Precocentration method using an activatable yield tracer for neutron activation analysis

Previously, the use of an enriched stable isotope as an activatable yield tracer in preconcentration steps has been tested by use of commercially available enriched¹¹⁶Cd and¹⁵⁶Dy for biological standard reference materials.^1,2 In the present work, this method has been further applied to the determination of lanthanoid contents in various kinds of samples: one coal fly-ash, three Japanese standard rocks, and eight standard soils. Samples were decomposed by alkali fusion in the preconcentration step. Thirteen elements were determined for coal fly-ash and soil samples, and 14 elements for rocks. The data obtained for coal fly-ash and standard rocks are compared with the data reported in literature. The data for soil samples have been newly determined in the present work. The ordinary instrumental neutron activation analysis and radiochemical neutron activation analysis were also performed to confirm the accuracy and usefulness of the present method.     

Thermal and epithermal neutron activation analysis using the monostandard method

A new approach is presented for neutron activation analysis using the monostandard (single comparator) method. Elements to be determined are classified into two groups; those with σ_o>I_o are activated with whole neutron spectrum (without Cd-cover), using a standard of the same group (e.g. Sc), while elements with I_o>σ_o are activated with epithermal neutrons (under Cd-cover) using a standard of the same group (e.g. Au or Co). Epithermal activation increases the number of determinable elements and its coupling with the monostandard method has the advantage of using a small Cd-cover. The σ_o and I₀ values of some elements were determined to test this approach.     

Determination of trace elements in water by non-destructive neutron activation

A systematic study was undertaken in order to find out which of the most relevant elements can be determined in water under normal conditions by non-destructive neutron activation simultaneously using a suitable monostandard method. Standardized water samples as well as natural water of different kind were used, brought to dryness by freeze-drying and irradiated in quartz at a neutron flux of 10¹⁴ cm⁻² s⁻¹ for 1 day. The trace element content in quartz ampoules of different origin was determined separately. The following elements are discussed in detail including possible interferences: As, Au, Br, Ca, Cd, Co, Cr, Cu, Eu, Fe, Hg, K, La, Mo, Na, Ni, Sb, Sc, Se, U, Zn. Presented at the Euroanalysis II Conference, Budapest, 25–30. Aug. 1975.     

Ergebnisse der Untersuchung Geologischer Standards

Using instrumental neutron activation analysis 18 elements are determined in 9 standard rocks of the central geological institut of the GDR. The results are compared with certified values.      

Application of k 0-based internal mono-standard PGNAA for compositional characterization of cement samples

The k ₀-based internal mono-standard prompt gamma-ray neutron activation analysis (IM-PGNAA) method was used for compositional analysis of a cement standard provided by the International Atomic Energy Agency as a part of inter-laboratory comparison exercise. The PGNAA was also applied to a local cement sample for comparison purpose. The concentration ratios of elements with respect Ca were determined using the internal mono-standard method. The concentration ratios were then converted to the absolute concentrations by determining concentration of Ca in the cement using relative method. Concentrations of 11 elements were determined in both sample and standard of cement. The results of cement standard are found to be in good agreement with the certified values. The uncertainties on the elemental concentrations were in the range of 5–10 %.     

Multi-element determination in sandstone rock by instrumental neutron activation analysis

Summary Instrumental neutron activation analysis (INAA) was used for the qualitative and quantitative analysis of sandstone samples of Aswan area, in South Egypt. The samples were properly prepared together with standards and simultaneously irradiated by a neutron flux of 7 ^. 10¹¹ n ^. cm^-2.s^-1. in the TRIGA research reactor facilities in Mainz. The gamma-spectra from a hyperpure germanium HPGe detector were analyzed. The present study provides the basic data of elemental concentrations of a sandstone rock. The following elements have been determined: Na, K, Fe, Sc, Cr, Co, Zr, Ce, La, Nd, Sm, Eu, Yb, Lu, Hf, Ta, Th and U. Energy dispersive X-ray fluorescence (EDXRF) was used for comparison and to detect elements which can be detected only by this method.     

Heavy Metal Ions Determination in the Arctic Soils

ABSTRACT

Soil samples collected in the following areas: Greenland, Svalbard and North Siberia have been analyzed. Seventeen micro and trace elements were determined by ICP-AES.     

Application of the k0 standardization method in reactor nuetron activation analysis of standard steels and fly ash

The method of k₀ standardization is suitable for routine multi-element determinations by reactor neutron activation. Investigation of NBS steel standards showed the systematic error of the method to be less than 3%. Numerical evaluation of the spectra was found to be fast and convenient. Fourteen elements in the steel samples were determined; for nine, the standard deviation was less than 4%. Thirty seven elements were determined in NBS SRM-1663a Coal Fly Ash; agreement with certified values was again very good.     

