TY - JOUR A1 - Peplinski, Burkhard A1 - Feldmann, Ines A1 - Adam, Karin T1 - Können 5 ng oder 30 ng/g einer Nebenphase das Diffraktogramm einer Pulverprobe signifikant verändern? T2 - Gemeinsame Jahrestagung der Deutschen Gesellschaft für Kristallographie e. V. und der Deutschen Gesellschaft für Kristallwachstum und Kristallzüchtung e. V. CY - Jena DA - 2004-03-15 PY - 2004 SN - 0930-486X SP - 109 PB - Oldenbourg CY - München AN - OPUS4-3432 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stemann, Jan A1 - Peplinski, Burkhard A1 - Adam, Christian T1 - Thermochemical treatment of sewage sludge ash with sodium salt additives for phosphorus fertilizer production - Analysis of underlying chemical reactions N2 - Stocks of high grade phosphate rock are becoming scarce, and there is growing concern about potentially harmful impurities in conventional phosphorus fertilizers. Sewage sludge ash is a promising secondary phosphorus source. However, to remove heavy metals and convert the phosphorus contained in sewage sludge ash into mineral phases available to plants, an after-treatment is required. Laboratory-scale calcination experiments of sewage sludge ash blended with sodium salts using dried sewage sludge as a reducing agent were carried out at 1000 °C. Thus, the Ca3(PO4)2 or whitlockite component of raw sewage sludge ash, which is not readily plant available, was converted to CaNaPO4 (buchwaldite). Consequently, nearly complete phosphorus solubility in ammonium citrate (a well-established indicator for plant availability) was achieved. Moreover, it was shown that Na2CO3 may be replaced by moderately priced Na2SO4. However, molar ratios of Na/P > 2 were required to achieve >80% phosphorus solubility. Such over-stoichiometric Na consumption is largely caused by side reactions with the SiO2 component of the sewage sludge ash – an explanation for which clear evidence is provided for the first time. KW - Phosphorus recovery KW - Plant availability KW - Solubility in ammonium citrate KW - Whitlockite-to-buchwaldite transformation PY - 2015 DO - https://doi.org/10.1016/j.wasman.2015.07.029 SN - 0956-053X VL - 45 SP - 385 EP - 390 PB - Pergamon Press CY - New York, NY AN - OPUS4-33876 LA - eng 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 DO - 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 - Adam, Christian A1 - Peplinski, Burkhard A1 - Kley, Gerd A1 - Kratz, S. A1 - Schick, J. A1 - Schnug, E. T1 - Phosphorrückgewinnung aus Klärschlammaschen - Ergebnisse aus dem EU-Projekt SUSAN N2 - Phosphor ist ein für alle Lebewesen essenzielles Element und kann in seinen Funktionen z. B. als Bestandteil der DNS und RNS sowie als Schlüsselelement beim Energiestoffwechsel (ADP/ATP) nicht ersetzt werden. Klärschlammaschen sind aufgrund ihrer hohen Gehalte an Phosphor (15–25 % P2O5) geeignete Sekundärrohstoffe für die Herstellung von P-Düngemitteln. Aufgrund der schlechten Pflanzenverfügbarkeit des Phosphors und der Gehalte an umweltrelevanten Schwermetallen sollten diese allerdings nicht direkt in der Landwirtschaft eingesetzt werden. Im Mittelpunkt des EU-Projekts SUSAN steht die Entwicklung und Optimierung einer thermochemischen Behandlung von Klärschlammaschen, mit der die Düngewirkung der Aschen auf das Niveau konventioneller Mineraldünger (Thomaskali und Superphosphat SSP) angehoben wird und die Schwermetallkonzentrationen unter die Grenzwerte nach Düngemittelverordnungen europäischer Länder abgesenkt werden. Die sehr positiven Ergebnisse, die bisher im SUSAN-Projekt erzielt wurden, und die darauf basierenden ökonomischen Betrachtungen legen eine großtechnische Umsetzung des Verfahrens nahe. KW - Klärschlamm KW - Phosphor KW - Ressource KW - Klärschlammasche KW - P-Düngemittel KW - Mineralische Phasen PY - 2008 DO - https://doi.org/10.1007/s00506-008-0152-3 SN - 0945-358X SN - 1613-7566 VL - 60 IS - 3-4 SP - 55 EP - 64 PB - Springer CY - Wien AN - OPUS4-17449 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Adam, Christian A1 - Peplinski, Burkhard A1 - Wellendorf, Stephan T1 - Chemical reactions during the preparation of P and NPK fertilizers from thermochemically treated sewage sludge ashes KW - NPK fertilizer KW - P fertilizer KW - Phosphorus recycling KW - Sewage sludge ash KW - Urban mining PY - 2010 DO - https://doi.org/10.1111/j.1747-0765.2010.00485.x SN - 0038-0768 SN - 1747-0765 VL - 56 IS - 4 SP - 627 EP - 635 PB - Blackwell Publ. Asia CY - Tokyo, Japan AN - OPUS4-21924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donėlienė, J. A1 - Rudzikas, M. A1 - Rades, Steffi A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Sahre, Mario A1 - Pellegrino, F. A1 - Maurino, V. A1 - Ulbikas, J. A1 - Galdikas, A. A1 - Hodoroaba, Vasile-Dan T1 - Morphology and structure of TixOy nanoparticles generated by femtosecond laser ablation in water N2 - In this work femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated byXRD(two instruments operated in different geometries) and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. KW - Titanium oxide KW - Nanoparticles KW - Laser ablation in liquid KW - Particle morphology KW - Nanoparticle structure PY - 2018 DO - https://doi.org/10.1088/2053-1591/aaba56 