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Summary  

A simple sample decomposition and laser fluorimetric determination of uranium at trace level is reported in certain refractory minerals, like ilmenite, rutile, zircon and monazite; environmental samples viz. soil and sediments; industrial waste materials, such as, coal fly ash and red mud. Ilmenite sample is decomposed by heating with ammonium fluoride. Rutile, zircon and monazite minerals are decomposed by fusion using a mixture of potassium bifluoride and sodium fluoride. Environmental and industrial waste materials are brought into solution by treating with a mixture of hydrofluoric and nitric acids. The laser induced fluorimetric determination of uranium is carried out directly in rutile, zircon and in monazite minerals and after separation in other samples. The determination limit was 1 μg . g-1 for ilmenite, soil, sediment, coal fly ash and red mud samples, and it is 5 μg . g-1 for rutile, zircon and monazite. The method is also developed for the optical fluorimetric determination of uranium (determination limit 10 μg . g-1) in ilmenite, rutile, zircon and monazite minerals. The methods are simple, accurate, and precise and they require small quantity of sample and can be applied for the routine analysis.

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Abstract  

Instrumental neutron activation analysis (INAA) together with scanning electron microscopy (SEM) have been used in the study of fly ash from large electric power and heating plants. Two basic kinds of fly ash originating either from brown coal or heavy-oil combustion can be characterized both by morphology and trace element composition. INAA technique used consisted of both short (1 min) and long (2 h) activations to ensure the determination of 30–40 elements in each fly ash sample. The average composition and determination limits obtained by INAA for coal fly ash produced in several electric power plants burning two kinds of brown coal have been compared with those obtained for fly ash originating from heating plants burning heavy-oil. Coal fly ash showed much higher concentrations of many elements especially of Sc. La, Th, Cs, Ce, Sm, Rb and Al in comparison with oil fly ash. On the other hand, the latter contained relatively high concentrations of V and Ni. The results of INAA of fly ash samples can be used for the projection of efficient separating devices and for the evaluation and prediction of contamination levels in the vicinity of large emission sources.

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Abstract  

Landfills and waste disposal sites are now routinely used for disposal of solid wastes and their incinerator ashes. Trace elements from these ashes are leached by rain and acid rain into nearby waterways providing a pathway for toxic elements to re-enter the food chain and the human life cycle. This paper examines the mechanism and the extent of leaching of 20 elements viz. Ag, Al, As, Ba, Br, Ca, Cd, Co, Cr, Fe, Hg, La, Sb, Sc, Ce, Sm, Ta, V, W and Zn. Instrumental neutron activation analysis (INAA) was used for the assay. The solid wastes studied are municipal refuse incinerator ash, coal fly ash, hospital incinerator ash, raw sewage sludge and its incinerator ash.

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Abstract  

The k 0-IAEA program developed for implementation of the single comparator instrumental neutron activation analysis method (k 0-INAA) has been used for elemental analysis with NIRR-1 irradiation and counting facilities. The existing experimental protocols for routine analysis based on the relative method were used to test the capability and reliability of the program for the analyses of geological and biological samples. The Synthetic Multi-element Standards (SMELS) types I, II and III recommended by the international k 0 user community for the validation of k 0-NAA method in NAA laboratories, furthermore, the following standard reference materials: NIST-1633b (Coal Fly Ash) and IAEA-336 (Lichen) were analyzed. Results obtained with the version 3.12 of the k 0-IAEA program were found to be in good agreement with the data obtained with the established relative method using WINSPAN-2004 software. Detection limits for elemental analysis of geological and biological samples with NIRR-1 facilities are provided.

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Abstract  

To order to examine experimentally the modified monostandard method implemented in the program MULTINAA, the FRM reactor in Garching (Germany) was calibrated and an INAA of a standard reference material NIST/SRMI1633b Coal Fly Ash was performed. The relative, thek 0-and the modified monostandard standardizations are applied. This work shows that for all of the examined 1/-nuclides the modified monostandard method provides identical analytical results to those determined by thek 0-method. For the non-1/ nuclides177Lu and152Eu the monostandard results are correct. Compared with the certified values of the analysed SRM1633b sample and also with the results of the relative method, it can be concluded that the modified monostandard method performed at our experimental conditions gives analytical results with accuracy better than 5%.

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Abstract  

A permanent and stand-alone neutron-induced prompt -ray analysis (PGA) system, usable at both cold and thermal neutron beam guides of JRR-3M has been constructed. The characteristics of the system, including neutron beam and -ray spectrometer were measured. Owing to the absence of fast neutrons and the low -ray background, analytical sensitivities and detection limits better than those in other PGA systems have been achieved. Analytical results of ten elements in Standard Reference Material of Coal Fly Ash agreed well with those obtained by other methods. Isotopic analysis of Ni and its application to accurate and precise determination of Ni by stable isotope dilution method were performed.

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Abstract  

A new Compton suppression system (CSS) for the gamma-ray spectrometer portion of the neutron activation analysis (NAA) was set up at the RPI/ITN. The pneumatic transfer system, SIPRA, for short-lived nuclides and cyclic irradiations was improved. A full calibration procedure of the CSS and SIPRA systems was performed. Two certified reference materials, NIST-SRM-1572 (Citrus Leaves) and NIST-SRM-1633a (Coal Fly Ash) were analyzed using the calibration factors. The CSS was instrumental in lowering the detection limits of Cr, Fe, Hg, Rb, Sr, Th and Zn by reducing background and/or spectral interference considerably. The analytical results were evaluated by comparison to the NIST certified values with deviations ranging from 2% to 8% for the above mentioned elements, except Zn ranging from 10% to 15% for biological and environmental samples, respectively.

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Abstract  

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.

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Abstract  

Different reference materials of environmental and geological origin, such as NBS 1633a (Coal Fly Ash, CFA), NBS 1645 (River Sediment, RS), GXR-2, and IAEA Soil-5, were investigated by short time activation analysis. The samples were analyzed in 5 replicates each between 100 to 150 mg, at neutron flux of 1.3 E 12 cm–2 s–1, using a high rate — high resolution gamma spectroscopy with a Loss Free Counting (LFC) System to correct the dead time and pile up to 500,000 cps. The results of the measurements indicate that the precision in determination of28Al,46mSc, and52V is between 1 to 6%. Different evaluation programs (i.e. ALCHEM, AKTAN, and ND-PEAK) were used to calculate the peak areas. The results indicate that, at lower counts, the statistical error of peak area calculation becomes more significant. Finally, Mössbauer spectroscopy was used to investigate the main Fe compounds present in some reference materials.

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Abstract  

Concentrations of 35 elements in Chinese Standard Rocks (GSR-1 to GSR-3) and Soils (GSS-1 to GSS-8) have been measured with INAA using the SLOWPOKE reactor. At the same time, the U. S. NBS reference standards: SRM-1632a (Bituminous Coal), SRM-1633a (Coal Fly Ash) and SRM-1646 (Estuarine Sediment) were also analyzed in order to cross-check the accuracy of this method. The results obtained indicate that the reproducibility of the method is satisfactory for most of the elements, namely the precision in general, is better than ±10%. Comparison of our values for NBS SRM-1632a, 1633a and 1646 with the certified values of NBS or with values cited in the literature indicates good agreement. The results were found to be accurate within ±10% error of the established results.

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