Dokument-ID Dokumenttyp Autoren/innen Persönliche Herausgeber/innen Haupttitel Abstract Auflage Verlagsort Verlag Herausgeber (Institution) Erscheinungsjahr Titel des übergeordneten Werkes Jahrgang/Band ISBN Veranstaltung Veranstaltungsort Beginndatum der Veranstaltung Enddatum der Veranstaltung Ausgabe/Heft Erste Seite Letzte Seite URN DOI Lizenz Datum der Freischaltung OPUS4-7248 Vortrag Michaelis, Matthias Einsatz der RFA bei der Zertifzierung von Referenzmaterialien Einsatz der RFA bei der Zertifizierung von Referenzmaterialien Der Bedarf an Referenzmaterialien für die chem. Analytik steigt stetig. Nur durch Einsatz moderner Analysenmethoden kann die Nachfrage gedeckt werden. Die RFA als hochpräzises Verfahren, ist aufgrund der sehr geringen Verfahrensstreuung in der Lage, bei der Beurteilung der Homogenität des Kanditatenmaterials entscheidene Informationen über die Analytverteilung zu liefern. Zur Zertifizierung von Referenzmaterial wird in der anorg. chem. Analytik häufig die ICP-OES eingesetzt. Die RFA, in Kombination mit der Rekonstitutions- und Boratschmelztechnik, ist bei der Zertifizierung eine Analysenmethode, die sich in Bezug auf Probenvorbereitung und Messmethodik grundsätzlich von der ICP-OES unterscheidet. Dadurch trägt sie zur analytischen Methodenvielfalt und damit zur Richtigkeit des zertifizierten Wertes bei und erfüllt zudem im vollsten Maße die Anforderung an metrologischer Rückführbarkeit. 2005 12. Anwendertreffen Röntgenfluoreszenz- und Funkenemissionsspektrometrie; Universität Dortmund 12. Anwendertreffen Röntgenfluoreszenz- und Funkenemissionsspektrometrie; Universität Dortmund Dortmund, Germany 2005-03-14 2005-03-15 2016-02-19 OPUS4-24695 Beitrag zu einem Tagungsband Illerhaus, Bernhard; Badde, Aurelia; Michaelis, Matthias; Berger, U.; Onel, Yener; Meinel, Dietmar; Goebbels, Jürgen Einsatz von mobilen Röntgenuntersuchungsmethoden im Museum. Zwei Fallbeispiele. Zwei Bildhauermodelle aus dem Georg-Kolbe-Museum Berlin standen zur Restaurierung an. Das kleinere, 'Lucino' (1920), 41cm, wurde hochauflösend mit CT gemessen, da mittels CT sowohl der Herstellungsprozeß einer Gipsstatue als auch der innere Zustand, wie Ergänzungen, Klebungen und Armierungen, festgestellt werden können. Aus den CT Bildern ergab sich eine für die vorher vermutete Gipszusammensetzung ungewöhnliche innere Struktur. Mit einer Freihand bedienten Röntgenpistole zur Messung der Röntgenfluoreszenz wurde daraufhin die Zusammensetzung des Materials der Statuette als Terracotta bestimmt. Durch den Einsatz von Helium als Spülmittel konnten auch leichte Materialien nachgewiesen und so eine Unterscheidung zwischen Gips und gebranntem Ton durchgeführt werden. Aus den CT Daten wurde eine virtuelle Darstellung der äußeren Geometrie gewonnen. Ein damit versuchsweise erstelltes Replik (Rapid Prototyping, 3D-Drucker, TU-Berlin) entsprach nicht den Anforderungen des Museums zur Erstellung einer Gußform für eine Bronzekleinserie der Statuette. Die zweite Statue, die 'Große Nacht' (1930) ist mit ihrer Größe von 2,12m und aufgrund des durch korrodierende Metallarmierung verursachten Schadensbildes nicht mehr transportfähig. Eine in-situ Untersuchung mit dem mobilen Tomographen, der in den 1980ern zur Untersuchung von Bäumen gebaut und jetzt mit einem modernen Flachdetektor und einer Röntgenröhre ausgestattet ist, wird vorgestellt. Die Möglichkeiten der in-situ CT für große Skulpturen werden anhand der Ergebnisse diskutiert. Berlin Deutsche Gesellschaft für Zerstörungsfreie Prüfung e.V. (DGZfP) 2010 DGZfP-Jahrestagung 2010 978-3-940283-26-9 DGZfP-Jahrestagung 2010 Erfurt, Deutschland 2010-05-10 2010-05-12 DGZfP-BB 122 (P12) 1 8 2016-02-19 OPUS4-17565 Zeitschriftenartikel Lange, Britta; Recknagel, Sebastian; Czerwensky, Michael; Matschat, Ralf; Michaelis, Matthias; Peplinski, Burkhard; Panne, Ulrich Analysis of pure copper - a comparison of analytical mehods Wien Springer 2008 Microchimica acta 160 97 107 10.1007/s00604-007-0849-1 2016-02-19 OPUS4-17692 Zeitschriftenartikel Brenneis, Rudolf; Kley, Gerd; Köcher, Peter; Michaelis, Matthias Untersuchungen zur ZnO-Reduktion beim Schmelzen von Filterstäuben im elektrischen Lichtbogenofen Berlin Erich Schmidt 2008 Müll und Abfall 40 6 294 300 2016-02-19 OPUS4-17855 Posterpräsentation Peplinski, Burkhard; Adam, Christian; Michaelis, Matthias Reaction sequences in the thermochemical treatment of sewage sludge ashes revealed by X-ray powder diffraction - A contribution to the European project SUSAN 2008 11. European Powder Diffraction Conference (EPDIC-11) 11. European Powder Diffraction Conference (EPDIC-11) Warsaw, Poland 2008-09-19 2008-09-22 2016-02-19 OPUS4-13479 Vortrag Michaelis, Matthias Nichts wissen macht nichts? Erfahrungen mit dem "Standardlosen" Analyseprogramm IQ+. Nichts wissen macht nichts? Erfahrungen mit dem "Standardlosen" Analyseprogramm IQ+. Die moderne semiquantitative Röntgenfluoreszensanalyse bietet als feststoffanalytisches Verfahren die Möglichkeit, chem. Elemente einer völlig unbekannten Probe schnell und zerstörungsfrei qualitativ und quantitativ zu bestimmen. Im Gegensatz zur konventionellen Kalibration, die sich auf eine Elementauswahl beschränkt, wird bei der semiquantitativen RFA das gesamte mögliche Elementspektrum (5?Z?92, B-U) erfasst. Nach einem Scan, der sich in anregungs- und erfassungsoptimierte Teilscans aufteilt, werden aus den Peaklagen zunächst die Elemente erkannt. Aus den Peakhöhen werden dann, über iterativ arbeitende Fundamentalparameter gestützte Rechenprogramme, die Elemente quantitativ bestimmt. Die gebräuchlichen semiquantitativen Programme basieren auf Universalkalibrationen wobei die Probenart (Metall, Glas, Pressling…) nicht berücksichtigt wird. In der BAM wurde nun begonnen, probenspezifische Kalibrationen zu erstellen, so dass die Richtigkeit des Analyseergebnisses gesteigert werden konnte. Ziel ist es, einen großen Teil der analytischen Fragestellungen an ständig wechselnd zusammengesetzten Proben feststoffanalytisch mit der RFA bearbeitbar zu machen. 2006 Panalytical Symposium 2006 Panalytical Symposium 2006 Kassel, Germany 2006-09-19 2006-09-20 2016-02-19 OPUS4-18605 Zeitschriftenartikel Adam, Christian; Peplinski, Burkhard; Michaelis, Matthias; Kley, Gerd; Simon, Franz-Georg Thermochemical treatment of sewage sludge ashes for phosphorus recovery Phosphorus (P) is an essential element for all living organisms and cannot be replaced. Municipal sewage sludge is a carrier of phosphorus, but also contains organic pollutants and heavy metals. A two-step thermal treatment is suggested, including mono-incineration of sewage sludge and subsequent thermochemical treatment of the ashes. Organic pollutants are completely destroyed by mono-incineration. The resulting sewage sludge ashes contain P, but also heavy metals. P in the ashes exhibits low bioavailability, a disadvantage in farming. Therefore, in a second thermochemical step, P is transferred into mineral phases available for plants, and heavy metals are removed as well. The thermochemical treatment was investigated in a laboratory-scale rotary furnace by treating seven different sewage sludge ashes under systematic variation of operational parameters. Heavy metal removal and the increase of the P-bioavailability were the focus of the investigation. The present experimental study shows that these objectives have been achieved with the proposed process. The P-bioavailability was significantly increased due to the formation of new mineral phases such as chlorapatite, farringtonite and stanfieldite during thermochemical treatment. New York, NY Pergamon Press 2009 Waste management 29 3 1122 1128 10.1016/j.wasman.2008.09.011 2016-02-19 OPUS4-20938 Zeitschriftenartikel Simons, C.; Mans, C.; Hanning, S.; Janßen, A.; Radtke, Martin; Reinholz, Uwe; Ostermann, Markus; Michaelis, Matthias; Wienold, Julia; Alber, D.; Kreyenschmidt, M. Study on microscopic homogeneity of polymeric candidate reference materials BAM H001-BAM H010 by means of synchrotron µ-XRF and LA-ICP-MS In this study the microscopic homogeneity of the newly developed plastic reference materials BAM H001-BAM H010 was investigated. The materials consist of an acrylonitryle-butadien-styrene terpolymer, doped with different amounts of the elements Br, Cd, Cr, Hg and Pb. For the quantitative determination of the degree of homogeneity, a procedure proposed by Kempenaers et al. (Fresenius J. Anal. Chem., 2001, 369, 733-737) was used. On every sample an extensive number of different points were analyzed and standard deviation for every element mentioned above was used to calculate a minimal sampling mass that is necessary to reach a certain level of uncertainty caused by inhomogeneity (mmin,5%). The experiments were taken out with synchrotron µ-XRF (SR µ-XRF) at BESSYII in Berlin and by laser ablation inductively coupled plasma mass spectroscopy (LA-ICP-MS). The calculated values for mmin,5% of both techniques showed comparable results for all elements. It could be shown that the materials are suitable for calibration of micro analytic techniques if at least 64 µg are used. London Royal Society of Chemistry 2010 Journal of analytical atomic spectrometry 25 40 43 10.1039/b917008a 2016-02-19 OPUS4-29703 Zeitschriftenartikel Peplinski, Burkhard; Adam, Christian; Adamczyk, Burkart; Müller, Ralf; Schadrack, Reinhard; Michaelis, Matthias; Emmerling, Franziska; Reuther, H.; Menzel, Michael Evidence of formation of the tridymite form of AlPO4 in some municipal sewage sludge ashes Evidence is provided that the tridymite component observed in the X-ray diffraction patterns of some sewage sludge ashes (SSAs) should not be interpreted as the tridymite modification of SiO2 but as the tridymite form of AlPO4. This proof is based on a combined X-ray Powder Diffraction (XRD), X-ray fluorescence (XRF) and Mossbauer spectroscopy investigation of two SSAs produced at two fluidized bed incineration facilities, located in different municipalities and operated differently. The structural and chemical characterization was carried out on the 'as received' SSA samples as well as on the residues of these two SSAs pretreated by leaching in citric acid. In addition, direct proof is presented that the tridymite form of AlPO4 does crystallize from X-ray amorphous precursors under conditions that mimic the huge heating rate and short retention time (just seconds at T ≈ 850 °C) typical for fluidized bed incinerators. Swarthmore, Pa. JCPDS 2013 Powder diffraction 28 S2 S425 S435 10.1017/S0885715613000869 2016-02-20 OPUS4-19349 Zeitschriftenartikel Recknagel, Sebastian; Michaelis, Matthias Certification of the mass fractions of Pt, Pd and Rh in a used car catalyst reference material The high economic value of catalysts containing the platinum group elements platinum, rhodium and palladium as active components causes the need to be able to measure the precious metal loading with small uncertainty and to have suitable certified reference materials fulfilling high demands on the quality of the certified values. In European Reference Material ERM®-EB504, a used cordierite-based car catalyst material, mass fractions of platinum, palladium and rhodium were certified. The raw material was milled, homogenised and annealed before analysis. Seventeen laboratories experienced in precious metals analysis participated in the certification interlaboratory comparison, most of them analysing with inductively coupled plasma optical emission spectrometry using different