TY - CONF A1 - Michaelis, Matthias T1 - Einsatz der RFA bei der Zertifzierung von Referenzmaterialien N2 - 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. T2 - 12. Anwendertreffen Röntgenfluoreszenz- und Funkenemissionsspektrometrie; Universität Dortmund CY - Dortmund, Germany DA - 2005-03-14 PY - 2005 AN - OPUS4-7248 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard A1 - Badde, Aurelia A1 - Michaelis, Matthias A1 - Berger, U. A1 - Onel, Yener A1 - Meinel, Dietmar A1 - Goebbels, Jürgen T1 - Einsatz von mobilen Röntgenuntersuchungsmethoden im Museum. Zwei Fallbeispiele. N2 - 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. T2 - DGZfP-Jahrestagung 2010 CY - Erfurt, Deutschland DA - 2010-05-10 KW - Mobile CT KW - Mobile RFA PY - 2010 SN - 978-3-940283-26-9 IS - DGZfP-BB 122 (P12) SP - 1 EP - 8 CY - Berlin AN - OPUS4-24695 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, Britta A1 - Recknagel, Sebastian A1 - Czerwensky, Michael A1 - Matschat, Ralf A1 - Michaelis, Matthias A1 - Peplinski, Burkhard A1 - Panne, Ulrich T1 - Analysis of pure copper - a comparison of analytical mehods KW - Pure copper KW - Elemental analytical mehtods KW - Reference material KW - Sample dissolution PY - 2008 U6 - https://doi.org/10.1007/s00604-007-0849-1 SN - 0026-3672 SN - 1436-5073 VL - 160 SP - 97 EP - 107 PB - Springer CY - Wien AN - OPUS4-17565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brenneis, Rudolf A1 - Kley, Gerd A1 - Köcher, Peter A1 - Michaelis, Matthias T1 - Untersuchungen zur ZnO-Reduktion beim Schmelzen von Filterstäuben im elektrischen Lichtbogenofen KW - Filterstäube aus Müllverbrennungsanlagen KW - Elektrischer Lichtbogenofen KW - Inertisierung KW - ZnO-Reduktion KW - Röntgenfluoreszenzanalyse PY - 2008 SN - 0027-2957 SN - 1863-9763 VL - 40 IS - 6 SP - 294 EP - 300 PB - Erich Schmidt CY - Berlin AN - OPUS4-17692 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Peplinski, Burkhard A1 - Adam, Christian A1 - Michaelis, Matthias A1 - Kley, Gerd A1 - Emmerling, Franziska A1 - Simon, Franz-Georg T1 - Reaction sequences in the thermochemical treatment of sewage sludge ashes revealed by X-ray powder diffraction - A contribution to the European project SUSAN T2 - 11. European Powder Diffraction Conference (EPDIC-11) CY - Warsaw, Poland DA - 2008-09-19 PY - 2008 AN - OPUS4-17855 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Michaelis, Matthias T1 - Nichts wissen macht nichts? Erfahrungen mit dem "Standardlosen" Analyseprogramm IQ+. N2 - 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. T2 - Panalytical Symposium 2006 CY - Kassel, Germany DA - 2006-09-19 PY - 2006 AN - OPUS4-13479 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adam, Christian A1 - Peplinski, Burkhard A1 - Michaelis, Matthias A1 - Kley, Gerd A1 - Simon, Franz-Georg T1 - Thermochemical treatment of sewage sludge ashes for phosphorus recovery N2 - 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. KW - P-recovery KW - Sewage sludge ash KW - Thermochemical treatment KW - Mineral phases KW - X-ray diffraction PY - 2009 U6 - https://doi.org/10.1016/j.wasman.2008.09.011 SN - 0956-053X VL - 29 IS - 3 SP - 1122 EP - 1128 PB - Pergamon Press CY - New York, NY AN - OPUS4-18605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simons, C. A1 - Mans, C. A1 - Hanning, S. A1 - Janßen, A. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Ostermann, Markus A1 - Michaelis, Matthias A1 - Wienold, Julia A1 - Alber, D. A1 - Kreyenschmidt, M. T1 - Study on microscopic homogeneity of polymeric candidate reference materials BAM H001-BAM H010 by means of synchrotron µ-XRF and LA-ICP-MS N2 - 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. KW - XRF KW - LA-ICP-MS KW - RoHS KW - CRM PY - 2010 U6 - https://doi.org/10.1039/b917008a SN - 0267-9477 SN - 1364-5544 VL - 25 SP - 40 EP - 43 PB - Royal Society of Chemistry CY - London AN - OPUS4-20938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Müller, Ralf A1 - Schadrack, Reinhard A1 - Michaelis, Matthias A1 - Emmerling, Franziska A1 - Reuther, H. A1 - Menzel, Michael T1 - Evidence of formation of the tridymite form of AlPO4 in some municipal sewage sludge ashes N2 - 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. KW - Aluminium phosphate KW - Ash KW - Fly ash KW - Incinerator ash KW - Sewage sludge ash KW - Tridymite form PY - 2013 U6 - https://doi.org/10.1017/S0885715613000869 SN - 0885-7156 VL - 28 IS - S2 SP - S425 EP - S435 PB - JCPDS CY - Swarthmore, Pa. AN - OPUS4-29703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Michaelis, Matthias T1 - Certification of the mass fractions of Pt, Pd and Rh in a used car catalyst reference material N2 - 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. KW - Precious metals KW - CRM KW - European reference material KW - Platinum KW - Rhodium KW - Palladium KW - ICP OES PY - 2009 U6 - https://doi.org/10.1007/s00769-009-0508-9 SN - 0949-1775 SN - 1432-0517 VL - 14 IS - 5 SP - 277 EP - 280 PB - Springer CY - Berlin AN - OPUS4-19349 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wienold, Julia A1 - Recknagel, Sebastian A1 - Scharf, Holger A1 - Hoppe, Marion A1 - Michaelis, Matthias T1 - Elemental analysis of printed circuit boards considering the ROHS regulations N2 - 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. KW - RoHS KW - Printed circuit boards KW - Electrotechnical products KW - Elemental composition PY - 2011 U6 - https://doi.org/10.1016/j.wasman.2010.10.002 SN - 0956-053X VL - 31 IS - 3 SP - 530 EP - 535 PB - Elsevier Ltd. CY - New York, NY AN - OPUS4-23986 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Noack, Siegfried A1 - Matschat, Ralf A1 - Michaelis, Matthias T1 - Zur Homogenitätsuntersuchung an kompakten metallischen Referenzmaterialproben - Vergleich der Präzisionseigenschaften der Funken-Emissionsspektrometrie und der Röntgenfluoreszenzanalyse KW - Röntgenfluoreszenzanalyse KW - Funkenspektrometrie KW - Homogenitätstest KW - Verfahrenspräzision KW - Referenzmaterialien PY - 2009 SN - 1613-2394 VL - 62 IS - 4 SP - 210 EP - 223 PB - GDMB, Ges. für Bergbau, Metallurgie, Rohstoff- und Umwelttechnik CY - Clausthal-Zellerfeld AN - OPUS4-20054 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adam, Christian A1 - Michaelis, Matthias A1 - Kley, Gerd A1 - Emmerling, Franziska A1 - Simon, Franz-Georg T1 - Reaction sequences in the thermochemical treatment of sewage sludge ashes revealed by X-ray powder diffraction - A contribution to the European project SUSAN N2 - 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. KW - XRD KW - Phosphorus recovery KW - Sewage sludge ash KW - Urban mining KW - Fertilizers PY - 2009 U6 - https://doi.org/10.1524/zksu.2009.0068 SN - 0930-486X VL - 30 EPDIC 2008 SP - 459 EP - 464 PB - Oldenbourg CY - München AN - OPUS4-20562 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Müller, Ralf A1 - Michaelis, Matthias A1 - Krahl, T. A1 - Emmerling, Franziska T1 - Nanocrystalline and stacking-disordered beta-cristobalite AlPO4: the now deciphered main constituent of a municipal sewage sludge ash from a full-scale incineration facility N2 - 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. KW - Aluminum phosphate KW - Chemical stabilization of high-temperature forms KW - Cristobalite form KW - Stacking disorder KW - Incinerator ash KW - Sewage sludge ash PY - 2015 U6 - https://doi.org/10.1017/S0885715614001213 SN - 0885-7156 VL - 30 IS - Supplement S 1 SP - S31 EP - S35 PB - JCPDS CY - Swarthmore, Pa. AN - OPUS4-33435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Andresen, Elina A1 - Resch-Genger, Ute A1 - Michaelis, Matthias A1 - Prinz, Carsten A1 - Würth, Christian T1 - Time-resolved luminescence spectroscopy for monitoring the stability and dissolution behaviour of upconverting nanocrystals with different surface coatings† N2 - 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. KW - Fluorescence KW - Lifetime KW - Method KW - Quantification KW - Stability KW - Coating KW - Surface chemistry KW - Lanthanide KW - Fluoride KW - Electrochemistry KW - ICP-OES KW - Upconversion KW - Nano KW - Particle KW - Aging KW - Quality assurance KW - TEM PY - 2020 U6 - https://doi.org/10.1039/d0nr02931a VL - 12 IS - 23 SP - 12589 EP - 12601 PB - Royal Society od Chemistry AN - OPUS4-52088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -