TY - JOUR A1 - Vogl, Jochen A1 - Quétel, C. A1 - Ostermann, Markus A1 - Papadakis, I. A1 - Van Nevel, L. A1 - Taylor, P.D.P. T1 - Contribution to the certification of B, Cd, Mg, Pb, Rb, Sr, and U in a natural water sample for the International Measurement Evaluation Programme Round 9 (IMEP-9) using ID-ICP-MS JF - Accreditation and quality assurance N2 - The present paper describes the contribution of the Institute for Reference Materials and Measurements to the certification of B, Cd, Mg, Pb, Rb, Sr, and U amount contents in a natural water sample, in round 9 of the International Measurement Evaluation Programme (IMEP-9). The analytical procedure to establish the reference values for B, Cd, Mg, Pb, Rb, Sr, and U amount contents was based on isotope dilution inductively coupled plasma-mass spectrometry used as a primary method of measurement. Applying this procedure reference values, traceable to the SI, were obtained for the natural water sample of IMEP-9. For each of the certified amount contents presented here a total uncertainty budget was calculated using the method of propagation of uncertainties according to ISO and EURACHEM guidelines. The measurement procedures, as well as the uncertainty calculations are described for all seven elements mentioned above. In order to keep the whole certification process transparent and so traceable, the preparations of various reagents and materials as well as the sample treatment and blending, the measurements themselves, and finally the data treatment are described in detail. Explanations focus on Pb as a representative example. The total uncertainties (relative) obtained were less than 2% for all investigated elements at amount contents in the pmol/kg up to the high 7mol/kg range, corresponding to low 7g/kg and mg/kg levels. KW - IMEP-9 KW - ID-ICP-MS KW - IDMS KW - Uncertainty budget KW - Certification PY - 2000 DO - https://doi.org/10.1007/s007690000145 SN - 0949-1775 SN - 1432-0517 VL - 5 SP - 272 EP - 279 PB - Springer CY - Berlin AN - OPUS4-7216 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Ostermann, Markus A1 - Becker, Dorit A1 - Janisch, N. T1 - Zertifiziertes Referenzmaterial ERM-AE104 bzw. BAM-I004 N2 - Dieser Bericht beschreibt die Zertifizierung einer synthetischen Isotopenmischung aus natürlicher und angereicherter Borsäure. Dieses Isotopen-ZRM liegt als konzentrierte, wässerige Borsäure-Lösung vor und ist bezüglich ihrer Isotopenzusammensetzung zertifiziert. Der Bor-Gesamtgehalt ist als Richtwert angegeben. Die Unsicherheiten sind erweiterte Messunsicherheiten mit k=2. Sie sind in Klammern angegeben und beziehen sich auf die letzten beiden Stellen. Das vorliegende Isotopen-ZRM ist bezüglich der Isotopenzusammensetzung mit erweiterten relativen Messunsicherheiten kleiner 0,08% zertifiziert. Die absolute, kombinierte Standardmessunsicherheit des prozentualen Stoffmengenanteils der Isotope (Isotopenhäufigkeit) liegt bei 0,014. In diesem Zertifizierungsbericht wird nur auf die Kapitel eingegangen, die abweichend vom bestehenden Zertifizierungsreport für die Referenzmaterialien BAM I001 bis BAM I003 sind und Einfluss auf die Endergebnisse haben. Dabei handelt es sich um die Kapitel 3.3, 3.4, 4, 6, 7 und 8, Die Kapitel 1, 2, 3, 3.1, 3.2, 5, 9 und 10 des alten Zertifizierungsberichts für die Referenzmaterialien BAM I001 bis BAM I003 behalten unverändert ihre Gültigkeit und sind nicht noch einmal aufgeführt worden. KW - Isotope KW - Kernkraftwerk KW - Bor PY - 2009 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355786 SP - 1 EP - 9 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35578 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Ostermann, Markus T1 - On the measurement of the moisture content in different matrix materials JF - Accreditation and quality assurance N2 - Twelve different samples were analyzed for their water content by the classical oven-drying method and a commercial moisture analyzer. Nominal values have been set by Karl Fischer titration and gravimetry. The decomposition during the drying process of samples containing organic compounds was checked by thermogravimetry coupled with Fourier transform infrared spectrometric and mass spectrometric detection. Summarizing all measurement results, the commercial moisture analyzer demonstrated an average bias for the determination of water contents, which is much smaller than the stated uncertainty and thus is negligible. Compared to the classical oven-drying method, the commercial moisture analyzer shows a smaller bias, more ease in handling and less time consumption per analysis. When validated by a reference procedure like Karl Fischer titration the commercial moisture analyzer is the method of choice for routine analysis. KW - Classical oven-drying KW - Commercial moisture analyzer KW - Karl Fischer titration KW - Moisture KW - Reference materials KW - Thermogravimetry KW - Matrix samples PY - 2006 DO - https://doi.org/10.1007/s00769-006-0159-z SN - 0949-1775 SN - 1432-0517 VL - 11 IS - 7 SP - 356 EP - 362 PB - Springer CY - Berlin AN - OPUS4-12638 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Liesegang, D. A1 - Ostermann, Markus A1 - Diemer, J. A1 - Berglund, M. A1 - Quétel, C. A1 - Taylor, P. A1 - Heumann, K. T1 - Producing SI-traceable reference values for Cd, Cr and Pb amount contents in polyethylene samples from the Polymer Elemental Reference Material (PERM) project using isotope dilution mass spectrometry JF - Accreditation and quality assurance N2 - The present paper describes the certification of the amount content of Cd, Cr and Pb in two different polyethylene materials within the third phase of the Polyethylene Elemental Reference Material (PERM) project. The analytical procedure to establish the reference values for Cd, Cr and Pb amount contents in these materials is based on isotope dilution mass spectrometry used as a primary method of measurement. Cd and Pb were measured with inductively coupled plasma-mass spectrometry and Cr with positive thermal ionization-mass spectrometry. The decomposition of the polymer matrix was carried out using a high pressure asher. Reference values for amount content, traceable to the SI-system, have been obtained for these three elements in both of the polyethylene samples of PERM. For each of the certified amount content values an uncertainty budget was calculated using the method of propagation of uncertainties according to ISO and EURACHEM guidelines. The measurement procedures, as well as the uncertainty calculations, are described for all three elements. In order to keep the whole certification process as transparent as possible, the preparations of various reagents and materials as well as the sample treatment and blending are described in detail. The mass spectrometry measurements and the data treatment are also explained carefully. The various sources of uncertainty present in the procedure are displayed in the uncertainty budgets. The obtained combined uncertainties for the amount content values were less than 2% relative (k=1) for all investigated elements. The amount contents were in the ?mol/kg range, corresponding to mg/kg levels. KW - PERM KW - ICP-MS KW - PTI-MS KW - IDMS KW - Uncertainty budget KW - Certification KW - Polyethylene PY - 2000 DO - https://doi.org/10.1007/s007690000146 SN - 0949-1775 SN - 1432-0517 VL - 5 SP - 314 EP - 324 PB - Springer CY - Berlin AN - OPUS4-7217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taube, Mareike Carolin A1 - Adamczyk, Burkart A1 - Adam, Christian A1 - Feldmann, Ines A1 - Ostermann, Markus A1 - Reuter, M. A1 - Stelter, M. T1 - Tantalrecycling aus pyrometallurgischen Rückständen JF - World of Metallurgy – ERZMETALL N2 - Gegenstand dieser Arbeit ist die Untersuchung eines bestehenden pyrometallurgischen Prozesses zur Rückgewinnung von Tantal und Niob aus metallurgischen Reststoffen mit vorwiegend niedriger Wertstoffkonzentration. Zur näheren Erforschung der im vorliegenden Stoffsystem ablaufenden Reduktionsprozesse wurden in einem Elektrolichtbogenofen Schmelzversuche im Pilotmaßstab durchgeführt. Als Reduktionsmittel diente Koks, welcher mithilfe einer Argon-gespülten Eisenlanze in die flüssige mineralische Schmelze eingebracht wurde. Während der Reduktionsbehandlung werden Refraktärmetalle wie Tantal und Niob in ihre Carbide überführt und anschließend in der erschmolzenen eisenbasierten Metallphase am Boden des Reaktors angereichert. Neben Tantal und Niob gelangt auch ein Teil des im Einsatzmaterial enthaltenen Titans als unerwünschtes Begleitelement in die Metallphase. Sein Großteil verbleibt jedoch als Oxid in der Schlacke und wird dort hauptsächlich im Mineral Perowskit (CaTiO3) gebunden. Die erstarrten Schlackeproben wurden mit verschiedenen Methoden wie Röntgenfluoreszensanalyse, Röntgenbeugung und Rasterelektronenmikroskopie mit gekoppelter energiedispersiver Röntgenanalyse untersucht, um die Bildung tantalhaltiger Mineralphasen zu verschiedenen Stadien des Reduktionsprozesses zu verfolgen. Die hier gewonnenen Erkenntnisse zeigen, dass weniger die durch das Einblasen von Koks verursachte Reduktionsreaktion, sondern das Absinken der tantalreichen Eisentröpfchen in der flüssigen mineralischen Schmelze, gefolgt von ihrer Anreicherung in die Metallphase, für die Kinetik ausschlaggebend ist. N2 - An existing pyrometallurgical process for tantalum and niobium recovery, mainly from low grade pyrometallurgical residues, was investigated. Melting experiments were carried out in a pilot-scale electric arc furnace to study the material system during the reduction process caused by blowing coke into the liquid mineral melt. During the pyrometallurgical treatment