caa a22 4500 44588097X CHVBK 20180317145543.0 cr unu---uuuuu 170323e20110401xx s 000 0 eng 10.1007/s00604-011-0546-y doi (NATIONALLICENCE)springer-10.1007/s00604-011-0546-y Micro-homogeneity studies of boron carbide powders [Elektronische Daten] [Alexander Kadenkin, Martin Amberger, Ursula Fittschen, José Broekaert] We have studied the micro-homogeneity of boron carbide powders by inductively coupled plasma optical emission spectrometry (ICP-OES) and total reflection X-ray fluorescence spectrometry (TXRF) using slurry sampling. To get information on the particle size distributions of the powders, the stabilized slurries of boron carbide powders were nebulized, the aerosols were transported into a Batelle impactor and the droplets were collected on the impactor stages bearing TXRF sample holders. In a first series of measurements, parameters of the impaction like the duration of the impaction and the use of glutinous substance on the sample holders were optimized. The different mass size fractions for industrial boron carbide powders were determined by weight measurements of the fractions collected on the different stages. The established particle size distributions were in the range of 0.5 to >16μm and found similar to those determined by laser diffraction reported elsewhere. Analyses of the mass fractions by slurry sampling TXRF showed that Ca, Ti, Cr, Mn, Fe, Ni and Cu within the measurements errors were homogeneously distributed over the mass fractions between 0.5 and 4μm and that their concentrations agreed with the bulk composition, as determined with ICP-OES subsequent to digestion. However, light underestimates were found at the 5 (Mn) up to 150μgg−1 (Fe) level. Finally, boron carbide powders were washed out with nitric acid with different concentrations and leaching solutions and the residues were analyzed by ICP-OES and TXRF respectively. It is shown that up to 60% of the residual trace impurities in the powder studied can be removed by leaching with 34% (v/v) of nitric acid. Figure The trace element concentrations over different particle size fractions in boron carbide powders could be shown by total reflection x-ray fluorescence spectrometric measurements at the cascade impactor separated fractions not to vary too much over the different fractions. Springer-Verlag, 2011 Boron carbide nationallicence Micro-homogeneity nationallicence ICP-OES nationallicence TXRF nationallicence Impaction nationallicence Kadenkin Alexander Department of Chemistry, Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146, Hamburg, Germany aut Amberger Martin Department of Chemistry, Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146, Hamburg, Germany aut Fittschen Ursula Department of Chemistry, Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146, Hamburg, Germany aut Broekaert José Department of Chemistry, Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146, Hamburg, Germany aut Microchimica Acta Springer Vienna 173/1-2(2011-04-01), 183-188 0026-3672 173:1-2<183 2011 173 604 https://doi.org/10.1007/s00604-011-0546-y text/html Onlinezugriff via DOI 1 research-article jats NATIONALLICENCE 856 40 https://doi.org/10.1007/s00604-011-0546-y text/html Onlinezugriff via DOI NATIONALLICENCE 700 1- Kadenkin Alexander Department of Chemistry, Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146, Hamburg, Germany aut NATIONALLICENCE 700 1- Amberger Martin Department of Chemistry, Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146, Hamburg, Germany aut NATIONALLICENCE 700 1- Fittschen Ursula Department of Chemistry, Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146, Hamburg, Germany aut NATIONALLICENCE 700 1- Broekaert José Department of Chemistry, Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146, Hamburg, Germany aut NATIONALLICENCE 773 0- Microchimica Acta Springer Vienna 173/1-2(2011-04-01), 183-188 0026-3672 173:1-2<183 2011 173 604 Metadata rights reserved Springer special CC-BY-NC licence nationallicence BK010053 XK010053 XK010000 NATIONALLICENCE NATIONALLICENCE NL-springer