SN - 2053-1591 VL - 5 IS - 4 SP - 045015-1 EP - 045015-12 PB - IOP Publishing CY - London, UK AN - OPUS4-44678 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Petzet, S. A1 - Peplinski, Burkhard A1 - Cornel, P. T1 - On wet chemical phosphorus recovery from sewage sludge ash by acidic or alkaline leaching and an optimized combination of both N2 - The advantages and drawbacks of existing wet chemical phosphorus (P) recovery technologies, their applicability to different types of sewage sludge ash (SSA) and the role of the decay products of detergent zeolites as a source of reactive Al in SSA are analyzed. Since neither a purely acidic nor a purely alkaline treatment are able to provide satisfactory technical solutions a wet chemical phosphorus (P) recovery process for sewage sludge ashes (SSAs) is investigated in detail that is based on a sequential treatment of SSA with an acid and a base. As a result of an acidic pre-treatment, the P fraction of the raw SSA that was bound as – alkaline-insoluble – calcium phosphate (Ca–P) is converted into aluminum phosphate (Al–P). This newly formed Al–P can be easily dissolved via alkaline treatment and then easily separated from the alkaline leachate via precipitation of Ca–P. The Al-component can be reused as precipitant for P-removal in waste water treatment plants (WWTPs). The investigated process requires fewer chemicals than the direct acidic dissolution of all P-compounds contained in the SSA. This is due to the described rearrangement of the P component from Ca–P to Al–P. That such a rearrangement of P occurs indeed was confirmed through a combination of XRD, ICP and XRF analyses together with mass balance calculations. The present investigation proves that the process works for very different types of SSAs: For Al-rich SSAs that come from WWTPs where Al-salt is used for chemical P-removal the described sequential treatment process works best and yields P-recovery rates as high as 70–77%. But even for SSAs from WWTPs where only iron salt is used for chemical P-removal, a considerable amount of the reactive Al necessary for the described P-rearrangement is supplied by decay products of detergent zeolites, a hidden Al-source present in most SSAs produced in Europe. KW - Phosphorus recovery KW - Sewage sludge ash KW - Alkaline and acidic leaching KW - Calcium phosphate KW - Aluminum phosphate KW - Detergent zeolites KW - XRD analysis PY - 2012 DO - https://doi.org/10.1016/j.watres.2012.03.068 SN - 0043-1354 VL - 46 IS - 12 SP - 3769 EP - 3780 PB - Elsevier CY - Amsterdam AN - OPUS4-26005 LA - eng 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 DO - 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 - Reuther, H. A1 - Vogel, Christian A1 - Adamczyk, Burkart A1 - Menzel, Michael A1 - Emmerling, Franziska A1 - Simon, Franz-Georg T1 - First identification of the tridymite form of AlPO4 in municipal sewage sludge ash N2 - Sewage sludge and sewage sludge ashes (SSA) are produced in huge amounts at municipal waste water treatment plants (WWTP) all around the world and have become an issue for many urbanized areas. To deal with this unceasing mass flow in an ecologically and economically responsible way a comprehensive chemical and structural characterization of all types of SSA is needed. X-ray powder diffraction (XRD) is one of the most promising analytical methods for this task. Although, there has been ample chemical evidence showing that many SSA contain aluminium phosphate as a major component up to now no aluminium phosphate or aluminium-rich mixed phosphate phase has been reported to be identified by XRD in a SSA produced at a mono-incineration facility. The outcome of the present com-bined XRD and Mossbauer spectroscopy investigation provides comprehensive evidence closing this gap for the first time. KW - Aluminium phosphate KW - AlPO4 KW - Tridymite KW - Sewage sludge ash KW - Incinerator KW - Ash PY - 2011 DO - https://doi.org/10.1524/zkpr.2011.0067 SN - 0044-2968 VL - 1 SP - 443 EP - 448 PB - Oldenbourg CY - München AN - OPUS4-24297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Fitch, A.N. A1 - Evans, A. A1 - Ibberson, R.M. A1 - Többens, D.M. A1 - Cranswick, L.M.D. A1 - Dörfel, Ilona A1 - Emmerling, Franziska A1 - Matschat, Ralf T1 - Structural characterization of a coarse-grained transparent silicon carbide powder by a combination of powder diffraction techniques N2 - Diffraction of hard synchrotron radiation as well as constant-wavelength and time-of-flight neutron diffraction were used for the structural characterization of a silicon carbide powder having extremely low levels of chemical impurities, high perfection of the crystalline lattice and a grain size of up to 150 µm. The presence of three polytypes was ascertained and the ratios of their mass fractions were determined to be w15R : w6H = 0.002,3(8) and w4H : w6H = 0.000,6(2). KW - Silicon carbide KW - Polytypes KW - Phase quantification KW - Reference material PY - 2009 DO - https://doi.org/10.1524/zksu.2009.0009 SN - 0930-486X VL - 30 EPDIC 2008 SP - 61 EP - 66 PB - Oldenbourg CY - München AN - OPUS4-20561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -