TY - JOUR A1 - Kadenkin, Alexander A1 - Broekaert, J.A.C. T1 - Studies with a miniaturized microwave induced plasma for element specific detection in gas chromatographic separations of halogenated hydrocarbons N2 - The possibilities of a helium microstrip microwave induced plasma, operated at less than 40 W and less than 250 mL min-1 of gas, as source for optical emission spectrometry (MSP-OES) were studied for the element specific detection of halogenated volatile organic compounds, such as chlorinated and brominated alkanes and arenes, after their separation by capillary gas chromatography (GC). After hyphenation of the GC with MSP-OES with the aid of a heated transfer line, different gas chromatographic parameters, like the carrier gas flow (1.4–3.3 mL min-1) and the oven temperature (100–200), as well as different plasma specific parameters, like the forward power (30–40 W) and the plasma gas flow (100–200 mL min-1), were optimized. In the next step, rotational and excitation temperatures of microstrip plasma were studied in dependence on analyte concentrations between 1 and 10% v/v in pentane and found to be in the order of 1250–1650, as measured with OH bands, and 6100–6900 K, as measured with Fe-lines from ferrocene vapor entered in the plasma gas, respectively. Further, it could be shown that the hyphenated technique GC-MSP-OES can be used for the determination of volatile halogenated organic compounds under the use of an internal standard with recovery rates at the order of 90–110% at the 2–5 mg g-1 level. The absolute limits of detection for volatile halogenated organic compounds, obtained with GC-MSP-OES and the Cl I 837.594 nm, Br I 827.244 nm and C I 247.856 nm, were found to be in the ng-range and the relative detection limits in pentane in the µL L-1 range. KW - Gas chromatography KW - Microwave induced plasma PY - 2011 DO - https://doi.org/10.1039/c1ja10028a SN - 0267-9477 SN - 1364-5544 VL - 26 IS - 7 SP - 1481 EP - 1487 PB - Royal Society of Chemistry CY - London AN - OPUS4-24160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kadenkin, Alexander A1 - Amberger, M. A1 - Fittschen, U.E.A. A1 - Broekaert, J.A.C. T1 - Micro-homogeneity studies of boron carbide powders N2 - 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 >16 µm 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 4 µm 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 150 µg g-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. KW - Boron carbide KW - Micro-homogeneity KW - ICP-OES KW - TXRF KW - Impaction PY - 2011 DO - https://doi.org/10.1007/s00604-011-0546-y SN - 0026-3672 SN - 1436-5073 VL - 173 IS - 1-2 SP - 183 EP - 188 PB - Springer CY - Wien AN - OPUS4-24161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kadenkin, Alexander T1 - Determination of salt pollutants in building materials using Raman spectroscopy T2 - TECHNART 2011 CY - Berlin, Germany DA - 2011-04-26 PY - 2011 AN - OPUS4-24128 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kadenkin, Alexander T1 - Laser induced breakdown spectroscopy with the use of fast diode pumped solid state laser T2 - EUROANALYSIS 16 CY - Belgrade, Serbia DA - 2011-09-11 PY - 2011 AN - OPUS4-24632 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kadenkin, Alexander T1 - Laser induced breakdown spectroscopy with the use of fast diode pumped solid state laser T2 - Doktorandenseminar Spektroskopie und Spurenanalytik der Arbeitskreise DASp und A.M.S.El. CY - Mainz, Germany DA - 2012-07-09 PY - 2012 AN - OPUS4-27301 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -