Determination of uranium in thorium matrixes by epithermal neutron activation analysis

Uranium in thorium matrixes or in minerals and ores containing thorium is determined by epithermal neutron activation analysis (ENAA). In some minerals and ores, such as monazite sands, the analysis can be carried out by purely instrumental means with no chemical separation of uranium or thorium from the irradiated matrix. For thorium compound matrixes with very low uranium contents, a rapid radiochemical separation method, based on the retention of uranyl ion on anion-exchange resins, is first carried out, before counting the gamma-ray peaks for²³⁹U in multichannel analysers coupled to NaI(Tl) scintillators or to Ge(Li) detectors.     

Determination of silver using cyclic epithermal neutron activation analysis

A fast pneumatic transfer facility was installed in Nuclear Engineering Teaching Laboratory (NETL) of the University of Texas at Austin for the purpose of cyclic thermal and epithermal neutron activation analysis. In this study efforts were focused on the evaluation of cyclic epithermal neutron activation analysis (CENAA). Various NIST and CANMET certified materials were analyzed by the system. Experiment results showed ¹¹⁰Ag with its 25 s half-life as one of the isotopes favored by the system. Thus, the system was put into practical application in identifying silver in metallic ores. Comparison of sliver concentrations as determined by CENAA in CANMET certified reference materials gave very good results.     

Determination of fluorine in coral skeletons by instrumental neutron activation analysis

Summary A systematic and non-destructive technique is proposed for the determination of fluorine in coral samples by instrumental neutron activation analysis using the ¹⁹F(n,γ)²⁰F reaction. About 50 to 80-mg samples in polypropylene capsules were irradiated for 15 seconds in the pneumatic transfer tube system (PN-3) of JRR-3M reactor. After the irradiation at a thermal neutron flux of 1.5 ^. 10¹³ n ^. cm^{-2 .} s^-1, the coral samples and standards were cooled for 6 seconds and the g-rays emitted were measured for 15 seconds with a Ge detector. The sequence from sample irradiation to g-ray counting was performed under a computer-control mode. The analytical precision was ~5% for the JCp-1 coral standard. The present method was applied to the determination of fluorine in corals from Thailand, Okinawa and the Philippines. The advantage of one method over destructive techniques is discussed by comparing the analytical results obtained for the JCp-1 coral standard using INAA, ion chromatography and spectrophotometry. Factors that may control the levels of fluorine in corals are also discussed.     

Determination of iodine in human brain by epithermal and radiochemical neutron activation analysis

Despite the role of iodine for proper development of the brain and the functions of the element, the accurate data on its concentration in brain tissue are largely lacking, the main reason being analytical difficulties associated with determination of the element especially at low levels. In this work, samples from human brain regions from Hungarian patients were analyzed using epithermal and radiochemical neutron activation analysis (ENAA and RNAA, respectively). The RNAA procedure is based on alkaline-oxidative fusion followed by extraction of elemental iodine in chloroform. The results were checked by the analysis of biological standard reference materials, namely bovine liver, bone meal and diet, and by comparison with previous results obtained by a different RNAA procedure.     

Determination of iodine in Asian diets by epithermal and radiochemical neutron activation analysis

Samples of diets from China, Japan, Korea, India, Pakistan and Philippines were analyzed using epithermal and radiochemical neutron activation analysis (ENAA and RNAA, respectively) within the framework of the IAEA project “Reference Asian Man”. The RNAA procedure was based on alkaline-oxidative fusion followed by extraction of elemental iodine in chloroform. The analytical methods employed are discussed in terms of detection limits and uncertainties of the results obtained. For quality control purposes a number of NIST biological reference materials, namely diets and foods were analyzed. Results for the diet samples indicate that achieving the WHO recommended daily allowance for iodine may be a problem in most of the above given countries. This revised version was published online in August 2006 with corrections to the Cover Date.     

Determination of trace elements in biological materials by instrumental epithermal neutron activation analysis

The use of reactor epithermal neutrons in instrumental activation analysis is described for the determination of trace elements via long-lived isotopes. A boron carbide filter is used. Results of analyses of human erythrocytes, plasma, urine and some biological reference materials are given to demonstrate the applicability of the method to biological samples. Bromine, iron, cesium, rubidium, selenium and zinc and cobalt are determined. The method provides accuracy and reliability similar to conventional thermal neutron activation but is faster. Limits of detection attainable with the two techniques are compared.     

Determination of iodine in human nails via epithermal neutron activation analysis

An epithermal instrumental neutron activation analysis (EINAA) method, using a boron nitride irradiation capsule compatible with use in the University of Missouri Research Reactor pneumatic-tube irradiation facility, has been developed for the analysis of iodine in human nails. The principal objective was to determine if the nail could be used as a means of monitoring dietary intake of iodine. The EINAA method was used to analyze nails from subjects having iodine intakes that could be qualitatively differentiated. Iodine concentrations in nails from these subjects were positively correlated with apparent iodine intake.     

Determination of some elements by epithermal neutron activation analysis for the Arctic aerosol

Summary We have determined nineteen trace elements in 685 aerosol filter samples collected during 1964-1978 in northern Finland by the Finnish Meteorological Institute. In this paper we present some procedures and results for very short (~25 s), short (~3-54 min), and medium (12-35 h) lived isotopes as determined by epithermal NAA in conjunction with and without Compton suppression. Elements with a I_γ/σthratio are favorable to be determined by epithermal NAA. Silver was determined by a one minute epithermal irradiation because of a very short ¹¹⁰Ag half-life. Antimony, arsenic, cobalt, bromine, indium, iodine, potassium, silicon, tin, tungsten, and zinc were determined by a ten minute epithermal irradiation. For silver determination, samples were counted without transferring the filter from the irradiated vial, however, for ten minute irradiation all samples were transferred to a non-irradiated vial and counted both in the normal and Compton mode by the HPGe gamma-spectrometry system with a decay time of about 10 minutes and counting time of 15 minutes. Each day a maximum of 16 samples were irradiated and immediately following the short counting, these samples were loaded into an automatic sample changer in sequence of irradiation and counted for an hour in both normal and Compton modes. This has proven to be an extremely cost effective measure thus reducing the need to employ long-lived NAA to analyze other elements such as Ag, Co, Sn and Zn and Ag for air pollution source receptor modeling.     

Determination of arsenic and gallium in standard materials by instrumental epithermal neutron activation analysis

Epithennal neutron activation analysis has been applied to the determination of arsenic and gallium in standard materials at trace concentrations. The reduction of ²⁴Na activity compared to thermal neutron activation is advantageous. Arsenic detection limits (1σ) are 0.04 and 0.015 μg for inorganic and organic materials, respectively. The corresponding gallium detection limits, for the best cases, are 0.13 and 0.29 μg. Gallium determinations with the 834-keV photopeak of ⁷²Ga suffered interferences attributed to the threshold reaction ⁵⁴Fe(n,p) ⁵⁴Mn; the less intense ⁷²Ga peaks at 629 and 2200 keV provided quantitative results for all samples tested. Gallium detection limits with the less intense, but more reliable 629-keV peak were 0.9 and 0.1 μg for inorganic and organic materials, respectively. Arsenic determinations are best performed with the more intense ⁷⁶As 559-keV line, as the 657-keV line has an unknown interference.     

Determination of trace cadmium and other elements in bone by epithermal neutron activation analysis

Epithermal neutron activation analysis (ENAA) was applied to measure quantitatively Cd and other elements in bone samples from control and Cd-fed rats. This method was found to be non-destructive to the bone samples, with no sign of radiolytic charring and was sensitive enough to detect and quantify Cd in bone samples at normal levels for mammals (viz. 0.5–1.0 g/g) and higher. Two different thermal neutron shield materials were utilized, namely cadmium and boron. The boron shield resulted in a 27% improvement in the detection limit of Cd in bone. The accuracy of ENAA for Cd was assessed by intercomparison with electrothermal atomic absorption spectrophotometry (ETAAS), and the results were in fair agreement (±23%) with those from ENAA.     

Trace multielement analysis in boron materials by epithermal neutron activation analysis

A method, based on epithermal neutron activation analysis using a boron filter is described for the determination of ～60 trace elements in boron and its compounds. The method has an accuracy of ～20%, a precision of ～15% RSD and limits of detection for most elements are either at the sub-ppm or low ppm levels. The method requires no sample preparation and is economical in effort.     

Uranium in coral skeletons determined by epithermal neutron activation analysis

A simple and non-destructive method has been proposed for the routine determination of uranium by epithermal neutron activation analysis in coral skeletons. Using a cadmium capsule, about 0.1-0.2 g samples were irradiated for 6 hours in the Triga Mark II Reactor. Measurements of -ray (²³⁹Np via ²³⁹U) were performed with each sample and standard after cooling for about three days. Compared with a non-destructive thermal NAA, the present method was found to improve the sensitivity because it reduced the intense Compton background induced by ²⁴Na. We determined uranium in coral standards within 2% of analytical precision. The data obtained for the carbonate standards are mostly consistent with reported values. The present method could be usefully applied to determine uranium contents in fossil corals from the Funafuti Atoll in the Pacific. The distribution of uranium between seawater and coral skeletons is also discussed in order to understand the environmental media in which the coral grew.     

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.     

Analysis of foods for iodine by epithermal neutron activation analysis

Epithermal-neutron activation analysis (ENAA) was applied to the analysis of foods for iodine. The procedure involves irradiation of wet foods in a boron nitride, vessel, followed by direct counting of the 442.9 keV gamma ray of¹²⁸I without any processing of the sample. Three research reactors were evaluated for use in determining iodine by ENAA. The University of Virginia reactor at Charlottesville was chosen for this study because the reactor facilities minimized thermal heating of the boron nitride vessel, enabling irradiation of larger, more representative analytical portions. Iodine concentrations ranging from <0.003 to 0.74 g/g are reported for 17 different food matrices.     

Estimates of iodine in biological materials by epithermal neutron activation analysis

Iodine abundances in NBS biological SRMs and various organs of rats were evaluated by epithermal neutron activation analysis with a boron carbide filter. Detectability of iodine in different biological materials by this method is discussed.

     

Determination of selenium in nickel and cobalt concentrates applying epithermal neutron activation analysis

The physicochemical association of plutonium in soil near the Subsurface Disposal Area (SDA) at the Idaho National Engineering and Environmental Laboratory (INEEL) has been determined using selective sequential extraction techniques. Our results suggest that plutonium in surface soils is associated primarily with the hydrous oxide coatings of the soil (37±5.3%). Appreciable amounts of plutonium were also removed with the organic matter (22±2.8%) and carbonates (13±3.1%). On the other hand it appears that plutonium association with the soluble and exchangeable components of the soil is relatively small (>4.0%). The remainder of plutonium (21±4.7%) is tightly bound to the refractory silicate residue of the soil. Relatively little plutonium is available for physicochemical mobilization from the soil under the present prevailing conditions of the INEEL site.     

Determination of trace concentrations of thorium in uranium oxide matrix by epithermal instrumental neutron activation analysis

An epithermal instrumental neutron activation analysis (EINAA) method using cadmium filter was standardized to determine trace concentrations of thorium in four samples of uranium oxide (U₃O₈) samples. Samples and thorium standards, wrapped with cadmium foil, were irradiated at a reactor neutron flux of about 10¹² cm^?2 s^?1. Radioactive assay was carried out using a Compton suppressed anticoincidence gamma ray spectrometer consisting of HPGe-BGO detectors coupled to MCA. Concentrations of thorium in these samples were found to be in the range of 15–72 mg kg^?1. EINAA results were validated by determining thorium concentrations in uranium matrix by standard addition method. EINAA results were compared with those obtained by two wet chemical methods namely ion chromatography (IC) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The results obtained by the three methods were found to be in good agreement, indicating further validity of the proposed EINAA method.     

Silicon determination in plant materials by instrumental epithermal neutron activation analysis

The Si determination with epithermal neutrons using the reaction²⁸Si (n,p)²⁸Al is described. Thermal neutrons are eliminated from the irradiation position with a BN-shield. Two first order interfering reactions with P and with Al necessitate appropriate corrections. The interfering reaction on Al is shown to depend heavily on the hydrogen (H) content of the sample, which therefore must be taken into account. The lower application range in plant samles is estimated to be 500 g g^–1. Reproducibility is <5% in suitable cases, but not as good if the necessary corrections are large. The capacity is 25 samples per 8 h. The method is applied to 3 plant standards (rice, hay and pine needles) and to 47 samples of spruce needles. The applicability to different plant materials is mainly limited by their relative Al, P and Si concentrations. Literature values are use to find plant categories in which Si can be reasonably determined by instrumental epithermal neutron activation analysis (IENA).     

Determination of iodine in milk products and biological standard reference materials by epithermal neutron activation analysis

The biologically essential trace element, iodine, has been determined in various milk products by epithermal neutron activation analysis /ENAA/ after sealing in quartz and irradiating under cadmium cover. The method was extended to several IAEA and NBS biological reference materials.