sample pretreatment techniques. Homogeneity testing was carried out using X-ray fluorescence spectrometry. The certified mass fractions of Pt, Pd and Rh and their expanded uncertainties (k = 2) in ERM®-EB504 are (1777 ± 15), (279 ± 6) and (338 ± 4) mg/kg respectively. Berlin Springer 2009 Accreditation and quality assurance 14 5 277 280 10.1007/s00769-009-0508-9 2016-02-19 OPUS4-23986 Zeitschriftenartikel Wienold, Julia; Recknagel, Sebastian; Scharf, Holger; Hoppe, Marion; Michaelis, Matthias Elemental analysis of printed circuit boards considering the ROHS regulations The EU RoHS Directive (2002/95/EC of the European Parliament and of the Council) bans the placing of new electrical and electronic equipment containing more than agreed levels of lead, cadmium, mercury, hexavalent chromium, polybrominated biphenyl (PBB) and polybrominated diphenyl ether (PBDE) flame retardants on the EU market. It necessitates methods for the evaluation of RoHS compliance of assembled electronic equipment. In this study mounted printed circuit boards from personal computers were analyzed on their content of the three elements Cd, Pb and Hg which were limited by the EU RoHS directive. Main focus of the investigations was the influence of sample pre-treatment on the precision and reproducibility of the results. The sample preparation steps used were based on the guidelines given in EN 62321. Five different types of dissolution procedures were tested on different subsequent steps of sample treatment like cutting and milling. Elemental analysis was carried out using ICP-OES, XRF and CV-AFS (Hg). The results obtained showed that for decision-making with respect to RoHS compliance a size reduction of the material to be analyzed to particles ≤1.5 mm can already be sufficient. However, to ensure analytical results with relative standard deviations of less than 20%, as recommended by the EN 62321, a much larger effort for sample processing towards smaller particle sizes might be required which strongly depends on the mass fraction of the element under investigation. New York, NY Elsevier Ltd. 2011 Waste management 31 3 530 535 10.1016/j.wasman.2010.10.002 2016-02-19 OPUS4-20054 Zeitschriftenartikel Noack, Siegfried; Matschat, Ralf; Michaelis, Matthias Zur Homogenitätsuntersuchung an kompakten metallischen Referenzmaterialproben - Vergleich der Präzisionseigenschaften der Funken-Emissionsspektrometrie und der Röntgenfluoreszenzanalyse Clausthal-Zellerfeld GDMB, Ges. für Bergbau, Metallurgie, Rohstoff- und Umwelttechnik Gesellschaft Deutscher Metallhütten- und Bergleute 2009 World of metallurgy - Erzmetall 62 4 210 223 2016-02-19 OPUS4-20562 Zeitschriftenartikel Peplinski, Burkhard; Adam, Christian; Michaelis, Matthias; Kley, Gerd; Emmerling, Franziska; Simon, Franz-Georg Reaction sequences in the thermochemical treatment of sewage sludge ashes revealed by X-ray powder diffraction - A contribution to the European project SUSAN The sequence of reactions accompanying the thermochemical treatment of an iron- and aluminium-bearing sewage sludge ash was ascertained by investigating two systematic series of samples. The ash was thermochemically treated in a lab-scale rotary furnace after mixing it with a chlorine-donor, either CaCl2 or MgCl2. Within each of these two sample series only a single process parameter, the reaction temperature, was varied, namely between 350 and 1050°C. It was found, that among the numerous crystalline phases present in the raw ash only quartz and hematite continue to exist after thermochemical treatments carried out at 1050°C, whereas all other components undergo at least one decomposition-recrystallization cycle. Some of the components re-crystallize even several times. It was proved that the restructuring of the calcium- and phosphorus-bearing mineral phases proceeds via the formation of chlorspodioside, Ca2PO4Cl. The influence of the type of chlorine-donor on the final product was elucidated in detail and - to the best of our knowledge - for the first time crystalline AlPO4 was found in a sewage sludge ash and its decomposition was investigated, too. München Oldenbourg Deutsche Gesellschaft für Kristallographie 2009 Zeitschrift für Kristallographie / Supplement issue 30 EPDIC 2008 459 464 10.1524/zksu.2009.0068 2016-02-19 OPUS4-33435 Zeitschriftenartikel Peplinski, Burkhard; Adam, Christian; Adamczyk, Burkart; Müller, Ralf; Michaelis, Matthias; Krahl, T.; Emmerling, Franziska Nanocrystalline and stacking-disordered beta-cristobalite AlPO4: the now deciphered main constituent of a municipal sewage sludge ash from a full-scale incineration facility For the first time evidence is provided that a nanocrystalline and stacking-disordered, chemically stabilized β-cristobalite form of AlPO4 occurs in a sewage sludge ash (SSA). This proof is based on a combined X-ray powder diffraction and X-ray fluorescence investigation of an SSA produced at a large-scale fluidized bed incineration facility serving a catching area with a population of 2 million. The structural and chemical characterization was carried out on 'as received' SSA samples as well as on solid residues remaining after leaching this SSA in sodium hydroxide solution. Thus, it was ascertained that the observed nanocrystalline and stacking-disordered cristobalite-like component belongs to the aluminum phosphate component of this SSA, rather than to its silicon dioxide component. In addition, a direct proof is presented that the chemically stabilized β-cristobalite form of AlPO4 does crystallize from X-ray amorphous precursors under conditions that mimic the huge heating rate and short retention time (just seconds at T ≈ 850°C), typical for fluidized bed incinerators. Swarthmore, Pa. JCPDS 2015 Powder diffraction 30 Supplement S 1 S31 S35 10.1017/S0885715614001213 2016-02-20 OPUS4-52088 Zeitschriftenartikel Andresen, Elina; Resch-Genger, Ute; Michaelis, Matthias; Prinz, Carsten; Würth, Christian Time-resolved luminescence spectroscopy for monitoring the stability and dissolution behaviour of upconverting nanocrystals with different surface coatings† We demonstrate the potential of time-resolved luminescence spectroscopy for the straightforward assessment and in situ monitoring of the stability of upconversion nanocrystals (UCNPs). Therefore, we prepared hexagonal NaYF4:Yb3+,Er3+ UCNPs with various coatings with a focus on phosphonate ligands of different valency, using different ligand exchange procedures, and studied their dissolution behaviour in phosphate-buffered saline (PBS) dispersions at 20 °C and 37 °C with various analytical methods. The amount of the released UCNPs constituting fluoride ions was quantified by potentiometry using a Fluoride ion-sensitive electrode and particle disintegration was confirmed by transmission electron microscopy studies of the differently aged UCNPs. In parallel, the luminescence features of the UCNPs were measured with special emphasis on the lifetime of the sensitizer emission to demonstrate its suitability as Screening parameter for UCNP stability and changes in particle composition. The excellent correlation between the changes in luminescence lifetime and fluoride concentration highlights the potential of our luminescence lifetime method for UCNP stability screening and thereby indirect monitoring of the release of potentially hazardous fluoride ions during uptake and dissolution in biological systems. Additionally, the developed in situ optical method was used to distinguish the dissolution dynamics of differently sized and differently coated UCNPs. Royal Society od Chemistry 2020 Nanoscale 12 23 12589 12601 10.1039/d0nr02931a 2021-02-10