refractory metals such as tantalum and niobium are converted into their carbides and enriched in the molten iron-based metal phase. Titanium is also enriched in the metal phase as an unwanted accompanying element, but most of it remains in oxidic form in the slag and is mainly bound in the mineral perovskite. Cooled down slag samples were analysed using XRF, XRD, SEM and EDX to investigate the formation of mineral phases rich in tantalum during various stages of the reduction process. The results show that the settling of the tantalum-rich iron droplets in the molten slag into the metal phase May play a greater role for the kinetics than the actual reduction reaction caused by blowing in coke. KW - Tantal KW - Recycling KW - Reduktionsprozess KW - Perowskit KW - Elektrolichtbogenofen PY - 2020 SN - 1613-2394 VL - 73 IS - 4 SP - 196 EP - 205 PB - GDMB Verlag GmbH CY - Clausthal-Zellerfeld AN - OPUS4-51064 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sowoidnich, K. A1 - Maiwald, M. A1 - Ostermann, Markus A1 - Sumpf, B. T1 - Shifted excitation Raman difference spectroscopy for soil component identification and soil carbonate determination in the presence of strong fluorescence interference JF - Journal of Raman spectroscopy N2 - Detailed knowledge about soil composition is an important prerequisite for many applications, for example precision agriculture. Current standard laboratory methods are complex and time-consuming but could be complemented by non-invasive optical techniques. Its capability to provide a molecular fingerprint of individual soil components makes Raman spectroscopy a very promising candidate. A major challenge is strong fluorescence interference inherent to soil, but this issue can be overcome effectively using shifted excitation Raman difference spectroscopy (SERDS). A customized dual-wavelength diode laser emitting at 785.2 and 784.6 nm was used to investigate 117 soil samples collected from an agricultural field along a distance of 624 m and down to depths of 1 m. To address soil spatial heterogeneity, a raster scan approach comprising 100 measurement spots per sample was applied. Based on the Raman spectroscopic fingerprint extracted from intense fluorescence interference by SERDS, 13 mineral soil constituents were identified, and even closely related molecular species could be discriminated, for example polymorphs of titanium dioxide and calcium carbonate. For the first time, the capability of SERDS is demonstrated to predict the calcium carbonate content as an important soil parameter using partial least squares regression (R2 = 0.94, root mean square error of cross-validation RMSECV = 2.1%). Our findings demonstrate that SERDS can extract a wealth of spectroscopic information from disturbing backgrounds enabling qualitative and quantitative soil analysis. This highlights the large potential of SERDS for precision agriculture but also in further application areas, for example geology, cultural heritage and planetary exploration. KW - Calcium carbonate KW - Raman spectroscopy KW - Soil KW - X-Ray fluorescence KW - SERDS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569016 DO - https://doi.org/10.1002/jrs.6500 SN - 0377-0486 IS - Special Issue SP - 1 EP - 14 PB - John Wiley & Sons Ltd. CY - Hoboken, New Jersey, USA AN - OPUS4-56901 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 JF - Journal of analytical atomic spectrometry 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 DO - 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 - Sichler, Theresa Constanze A1 - Adam, Christian A1 - Becker, Roland A1 - Sauer, Andreas A1 - Ostermann, Markus A1 - Barjenbruch, M. T1 - Phosphorus determination in sewage sludge: comparison of different aqua regia digestion methods and ICP-OES, ICP-MS and photometric determination JF - Environmental Sciences Europe N2 - Phosphorus recycling from sewage sludge will be obligatory in Germany from 2029. Phosphorus content determination in sewage sludge is crucial to assess the prescribed recycling rates. Currently, German law regards sample preparation using aqua regia digestion in a microwave or under reflux conditions as well as instrumental phosphorus determination by ICP-OES, ICP-MS, or photometric determination with ammonium molybdate as equivalent. However, it is questionable whether these methods are indeed equivalent regarding phosphorus quantification in sludges near the limit of 20 g/kg for mandatory recycling. To answer this question, 15 sewage sludges of 11 different wastewater treatment plants were investigated with all permitted method (digestion and measurement) combinations. Moreover, one sewage sludge was also examined in an interlaboratory comparison (ILC) with 28 participants. This study shows that the above-mentioned methods differ in some cases significantly but across all method combinations and sludges, phosphorus recovery was between 80 and 121% after normalization to the grand mean (average of 15 sludges between 85 and 111%). The ILC and the examination of 15 sludges produced largely similar results. There is a tendency to higher phosphorus recovery after microwave digestion compared to reflux digestion and ICP-OES measurements determine higher phosphorus contents than ICP-MS and photometric phosphorus determination. As a result, the authors recommend ICP-OES determination of phosphorus in sewage sludge after microwave digestion. KW - Sewage sludge KW - ICP-OES KW - Phosphous recovery KW - ICP-MS KW - Photometric P determination KW - Interlaboratory comparison PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558869 DO - https://doi.org/10.1186/s12302-022-00677-1 VL - 34 IS - 99 SP - 1 EP - 14 PB - Springer AN - OPUS4-55886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen A1 - Büchele, Dominique A1 - Schmid, Thomas A1 - Ostermann, Markus T1 - Development of an online-analysis technique for the determination of plant essential nutrients in soils using XRF and LIBS T2 - Prozessanalytik in der Pharma- und Lebensmitteltechnologie N2 - Currently, there is almost no comprehensive mapping of agricultural cropland because of the lack of fast and affordable mapping methods for important soil properties. Arable land of some hectares in size show a broad range of different nutrient compositions. Because of this heterogeneity wrong fertilization can occur and can cause environmental pollution or lead to smaller harvests and this is simply a waste of resources. The goal of I4S (intelligence for soil) is to develop an integrated system for site-specific soil fertility management. The I4S consortium consists of 10 different institutions, which are testing various sensors for their suitability for the requested applications. Besides the preparation of reference materials, the main task of the Federal Institute for Materials Research and Testing (BAM) in this project is the method development for online-XRF (x-ray fluorescence spectroscopy) and for online-LIBS (laser-induced breakdown spectroscopy) sensor systems. Both methods have the advantage that there is no or only little sample preparation necessary. Each method provides a fast and simultaneous multi-element analysis. Both measurement setups can be utilized for a mobile application which is fundamental for reaching the goals of I4S. Having finally a set of some reference materials, further work will focus on the online-XRF and online-LIBS methods in order to obtain useable calibration models. The calibration models will then be tested using stationary and moving samples. T2 - 12. Kolloquium Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - RFA KW - LIBS KW - Soil KW - Agricultural KW - Online KW - Sensor system PY - 2016 SP - P12, 63 EP - 65 AN - OPUS4-38377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rühlmann, Madlen A1 - Büchele, Dominique A1 - Ostermann, Markus A1 - Bald, Ilko A1 - Schmid, Thomas T1 - Challenges in the quantification of nutrients in soils using laser-induced breakdown spectroscopy – A case study with calcium JF - Spectrochimica Acta Part B N2 - The quantification of the elemental content in soils with laser-induced breakdown spectroscopy (LIBS) is challenging because of matrix effects strongly influencing the plasma formation and LIBS signal. Furthermore, soil heterogeneity at the micrometre scale can affect the accuracy of analytical results. In this paper, the impact of univariate and multivariate data evaluation approaches on the quantification of nutrients in soil is discussed. Exemplarily, results for calcium are shown, which reflect trends also observed for other elements like magnesium, silicon and iron. For the calibration models, 16 certified reference soils were used. With univariate and multivariate approaches, the calcium mass fractions in 60 soils from different testing grounds in Germany were calculated. The latter approach consisted of a principal component analysis (PCA) of adequately pre-treated data for classification and identification of outliers, followed by partial least squares regression (PLSR) for quantification. For validation, the soils were also characterised with inductively coupled plasma optical emission spectroscopy (ICP OES) and X-ray fluorescence (XRF) analysis. Deviations between the LIBS quantification results and the reference analytical results are discussed. KW - Laser-induced breakdown spectroscopy (LIBS) KW - Soil KW - Multivariate data analysis KW - Principal component analysis (PCA) KW - Partial least squares regression (PLSR) PY - 2018 DO - https://doi.org/10.1016/j.sab.2018.05.003 VL - 146 SP - 115 EP - 121 PB - Elsevier B.V. AN - OPUS4-45070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -