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Abstract  

Several bioanalytical techniques have been employed in conjunction with instrumental neutron activation analysis (INAA) to study metalloproteins and protein-bound trace elements in bovine kidneys. The accuracy of the INAA method developed has been evaluated by analyzing certified reference materials. Up to 29 elements can be reliably determined in biological tissue samples by INAA. Dialysis of the bovine kidney homogenate shows that more than 90% of Ca, Cd, Cu, Fe, Mg, Mn, Mo, Se, V and Zn, and about 20% of Br are bound to macromolecules, mainly proteins. A combination of gel filtration and ion exchange chromatography, chromatofocusing, electrofocusing, ammonium sulphate precipitation and INAA of the bovine kidney microsomecytosol subcellular fraction further indicates that much of the copper is associated with a single protein of an isoelectric point around 5 and a molecular weight of about 30 000 daltons. Some results on manganese proteins are also reported.

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Abstract  

An analytical procedure was developed to determine the concentration of some elements regarded as trace impurities in nuclear fuel using inductively coupled plasma mass spectrometry (ICPMS) associated to the matrix matching method. The assessment of this approach was carried out using a set of certified reference materials produced by the New Brunswick Laboratory (NBL). Eighteen out of the twenty-four elements in the reference materials could be easily determined. It was found that the mean values for reproducibility and accuracy were 5.0% and 15.0%. The remaining six elements provided mean values of 11.0% and 37.0%, respectively. They could not be adequately determined due to the effects of analyte signal suppression and spectral interference.

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Abstract  

A new method for the selective radiochemical separation of cadmium from other elements, present in biological materials, using amphoteric ion exchange resin Retardion 11A8 has been elaborated. Cadmium can be taken up by the resin either as anionic chloride complexes or cationic ammine complexes, depending on the composition of the eluent, exploiting both cation and anion exchange functions of the ion exchanger. The conditions in which Cd is quantitatively retained and eluted from Retardion 11A8 were established. The method of selective isolation of cadmium was further used for the determination of Cd in three biological certified reference materials by neutron activation analysis. Analytical results obtained with the use of the proposed separation procedure show good agreement with the certified values.

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Abstract  

A series of measurements were carried out to establish the reliability associated with isotope ratio (235/238) measurements on uranium samples using a quadrupole inductively coupled plasma mass spectrometer (ICPMS). Figures of merit related to the isotopic measurements were determined using non certified as well as certified materials provided by the New Brunswick Laboratory (NBL). The experimental results showed that repeatability is around 0.5% while reproducibility was calculated as 0.27%. Mass discrimination was determined as 0.03% per mass unit and the system linearity check over five orders of isotope ratios yielded a mass discrimination factor (K factor) of 1.0002±0.0081 (0.81%, 2s). The mean error of measurement obtained from six different certified reference materials was 0.77%.

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Abstract  

A new approach for the determination of elemental uranium in uranium bearing ore, using high resolution -ray spectrometry, was applied. Using a variant of the enrichment technique an agreement of better than 1% has been obtained between -ray measurement results and a certified value obtained by other analytical methods. For the calibration of the -ray spectrometer uranium reference samples have been used which are made available jointly in Europe and the USA as Certified Reference Materials for Gamma-Ray Spectrometry (EC NRM 171 and NBS SRM 969, respectively). The measured ore has been put in a special designed container which ensured in all directions seen from the radiation window an uniform degree of infinite thickness of about 95%. The results can be taken as an example for the applicability of -ray spectrometry when high accuracy is required and under conditions were homogeneously distributed elemental uranium is embedded in larger amount of matrix material.

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Abstract  

The determination of the hydrogen concentrations in coal and metal samples were investigated by using the PGAA system at the HANARO Research Reactor, KAERI. The calibration curve of the hydrogen concentration was obtained from a standard sample and the effects of the interference peaks near the gamma-energy region of hydrogen were investigated. The background in the hydrogen peak of a prompt gamma-ray spectrum was measured for the sample chamber and shielding materials of an atmospheric state. The combined uncertainties estimated for the analysis procedure were in the range of 4–5%. Two kinds of certified reference materials, NIST SRM 1632c (Coal), NIST SRM 173c (Titaniumbase Alloy) and NIST SRM 2453 (Titanium Alloy) were used to verify the accuracy and precision of the measurement. The relative error was in the range of 3–6% and the relative standard deviation were less than 4%.

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Abstract  

Recently developed radiochemical separation scheme for the simultaneous detemination of trace amounts of molybdenum and uranium in biological materials by NAA has been further refined and used for the detemination of these elements in several certified reference materials. The method assures very selective and quantitative separation of the indicator radionuclides:99Mo-99mTc and239Np from practically all accompanying activities followed by almost interference-free measurement by gamma ray spectrometry. The method can be applied to materials of both animal and plant origin and enables correcting the molybdenum results for uranium fission interference reaction thus assuring good accuracy for both elements down to ppb levels. The detection limits amount to 2.5 ppb (Mo) and 0.15 ppb (U) for ca. 200 mg samples.

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Abstract  

The application of differential scanning calorimetry (DSC) for purity determination is well documented in literature and is used amongst others in the analysis of pure organic crystalline compounds. The aim of this work is to examine whether the DSC method for purity determination consistently produces values for the purity of polycyclic aromatic hydrocarbons (PAHs) which are sufficiently accurate as required for the certification of reference materials. For this purpose, 34 different existing PAH certified reference materials were tested. The DSC results are shown to be consistent with the results obtained by other methods assessing the organic impurities content in PAHs, like gas chromatography (GC), high performance liquid chromatography (HPLC) and mass spectrometry. Significant differences between the measured values and the certified purity values were observed only in a limited number of cases.

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Abstract  

Instrumental neutron activation analysis (INAA), inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) were used for the determination of major and trace elements in sediment samples of the Bouregreg river (Morocco). The reliability of the results was checked, by using IAEA Soil-7 certified reference material. Results obtained by the three techniques were compared to control digestions efficiencies. A general good agreement was found between INAA and both ICP-MS and ICP-AES after alkaline fusion (ICPf). The ICP-MS technique used after acid attack (ICPa) was satisfactory for a few elements. A principal component analysis (PCA) has been used for analyzing the variability of concentrations, and defining the most influential sites with respect to the general variation trends. Three groups of elements could be distinguished. For these groups a normalization of concentrations to the central element concentration (that means Mn, Si or Al) is proposed.

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Abstract  

A rapid and simple sample preparation method for plutonium determination in environmental samples by inductively coupled plasma sector field mass spectrometry (ICP-SFMS) and alpha-spectrometry is described. The developed procedure involves a selective CaF2 co-precipitation for preconcentration followed by extraction chromatographic separation. The proposed method effectively eliminates the possible interferences in mass spectrometric analysis and also removes interfering radionuclides that may disturb alpha-spectrometric measurement. For 239Pu, 240Pu and 241Pu limits of detection of 9.0 fg·g−1 (0.021 mBq), 1.7 fg·g−1 (0.014 mBq) and 3.1 fg·g−1 (11.9 mBq) were achieved by ICP-SFMS, respectively, and 0.02 mBq by alpha-spectrometry. Results of certified reference materials agreed well with the recommended values.

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