Browsing by Author "Pougnet, M A Bruno"

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    Direct determination of cadmium and beryllium in coal and fly ash slurries using graphite furnace atomic absorption spectrometry
    (1990) Haraldsen, Lana Celeste; Pougnet, M A Bruno
    Graphite Furnace Atomic Absorption Spectrometry (GFAAS) was used for the determination of cadmium and beryllium in coal and fly ash slurries. Sample preparation involved grinding the sample to a fine powder and slurrying it in a suitable solvent. Stable slurries were maintained by magnetic stirring during sampling. Pyrolytically coated graphite tubes were used for cadmium determinations, while beryllium was determined with platform atomisation. Ammonium dihydrogen orthophosphate and magnesium nitrate matrix modifiers were used for cadmium and beryllium determinations respectively. Calibration graphs constructed with aqueous standards containing the appropriate matrix modifier were rectilinear to at least 100 pg cadmium and 45 pg beryllium. Results were calculated with integrated peak area measurements. The detection limits were 2.9 pg for cadmium and 0.7pg for beryllium. Beryllium determinations were performed with semi-automatic sample introduction. The novel semi-automatic sampling unit utilised magnetic stirring for· the maintenance of stable slurries and operated with the standard Perkin-Elmer AS-40 autosampler. The principles of this unit were extended to the development of a fully automatic auto-sampling unit. The design and operation of both units are described. The accuracy of the methods was evaluated by analysing standard reference materials and in some cases, comparisons with acid digestion procedures. Data are presented for the analysis of South African coal and fly ash samples. The slurry methods had acceptable accuracy and precision. In comparison with the conventional acid digestion procedures using high pressure bombs, a time-saving advantage was realised.
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    Pixe analysis of adjacent elements
    (1991) Mateta, Nkaro Aldefrida; Peisach, Max; Pougnet, M A Bruno
    Proton induced X-ray emission (PIXE) analysis depends on the accurate stripping of the peaks of individual X-rays from the X-ray energy spectrum produced by the bombardment of a target material with charged particles. The energy separation between the Kᵦ X-ray of element Z and the Kα X-ray of element (Z + 1) increases with increasing Z. Accordingly, for adjacent lower Z elements, there is an overlap in energies between these two X-rays, and hence interference may be caused by one element in the determination of the other. The purpose of this investigation was to determine the extent of such possible interferences and to evaluate the accuracy and precision of the determination of adjacent elements, especially when one of the pair is present in overwhelming concentrations. Two elemental pairs, potassium-calcium, of biological significance, and vanadium-chromium, of metallurgical significance, were studied in detail. Mixtures of stock solutions of the two elements of each pair were made to provide samples with elemental ratios of the minor component decreasing from 10-¹ to 10-⁴ relative to the major one. A minimum of five of these samples were prepared on thin foils as well as on thick target pellets for each concentration level, and the PIXE spectra were recorded under bombardment with protons of 3 MeV. The spectra were analysed off-line by the program AXIL, which, in cases where the minor component could not be visually identified in the spectrum, was forced to evaluate the concentrations of both components. Under these conditions, low levels of the minor component were reported even though the component could not be resolved. All samples, the spectra of which showed the presence of both elements of the elemental pairs, could be analysed in mg/g concentration range. The precision and accuracy of such analysis were acceptable, except in the case of pellets onto which solutions containing both potassium and calcium were deposited. Chromatographic separation of potassium from calcium during the diffusion of the solution in the pellet matrix gave unacceptably erroneous results. When the concentration of the major component exceeded that of the minor by a factor of 200 or more, the presence of the minor component could no longer be recognised in the spectra. When such spectra were analysed by AXIL, forcing the program to determine both elements, results were a reflection of background levels in the energy region of the expected peak. It could therefore be concluded that the determination of the minor component in the presence of the major one for adjacent elements by PIXE is inaccurate for relative concentrations less than 1:200.