Direct analysis of Al2O3 powders by total reflection X-ray fluorescence spectrometry
A direct analysis procedure for the determination of trace impurities of Ca, V, Cr, Mn, Fe, Ni, Cu, Zn and Ga in Al2O3 ceramic powders by total reflection X-ray fluorescence spectrometry (TXRF) is described. The powders were analysed in the form of slurries containing 1–10 mg mL−1 of powder. The use of the procedure in the case of powders with differing grain size and for different slurry concentrations was investigated. Three different quantification possibilities were compared, namely the use of Al as a matrix component, the use of Fe as a trace element contained in the sample or of Co added in concentrations of 200 μg g−1 as internal standard. The homogeneity of elemental distributions in sample layers deposited on the TXRF quartz carriers by evaporating 5 μL of the 10 mg mL−1 slurries was studied by scanning the 4- to 5-mm-diameter spots of two samples by synchrotron radiation TXRF at Hasylab. For powders with differing graininess but mainly finer than about a few 10 μm, no systematic influence of the grain size on the accuracy of the determinations of Ca, V, Fe, Ni, Cu and Zn could be observed. The measurement precision, however, seemed to be limited by inhomogeneous distributions of the trace elements in the samples as testified by the synchrotron radiation TXRF scans. Detection limits of the developed TXRF procedure for Ca, V, Cr, Mn, Fe, Ni, Cu, Zn and Ga were found to be in the 0.3–7 μg g−1 range and were shown to increase slightly with the grain size of the samples. Quantification using Al (matrix) as internal standard led to systematically higher values out of the accuracy required, whereas the other two approaches in all cases led to reliable results.
Three empirical cases of the deposition morphology influence in the analytical quality of direct solid suspension measurements by total-reflection X-ray fluorescence
This work describes three empirical cases where the influence of the microscopic and macroscopic morphology of the sample depositions analyzed by total-reflection X-ray fluorescence with respect to the accuracy and uncertainties of its analytical results is shown. The first case was the direct solid analysis of reference clay, where a strong dependence between the accuracy and the uncertainty of the evaluated elements with respect to the microscopic morphology of the depositions obtained in water and toluene liquid medium was observed. The second case was the analysis of a solid suspension of magnetite nanoparticles, where the evaluation of the different macroscopic deposition morphologies, for different kinds of sample carriers and evaporation processes, produces an important variation of the uncertainty associated to the Fe measurements but not for its nominal values. Finally, the third case was the analysis of Ru and Se impregnated in carbon nanoparticles. In this case, the ultrasonic modifications of the particle size distributions in the solid suspensions, together with the macroscopic morphology variation of its solid depositions, produce drastic consequences in the uncertainties associated with the metallic content.
Effective adsorption of lead ions using fly ash obtained in the novel circulating fluidized bed combustion technology
Abstract Fly ash was examined for the separation efficiency of Pb2+ ions from water in batch experiments. Fly ash is industrial waste produced from the incineration of sewage sludge by the novel circulating fluidized bed combustion (CFBC) technology and was taken into the experiments. Physical and chemical properties of the material were characterized using several methods, such as fraction analysis, particle size distribution, bulk density, composition, morphology, surface and internal structure by elemental analysis, FT-IR, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction analysis, comprehensive thermal analysis, fly ash texture by BET adsorption isotherms, specific surface area, volume of pores, average pore diameter and pore volume distribution by the BJH method. The influence of pH values on zeta potential of the fly ash surface before and after the adsorption process was conducted. The calculated maximum adsorption capacity of Pb2+ by fly ash reached 51.98 mg/g. The kinetic analysis revealed that the adsorption process is better described by the pseudo-second order equation and it is well fitted to the Freundlich model. In conclusion, fly ash obtained in the CFBC technology is a promising low cost adsorbent for the highly effective recovery of Pb2+ from wastewater.