Dry-Ashing Preconcentration for Micro-Reactor-Based Neutron Activation Analysis of Food and Plant Samples

The application of preconcentration by dry-ashing to the neutron activation analysis of biological samples using a SLOWPOKE-2 low-power reactor is reported. Samples of selected food crops (banana, callaloo, carrot, mango, and yam) and bioindicator plants (lichen, moss, Tillandsia sp., and tree bark) were analysed both as plant tissue, and as ashed sample. The results are presented for 21 elements. Good agreement between both procedures (<10% relative standard error) was obtained for 13 elements: Al, Ca, Cd, Cr, Fe, K, La, Mg, Mn, Na, Sm, Ti, and V. For Dy, Rb, and Zn the agreement was 10-15%. Relatively poorer agreement (>15-30%) was obtained for As, Br, Cl, and Sb. Dry ashing produced improved analytical results for those samples that were of low ash content. However, the increased background counts observed in ashed samples can sometimes negate the concentration gain, particularly in plants with high ash contents but low levels of certain elements.     

A neutron activation analysis procedure for the determination of uranium,thorium and potassium in geologic samples

A neutron activation analysis procedure was developed for the determination of uranium, thorium and potassium in basic and ultrabasic rocks. The three elements are determined in the same 0.5-g sample following a 30-min irradiation in a thermal neutron flux of 2·10¹² n·cm^?2·sec^?1. Following radiochemical separation, the nuclides²³⁹U (T=23.5 m),²³³Th (T=22.2 m) and⁴²K (T=12.36 h) are measured by β-counting. A computer program is used to resolve the decay curves which are complex owing to contamination and the growth of daughter activities. The method was used to determine uranium, throium and potassium in the U. S. Geological Survey standard rocks DTS-1, PCC-1 and BCR-1. For 0.5-g samples the limits of detection for uranium, throium and potassium are 0.7, 1.0 and 10 ppb, respectively.     

Preconcentration of trace elements for neutron activation analysis using activable tracers

Use of an enriched isotope as an activable tracer is proposed for the preconcentration of trace elements in neutron activation analysis. As a test of this method, contents of cadmium in various biological standard samples were determined by addition of an enriched¹¹⁶Cd tracer in the preconcentration step followed by neutron irradiation and -ray spectrometry. The principle, advantage, and limitations of the method are also discussed.     

Determination of trace elements in human gallstone and bile by k0-INAA

Summary The trace elements composition of gallbladder stones samples of the types cholesterol, pigment and mixed stones in addition to bile have been investigated by k₀-instrumental neutron activation analysis (k₀-INAA). The samples were obtained from several individuals of adult subjects of the Libyan population who undergone open surgery of gallbladder (cholecystectomy) at Al-khadra University Hospital in Tripoli. The samples were lyophilized, irradiated together with Au wire and Zr foil, which serve as flux ratio monitor and a parameter at TNRC. Concentrations of 24 elements in gallstone and 23 elements in bile were determined. The levels of the trace elements in the various samples investigated are measured and discussed. The reliability of the analysis was checked with several biological standard reference materials.     

Multi-element determination in silicate rocks by instrumental neutron activation analysis

Instrumental neutron activation analysis technique was applied for the determination of 20 elements in 54 silicate rock samples which belong to three sedimentary geological formations located in the western desert of Iraq. The samples along with USGS standards were irradiated in an IRT-5000 reactor at a neutron flux of 3.7·10¹³ n·cm^–2·s^–1 The following minor and trace element constituents have been determined: Na, K, Ca, Fe, Sc, Cr, Co, Zr, Ce, La, Nd, Sm, Eu, Tb, Yb, Lu, Hf, Ta, Th and U.     

Determination of Trace Elements in Aerosol Samples Collected on Polycarbonate Filters by Atomic Absorption Spectrometry

Abstract

The multi-element analysis of aerosol samples collected on polycarbonate filters and the wet digestion procedure in open vessel were investigated. The concentrations of Na, K, Ca, Mg and Zn were determined by flame atomic absorption spectrometry with a micro injection system while Cd, Pb, Cu, Ni and V were determined by graphite furnace atomic absorption spectrometry (AAS).

NIES N[ddot] 8 “Vehicle Exhaust Particulate” Certified Reference Material from the Japan Environment Agency was used to study the decomposition of the samples. Different treatments were applied in order to completely dissolve the aerosol samples. It was found that, from all the methods tested, attack with micro-quantities of HNO₃ and HCIO₄ in an air pressure digestion system was the best procedure for the determination of the elements by AAS.

