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.
A new, very accurate (definitive) method for the determination of trace amounts of cobalt in biological materials has been devised. The method is based on combination of neutron irradiation with quantitative and selective post-irradiation separation of cobalt from all accompanying radionuclides followed by measurement by -ray spectrometry. Column chromatography in which owing to addition of Co carrier the course of separation can be followed visually is the key element of the separation scheme. Several criteria have been formulated which must be simultaneously fulfilled in order to acknowledge the result as obtained by a definitive method. The high accuracy of the method has been demonstrated by the analysis of several certified reference materials of widely different Co contents.
A new universal radiochemical separation scheme for selective and quantitative isolation of molybdenum and neptunium (formed from uranium), from neutron irradiated biological materials has been elaborated. The procedure is based on ion exchange and extraction chromatography with final fixation of molybdenum on a column with -benzoinoxime supported on Bio-Beads SM2 and neptunium on Dowex 1-X8 [No
]. The separated elements are quantified using gamma-spectrometric measurements. The new NAA method is able to overcome problems associated with high contents of phosphorous in some samples and assures detection limits better than 3 ppb for both elements. The validity of the proposed scheme has been demonstrated by the analysis of several CRM's.
Authors:B. Danko, H. Polkowska-Motrenko, and R. Dybczyński
The influence of irradiation conditions on the results of Co determination in plant samples by radiochemical neutron activation analysis (RNAA), after the conventional and microwave assisted wet digestion, has been investigated. Nine CRMs of botanical origin were examined. The study has demonstrated that the effectiveness of mineralization depended significantly on the kind of sample and the irradiation conditions. When analyzed CRMs were subjected to long-term irradiation in a high neutron flux, the mineralization using the microwave technique was necessary to obtain the correct results of Co determination in some of the plant samples. It has been proved that microwave digestion in a mixture of HNO3+H2O2+HF should be a standard method of wet ashing, independent on matrix and irradiation conditions.
Authors:R. Dybczyński, B. Danko, and H. Polkowska-Montrenko
Homogeneity of the existing (Virginia Tobacco Leaves CTA-VTL-2 (ICHTJ), Apatite Concentrate CTA-AC-1 (ICHTJ), Fine Fly Ash CTA-FFA-1 (ICHTJ) and candidate certified reference materials (CRMs) (IAEA-338 Lichen, IAEA-413 Algae, Spruce Shoots RMF II (Germany)) was studied by neutron activation analysis (NAA). Several samples of small mass (ca. 1 or 10 mg) taken from various containers were analyzed by instrumental NAA and the results for several elements were compared by Fisher's test and t-test with analogous series of results for samples taken from one container. In the second approach, sampling variance was estimated for some elements from overall variance and the components of analytical variance. The results were interpreted with the aid of Ingamells' sampling constant. Particle size distribution of the reference materials was also measured by several techniques. In addition quantitative determinations for some elements were performed and results compared with the certified values. The results of the present study were discussed with reference to suitability of CRMs to microanalytical techniques. It was pointed out that the term "microanalysis" itself is not always unequivocally understood and used.
A new method for the simultaneous determination of molybdenum and tungsten in biological materials by neutron activation analysis has been developed. It involves a single step radiochemical separation of both elements by extraction chromatography using -benzoinoxime supported on Bio-Beads SM 2. Good accuracy and precision of the method was demonstrated analyzing Bowen's Kale and IAEA's H-8 /Horse Kidney/ reference materials. The method was applied to check the reliability of the results obtained by one standard and one newly developed spectrophotometric methods for the molybdenum content in some plant materials.
Authors:B. Danko, R. Dybczyński, and Z. Samczyński
A new method has been developed aimed at determining traces of lanthanides in the materials of biological origin by NAA. The
chemical procedure that involves both, selective and quantitative pre-irradiation isolation of the elements of interest and
post-irradiation separation of lanthanides into two groups has been employed. The method is based on classical column ion-exchange
and extraction chromatography. In the pre-irradiation step all the accompanying elements are eliminated and the quantitatively
isolated lanthanides fraction is free from highly activating macro components, as well as from other trace elements, including
uranium, which is the source of spectral and nuclear interferences. After neutron irradiation, the lanthanide fraction is
divided into two sub-fractions, taking advantage of the different anion-exchange affinities of individual lanthanide complexes
with EDTA towards strongly basic anion-exchanger. This provides the favorable gamma-ray spectrometric measurement conditions
enabling reliable determination of 13 elements.
Authors:H. Polkowska-Motrenko, R. Dybczyński, B. Danko, and D. Becker
A very accurate and sensitive method for the simultaneous determination of trace amounts of Co and Ni in biological materials has been elaborated. The method is based on radiochemical neutron activation. Irradiation of samples in Cd-shielded channel of a nuclear reactor assures balanced activity ratio of58Co and60Co isotopes and favourable detection limits for both nickel and cobalt. Column chromatography (ion exchange and extraction) has been used for the quantitative and selective isolation of the determined radionuclides. High accuracy of the method has been demonstrated by the analysis of several certified reference materials.