Determination of radiostrontium in soil samples using a crown ether

A simple and rapid method has been developed for the separation and determination of total radiostrontium in soil. The method consists of three basic steps: oxalate precipitation to remove bulk potassium, chromatographic separation of strontium from most inactive and radioactive interferences utilizing a crown ether (Sr. Spec, EIChroM Industries, Il. USA) and oxalate precipitation of strontium to evaluate the chemical yield. Radiostrontium is then determined by liquid scintillation counting of the dissolved precipitate. When 10 g samples of soil are used, the sensitivity of the method is about 10 Bq/kg. The chemical yield is about 80%. The separation and determination of radiostrontium can be carried out in about 8 hours.     

Anomalous grazing incidence small-angle x-ray scattering studies of platinum nanoparticles formed by cluster deposition

The size evolution of platinum nanoparticles formed on a SiO2/Si(111) substrate as a function of the level of surface coverage with deposited clusters has been investigated. The anisotropic shapes of sub-nanometer-size nanoparticles are changed to isotropic on the amorphous substrate as their sizes increased. Using anomalous grazing incidence small-angle x-ray scattering (AGISAXS), the scattering from nanoparticles on the surface of a substrate is well separated from that of surface roughness and fluorescence. We show that AGISAXS is a very effective method to subtract the background and can provide unbiased information about particle sizes of less than 1 nm.     

Electron diffraction studies of the molecular structures of iron(II) chloride and iron(II) bromide. Evidence on the structure of dimeric species Fe2Br4

An expression for the extreme values of mean-square amplitudes of vibrations in polyatomic molecules has been derived which permits estimation of the mean-square amplitude without solving the vibrational problem. This expression can be improved for the stretching and scissoring modes when the assignment of frequencies is known. In turn, the corresponding vibrational frequency may be estimated from the experimental value of the mean-square amplitude. The mean-square amplitudes of the butadiene-1,3 molecule are considered as an example.     

Thermal analysis and X-ray studies of chiral ferroelectric liquid crystalline materials and their binary mixtures

Summary Thermal properties of a homologous series of ferroelectric liquid crystals S-(-)-[4-(2-n-alkoxy-propionyloxy)]biphenyl-4'-[n-alkoxy-(3,5-dimethyl)]benzoate have been investigated by polarizing optical microscopy and differential scanning calorimetry. The mesophases were identified and confirmed by X-ray too. Three binary mixtures were prepared from the individual homologues. In one of the mixtures (Mix1), the ferroelectric SmC* phase has broadened and became enantiotropic. This mesophase remained monotropic in the other two mixtures (Mix2, Mix3). The chiral nematic N* phase did not appear in Mix1, but remained monotropic for the other two mixtures. Two molecular parameters, the layer spacing and the average intermolecular distance have been calculated from the X-ray results for the homologues and their mixtures. An intercalated tail-to-tail packing of molecules was found both in the single compounds and their mixtures resulting in the layer spacing about half of the molecular length of the single compounds.     

Improved sample preparation method for environmental plutonium analysis by ICP-SFMS and alpha-spectrometry

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.     

Line absorption of matrix elements as a background correction error in atomic absorption spectrometry

Accurate measurement of weak atomic absorption signals is only possible after exact background correction. If the accompanying elements in excess have their own resonance lines in the immediate vicinity of the resonance line of the element to be determined,and these fall within the spectral band transmitted by the monochromator, then the value the measured apparent background absorbance is higher than the true one. The error may usually be diminished by choosing an appropriate spectral bandwidth. Tables of such bandwidths for a large number of pairs of elements are given.     

Sr and stable strontium in bones of wild, herbivorous animals from Poland

Activity concentration of ⁹⁰ Sr and stable strontium concentration was analysed in 42 samples of animal (deer, roe-deer, elk and boar) bones, which mostly originated from north-eastern Poland. Strontium separation was performed by extraction chromatography. Determination of chemical yield was controlled by means of stable Sr determination using atomic spectrometry at the beginning and at the end of the separation procedure. Equilibrated ⁹⁰ Sr and ⁹⁰ Y activity was measured using a liquid scintillator spectrometer. Stable strontium range was from 55.4±1.7 ppm to 91.8±4.5 ppm, the mean was 71.84 ppm with a standard deviation (SD) of 9.31 ppm. The mean recovery of strontium was 26.7% with SD = 16.1%. The maximum activity of ⁹⁰ Sr, equal to 629±13 Bq/kg (ash) was found for a deer sample from Augustów Primeval Forest. In average, deer show the highest radiostrontium level, followed by roe-deer, elk and the lowest level were observed for boar. Differences between boar and deer or roe-deer are significant in terms of Kruskal-Wallis statistical test. Animal bones from north-eastern Poland showed about twice the mean concentration of ⁹⁰ Sr, compared to those of south-central Poland, but the difference was found not significant. Activities observed in roe-deer bones suggest the deposition of a concentration of 1.9 to 3.5 kBq/m² in the average of Chernobyl-origin ⁹⁰ Sr in 1986 in north-eastern Poland.     

Analysis of actinides in the primary coolant of a WWER-440 type reactor

A simple and effective method has been developed for the determination of the transuranium isotopes in primary coolant samples of WWER-440 type reactors. Membrane filters containing undissolved particles from about one liter coolant were destroyed by mineral acids, then americium-curium isotopes and neptunium-plutonium isotopes were coprecipitated sequentially with NdF₃ based on their different redox behavior. Alpha-spectra were determined by silicon semiconductor detectors connected to multichannel analyzers. Activity ratios measured in a reactor unit with a failed fuel element were compared with calculated values of the same type of reactor under similar conditions. Parameters of the defective fuel (burnup, original enrichment) could be estimated.