The recommended method was appropriate for all elements and it was applied to real samples. Two nondestructive analytical techniques for the determination of Na, K, Ca, Mg, Zn and Pb have been compared with the proposed method: proton induced X-ray emission (PIXE) and neutron activation analysis (NAA). Results obtained by the application of these three techniques were similar.     

Prompt gamma-ray analysis (PGA) of meteorite samples, with emphasis on the determination of Si

Neutron-induced prompt gamma-ray analysis (PGA) was applied to seven meteorite samples (Allende, Zagami, Acfer 209, ALH77005, ALH84001, EET79001 and Neagari). Samples were irradiated in both the thermal neutron and the cold neutron guided beams of JRR-3M at JAERI. Multiple samples of an Allende standard powder were analyzed for Si using two different methods: (1) the comparison method, using a Si standard, and (2) the mono-standard method, using Fe as an internal reference element. The Si concentrations determined by these two methods are in good agreement with literature values. The analytical sensitivity for Si using the cold neutron guided beam is∼14.3× higher than that for the thermal neutron guided beam. Other elements determined (B, Ca, Ti and S) also showed higher sensitivities using the cold neutron beam. The other meteorites studied showed some anomalous B and S values likely due to the effects of terrestrial weathering/contamination.     

INAA of trace impurities in aluminium clads

As a contribution to nondestructive neutron assay of reactor grade aluminium, a number of elements have been investigated qualitatively and quantiatively using a vertical channel in the IRT-5000 reactor with a thermal neutron flux of 7.6·10¹²n·cm^–2·s^–1. The -ray spectra of irradiated samples were analysed with a 30 cm³ Ge(Li) detector connected to an HP-computer and a 4096 channel analyser. The following impurities have been determined: Sc, Ca, Cr, Fe, Ni, Co, Zn, As, Sb, W, Au, Th and U, while Lu and Hf have been determined qualitatively only.     

Activation Constants for Slowpoke and MNS Reactors Calculated from the Neutron Spectrum and k0 and Q0 Values

The relative thermal, epithermal and fast neutron fluxes were measured in the inner and outer irradiation sites of three Slowpoke reactors and one Miniature Neutron Source (MNS) reactor by the bare triple monitor method. Using the measured neutron spectrum parameters and a compilation of published k ₀ and Q ₀ values, activation constants were calculated for the most intense gamma-rays of all nuclides commonly used in NAA. The resulting table of constants can be used to standardize NAA measurements for all elements when combined with relative efficiency measurements and the measurement of the thermal neutron flux with one standard. The observed constancy of the neutron spectra suggests that these activation constants are valid for all 14 Slowpoke and MNS reactors.     

Determination of Gold and Palladium in Manganese and Nickel Compounds by Atomic Absorption Spectrometry After Separation by Use of Amberlite XAD-7 Resin

Abstract

A method for preconcentration and determination of traces of Au and Pd from manganese, nickel and their compounds is described. The trace elements are preconcentrated at a small column filled with Amberlite XAD-7 resin. After their eluation the elements are determined by flame AAS. The relative standard deviations (N=10) were found to be lower than 5%; the detection limit (3s, N=20) for Au and Pd in metal samples is 0.07 μg/g.     

The Determination of Arsenic in Soil and Sediment Digests by Graphite Furnace Atomic Absorption Spectrometry

Abstract

A method for the determination of As in siliceous materials from a fluoboric acid matrix by GFAAS is described. The basic analytical procedure also permits the measurement of major, minor and other trace elements by flame or graphite furnace AAS as appropriate. For As analysis, the incorporation of matrix modification with Ni and of corrective measures to overcome interference by Al, Na and Si are discussed. The validity of the method is demonstrated by the accurate analysis of four international standard reference materials and agreement with instrumental neutron activation analysis results for As in environmental samples. One application to the study of As geochemistry in lacustrine sediments is presented.     

Investigations on the preparation and application of some inorganic separators for the removal of the matrix activity in neutron-activated biological samples

For the selective removal of the matrix activity (²⁴Na,³²P and⁴²K) in the neutron activation analysis of biomedical samples the inorganic separators “hydrated antimony pentoxide”, zirconium phosphate, and titanium phosphate were prepared. The sorption parameters of the samples were determined via elution chromatography techniques, with appropriate tracers. The basic principles of the sorption processes were investigated, and the experimental conditions were optimized. These inorganic separators were then applied, combined with a distillation procedure and an ion-exchange separation, for the determination of the following trace elements in animal blood samples: Mn, Co, Cu, Fe and Zn.