TY - JOUR A1 - Ostermann, Markus A1 - Berglund, M. A1 - Taylor, P. D. P. T1 - Measurement of the content of sulfur in gas oils using a high pressure asher, isotope dilution and thermal ionization mass spectrometry JF - Journal of analytical atomic spectrometry N2 - A new method has been developed for the measurement of sulfur in gas oils using a high pressure asher (HPA) for sample digestion. This, combined with a calibrated enriched isotopic reference material, and high precision mass spectrometry, makes it a powerful tool for an accurate and precise determination of the sulfur content in fossil fuels. The method described here was one of the methods used in the certification of the candidate reference materials BCR-104R, BCR-671 and BCR-672. Approximately 0.2 g of the gas oil samples were spiked with the spike isotopic reference material IRMM-646, which is enriched in 34S, and combusted in an HPA using nitric acid. The isotopes of sulfur were measured as arsenic monosulfides (AsS+) using a thermal ionization mass spectrometer equipped with a Faraday detector. The total uncertainty of the sulfur content (k = 2) is about 1%. The certified reference materials NIST SRM-2724b and NIST SRM-1619b and BCR-105 were used as part of the method validation work. The mass content of sulfur in BCR-104R was measured to be 1014 µg g-1, BCR-671 has 450 µg g-1 sulfur and BCR-672 shows a sulfur mass content of 201 µg g-1. The sulfur content of the candidate reference materials is homogeneous for the sample size used. KW - TIMS KW - Gas-oil KW - Reference materials KW - Isotope dilution KW - Sulfur PY - 2002 DO - https://doi.org/10.1039/B111140J SN - 0267-9477 SN - 1364-5544 VL - 17 IS - 10 SP - 1368 EP - 1372 PB - Royal Society of Chemistry CY - London AN - OPUS4-1214 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ostermann, Markus A1 - Kettisch, P. A1 - Becker, Dorit A1 - Vogl, Jochen T1 - Measurements of sulfur in oil using pressurised wet digestion technique in open vessels and isotope dilution mass spectrometry JF - Analytical and bioanalytical chemistry KW - Wet digestion KW - Open vessel digestion KW - Sulfur in oil KW - Reference materials KW - TIMS KW - IDMS PY - 2003 UR - http://www.springerlink.com/content/b7alk8lgly2v/?p=6237db8a9c28481d87e7b017e6474b73&pi=88 SN - 1618-2642 SN - 1618-2650 VL - 377 IS - 4 SP - 779 EP - 783 PB - Springer CY - Berlin AN - OPUS4-2738 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hearn, R. A1 - Berglund, M. A1 - Ostermann, Markus A1 - Pusticek, N. A1 - Taylor, P.D.P. T1 - A comparison of high accuracy isotope dilution techniques for the measurement of low level sulfur in gas oils JF - Analytica chimica acta N2 - A comparison of high accuracy methods for the analysis of total sulfur in gas oils by three metrology institutes is described. The work contains a comparison of three different aspects of the analysis: sample digestion, instrumental measurement and isotope dilution strategies. Thermal ionisation mass spectrometry (TIMS) in combination with high pressure asher (HPA) or Carius tube digestion has traditionally been used for such high accuracy analysis. However, this paper demonstrates that the faster, less laborious technique of ICP-MS in combination with microwave digestion is equally capable. Results from the comparison experiments show excellent agreement for fuel samples containing sulfur concentrations in the range 11–200 µg g-1. This excellent agreement across the different sample preparation, measurement and isotope dilution techniques has been exploited in the certification of two new diesel fuel reference materials. KW - Sulfur KW - Gas oil KW - Isotope dilution KW - ICP-MS KW - TIMS KW - Uncertainty PY - 2005 DO - https://doi.org/10.1016/j.aca.2004.10.070 SN - 0003-2670 SN - 1873-4324 SN - 0378-4304 VL - 532 IS - 1 SP - 55 EP - 60 PB - Elsevier CY - Amsterdam AN - OPUS4-7280 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ostermann, Markus A1 - Kühn, Andreas A1 - Bjeoumikhov, A. A1 - Wedell, R. T1 - Einsatz der Röntgenfluoreszenzanalyse in der Prozessanalytik JF - Technisches Messen N2 - Elementanalyse mit Röntgenfluoreszenzspektrometrie direkt am Materialstrom in Produktionsprozessen gewinnt zunehmend an Bedeutung. Die Röntgenfluoreszenzspektrometrie kann aufgrund der technischen Entwicklung mittlerweile ohne aufwändige Probenvorbereitung als aussagekräftige Informationsquelle für Stoffparameter im industriellen Prozess eingesetzt werden. Der Einsatz von online Röntgenfluoreszenzanalyse zahlt sich sowohl finanziell als auch zeitlich schnell aus, da sie sowohl für den ökonomischen Einsatz von Rohmaterialien, als auch z. B. im Materialrecycling zu gebrauchen ist. In diesem Beitrag werden vier unterschiedliche Einsatzmöglichkeiten beschrieben. N2 - Elemental analysis directly at the material stream of production processes using X-ray fluorescence spectrometry is gathering importance. Thanks to technical developments, X-ray fluorescence analysis can be used as information source in the elemental analysis of material in industrial processes without tedious sample preparation steps. The employment of online X-ray fluorescence analysis pays off both in financial as well in time aspects, since it can be used for the economic application of raw materials or e. g. for recycling. This paper describes four different applications of X-ray fluorescence spectroscopy. KW - Röntgenfluoreszenzspektrometrie KW - Stoffparameter KW - Materialanalyse KW - X-ray fluorescence spectrometry KW - Elemental analysis KW - Material analysis PY - 2011 DO - https://doi.org/10.1524/teme.2011.0162 SN - 0340-837X SN - 0178-2312 SN - 0171-8096 VL - 78 IS - 12 SP - 559 EP - 568 PB - Oldenbourg CY - München AN - OPUS4-24973 LA - deu 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 - Horf, M. A1 - Gebbers, R. A1 - Vogel, S. A1 - Ostermann, Markus A1 - Piepel, M.-F. A1 - Olfs, H.-W. T1 - Determination of Nutrients in Liquid Manures and Biogas Digestates by Portable Energy-Dispersive X-ray Fluorescence Spectrometry JF - Sensors N2 - Knowing the exact nutrient composition of organic fertilizers is a prerequisite for their appropriate application to improve yield and to avoid environmental pollution by over-fertilization. Traditional standard chemical analysis is cost and time-consuming and thus it is unsuitable for a rapid analysis before manure application. As a possible alternative, a handheld X-ray fluorescence (XRF) spectrometer was tested to enable a fast, simultaneous, and on-site analysis of several elements. A set of 62 liquid pig and cattle manures as well as biogas digestates were collected, intensively homogenized and analysed for the macro plant nutrients phosphorus, potassium, magnesium, calcium, and sulphur as well as the micro nutrients manganese, iron, copper, and zinc using the standard lab procedure. The effect of four different sample preparation steps (original, dried, filtered, and dried filter residues) on XRF measurement accuracy was examined. Therefore, XRF results were correlated with values of the reference analysis. The best R2 s for each element ranged from 0.64 to 0.92. Comparing the four preparation steps, XRF results for dried samples showed good correlations (0.64 and 0.86) for all elements. XRF measurements using dried filter residues showed also good correlations with R2 s between 0.65 and 0.91 except for P, Mg, and Ca. In contrast, correlation Analysis for liquid samples (original and filtered) resulted in lower R2 s from 0.02 to 0.68, except for K (0.83 and 0.87, respectively). Based on these results, it can be concluded that handheld XRF is a promising measuring system for element analysis in manures and digestates. KW - XRF KW - Animal slurry KW - Fertilizer KW - Soil KW - Precision farming PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527622 DO - https://doi.org/10.3390/s21113892 VL - 21 IS - 11 SP - 3892 PB - MDPI CY - Basel, Switzerland AN - OPUS4-52762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ostermann, Markus A1 - Herzel, Hannes A1 - Kühn, A. A1 - Mory, D. A1 - Wedell, R. T1 - Prozessanalytik mit Online-RFA und Online-LIBS für die Regelung der Aufarbeitung von Klärschlammaschen T1 - Online Process Analytics with XRF and LIBS for the Control of the Recycling of Sewage Sludge Ashes JF - Chemie Ingenieur Technik N2 - Es wurde ein Online-Analysenverfahren zur Bestimmung von Elementgehalten in Klär-schlammaschen und deren Produkten aus einem thermochemischen Verfahren entwickelt. Durch das thermochemische Verfahren können Wertstoffe aus den Aschen wieder für die Kreislaufwirtschaft nutzbar gemacht und Schadstoffe sicher entfernt werden. Das Analysensystem ist eine Methodenkombination von Online-Laser induzierter Plasma Spektroskopie (LIBS) und Online-Röntgenfluoreszenzanalyse (RFA). Robustheit und modulare Bauweise des Verfahrens sind wichtige Anforderungen um auch für andere Anwendungen nutzbar zu sein. N2 - An online analysis method has been developed for the determination of element mass fractions in sewage sludge ashes and their products originating from a thermochemical process. Within this process resources from the sewage sludge ashes can be re-utilized for the recycling economy and pollutants can be removed. The applied analysis system is a method combination of Online-laser induced breakdown spectroscopy (LIBS) and online- X-ray fluorescence (XRF). Robustness and a modular construction are important demands for successful future applications. KW - Klärschlammasche KW - Phosphor KW - Prozessanalytik KW - Röntgenfluoreszenzanalyse KW - LIBS PY - 2016 DO - https://doi.org/10.1002/cite.201500186 SN - 1522-2640 VL - 88 IS - 6 SP - 786 EP - 792 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim, Germany AN - OPUS4-36334 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Görner, Wolf A1 - Haase, Oskar A1 - Ostermann, Markus A1 - Segebade, Christian T1 - Instrumental analysis of phosphorus in organic material using high energy beta-counting after photoactivation (IPAA) JF - Journal of radioanalytical and nuclear chemistry N2 - C, N, O, F and P can be analyzed by instrumental photon activation analysis (IPAA) including decay curve analysis. The interference of 30P (T1/2 = 149.9 s) by 15O (T1/2 = 122.2 s) can be ruled out by direct positron measurement making use of the largely different maximum β+-energies of both nuclides (3.24 MeV and 1.73 MeV, respectively). Interference by carbon (11C) can be avoided by sub-threshold activation with 17 MeV bremsstrahlung. The short half-life of 30P allows a high productivity of the method. Reliability was demonstrated in the range of 0.2%–2% P (detection limit = 40 µg/g). Analysis of a certified reference material (BCR-CRM 063) yielded excellent agreement with the certified data. KW - Instrumental analysis KW - Phosphorus KW - Photon activation PY - 2008 DO - https://doi.org/10.1007/s10967-007-0441-5 SN - 0236-5731 SN - 1588-2780 SN - 1417-2097 VL - 276 IS - 1 SP - 251 EP - 255 PB - Elsevier Sequoia CY - Lausanne AN - OPUS4-19157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ostermann, Markus A1 - Berger, Achim A1 - Mans, C. A1 - Simons, C. A1 - Hanning, S. A1 - Janßen, A. A1 - Kreyenschmidt, M. T1 - Results and effects of homogeneity and stability studies carried out by X-ray fluorescence on the new reference material BAM-H010 JF - Accreditation and quality assurance N2 - The Federal Institute for materials research and testing (BAM)in cooperation with the Fachhochschule Münster has developed a new certified polymeric reference material, BAM-H010. The reference material consists of acrylonitrile–butadiene–styrene terpolymer (ABS) and has been doped with different contents of the elements Br, Cd, Cr, Hg and Pb. The monitoring of these elements is demanded in the EU directive 2002/95/EG, commonly referred to as RoHS. We have shown that the uncertainty contribution of the thermal long-term stability (ustability) is negligible compared to the contribution to the uncertainty caused by the method used for the characterization of the elemental content and the batch inhomogeneity (uhomogeneity). The stability of theABS material during exposure of the samples with hard X-radiation leads to a degradation of the ABS matrix with either long- or short-chain products. KW - Reference material KW - Plastic KW - RoHS KW - WEEE KW - X-ray fluorescence PY - 2011 DO - https://doi.org/10.1007/s00769-011-0806-x SN - 0949-1775 SN - 1432-0517 VL - 16 IS - 10 SP - 515 EP - 522 PB - Springer CY - Berlin AN - OPUS4-24249 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 -