAA on environmental and nutritional samples are discussed herein, showing that PGAA — carried out at the Institute of Isotope Research (Budapest, Hungary) — brings about an effective input to assessing relevant elements. Sensitivity enhancement in NAA by Compton suppression is also illustrated. Through a judicious combination of methodologies, practically all elements of interest in pollution and nutrition terms can be determined.     

Preconcentration of lanthanides from natural waters with a lipophilic crown ether carboxylic acid

Lipophilic crown ether carboxylic acids such as 2-(sym-dibenzo-16-crown-5-oxy)stearic acid with a cavity size comparable to the ionic radius of rare-earth elements are selective chelation agents for preconcentration and separation of lanthanides from natural waters for NAA. Interfering matrix elements such as sodium and bromine can be simultaneously eliminated during the extraction. The lanthanides can be back-extracted into a dilute acid solution for NAA, thus providing a large preconcentration factor. This two-step extraction method appears suitable for the determination of lanthanides in natural waters and in biological samples.     

New Developments in Activation Analysis for Material and Environmental Sciences

Activation analysis in general and mainly reactor neutron activation analysis (NAA) has been used extensively for measuring trace elements in high purity materials, particularly semiconductor materials. The advantages of NAA in determination of trace elements differ from one semiconductor material to another. For all of them the inherent properties of activation analysis especially those of non contamination with the reagents, low blanks and high sensitivity are the reasons for the choice of NAA as the main analytical procedure. These inherent properties are essential for analysis of high-purity materials where concentrations of ppb's and sub ppb's have to be measured. NAA is specially suitable for the determination of trace elements in silicon due to the very short lived very low activity induced by neutron reaction in silicon. This enables easy instrumental (i.e. without chemical separations) determination of trace elements in silicon. In the HFR reactor at Peten, Netherlands, a special facility was constructed for irradiation of silicon samples of Philips, in which silicon wafers of up to 15 cm diameter can be irradiated with 4 × 10¹³n. cm^?2. sec^?1 and the irradiation is done for 72–96 hours. using large Ge(Li) detectors (100 to 150cc) and long counting time (8–16 hours) they measured 22 elements in concentrations below ppb and 10 others between ppb and 300 ppm. Trace elements in germanium have been determined both instrumentally after very long decay time (100 days) or after short decay time removing the activities from the matrix by chemical separation. Trace elements in GaAs are determined only after chemical separtion. Several other semiconductor material such as Sc, Te, GaP and CuInS₂ were also determined by NAA. Some trace elements cannot be determined by neutron activation. Carbon, nitrogen and oxygen are determined by activation with protons, alphas or ³He particles. Boron and hydrogen are determined by prompt emission induced by charged particle activation, which gives not only the total concentration but also the depth profile. Carbon, nitrogen, oxygen and phosphorus were also determined by prompt proton activation analysis. The environmental samples studied by activation analysis can be divided into three categories: atmospheric aerosols, water samples and solid wastes. NAA of atmospheric aerosols have been used for their posible toxicological hazards, their source identification and for studies of atmospheric transport processes.     

Aktivierungsanalytische Beiträge zur Geochemie der Regionalmetamorphose

In order to investigate the behaviour of elements during the progressive regional metamorphosis 28 elements have been determined by radiochemical and instrumental NAA. The concentrations are determined in different stages of metamorphosis. The results enable us to classify the 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.     

Use of NAA in marine environment and in archaeology in Greece

Neutron activation analysis (NAA) is a very sensitive and accurate multielement analytical method that is widely applied to the investigation of environmental and archaeological problems. The first part of this paper is a review of pollution studies of toxic trace elements in sediments, seawater and marine organisms of Saronikos Gulf, Greece by NAA. The second part of this paper is a review of provenance studies based on minor and trace element research in ancient ceramics, obsidian, flint, limestone, marble and lead by Instrumental NAA, performed at the NCSR Demokritos.     

四川某金矿中非金属单矿物的元素分析及意义

利用中子活化分析法对四川某地区的非金属单矿物(热液脉矿物)的元素进行了测试,并利用元素地球化学研究方法对元素间的相关关系进行了分析。结果表明,在该地区可以利用元素间的伴生关系指导找矿。     

Analytical problems related to the preparation of samples used in studies on metallobiochemistry of heavy metals pollution using neutron activation analysis

Severe analytical problems are associated with the analysis of heavy metals at very low levels in biological samples. This impose a high degree of sophistication of the NAA involving treatment of the sample before irradiation such as chemical separations, physical treatments and biochemical fractionation, the experimental evaluation of interfering nuclear reaction as well as the development of post-irradiation radiochemical separation. This paper treats of the problem related to the NAA of trace elements in environmental biochemical toxicology focussing attention of the sources of the elements during the analysis. Typical results and short discussion for every step of the analysis are reported.