TY - JOUR A1 - Steinhäuser, Lorin A1 - Piechotta, Christian A1 - Westphalen, Tanja A1 - Kaminski, Katja T1 - Evaluation, comparison and combination of molecularly imprinted polymer solid phase extraction and classical solid phase extraction for the preconcentration of endocrine disrupting chemicals from representative whole water samples N2 - Estrogens are endocrine disrupting chemicals and of high concerns due to demonstrated harmful effects on the environment and low effect levels. For monitoring and risk assessment, several estrogens were included in the "watch list" of the EU Water Framework Directive which sets very low environmental quality standard (EQS) levels for Estrone (E1) and 17β-Estradiol (E2) of 0.4 ng L−1 and for 17α-Ethinylestradiol (EE2) of 0.035 ng L−1 requiring sensitive detection methods, as well as extensive sample preparation. A sensitive, derivatization-free, isotope dilution calibration HPLC-MS/MS method for a panel of 5 selected estrogens (including the 3 estrogens of the EU WFD watchlist), and a procedure for the reproducible preparation of a representative whole water matrix including mineral water, humic acids and solid particulate matter are presented. These are used in a diligent comparison of classical solid phase extraction (SPE) on hydrophilic-lipophilic balanced (HLB) phase to SPE on an estrogen-specific molecularly imprinted polymer phase (MISPE) for ultra-trace levels of the analytes (1–10 ng L−1). Additionally, a two-step procedure combining HLB SPE disks followed by MISPE is evaluated. The tow-step procedure provides superior enrichment, matrix removal and sample throughput while maintaining comparable recovery rates to simple cartridge SPE. Estimated method quantification limits (MQLs) range from 0.109–0.184 ng L−1 and thus meet EQS-levels for E1 and E2, but not EE2. The representative whole water matrix provides a reproducible comparison of sample preparation methods and lays the foundation for a certified reference material for estrogen analysis. The presented method will serve as the basis for an extended validation study to assess its use for estrogen monitoring in the environment. KW - Estrogens KW - Whole water samples KW - Molecular imprinted polymers KW - EU-WFD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563547 DO - https://doi.org/10.1016/j.talo.2022.100163 SN - 2666-8319 VL - 6 SP - 1 EP - 5 PB - Elsevier B.V. CY - Amsterdam, Niederlande AN - OPUS4-56354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - Meermann, Björn T1 - Schnelle und einfache Extraktion von PFAS aus Bodenproben: Optimierte EOF-Bestimmung mittels HR-CS-GFMAS N2 - Per- und polyfluorierte Alkylsubstanzen (PFAS) bilden eine sehr komplexe Schadstoffgruppe mit über 6300 Einzelsubstanzen, die in vielfältiger Form in die Umwelt eingetragen werden. Für ein effektives Monitoring dieser Schadstoffklasse benötigt es ein Zusammenspiel aus Summenparameter-Analytik zur hot-spot-Identifizierung und Klassifizierung von Belastungssituationen sowie einer nachgeschalteten target-Analytik zur Identifizierung von Eintragswegen, die zugleich ein tieferes Verständnis von Transformationsprozessen ermöglicht. In diesem Beitrag präsentieren wir eine optimierte Extraktions-Methode für die PFAS-Summenparameteranalytik. Mit Hilfe dieser können bisher verwendete zeit- und kostenintensive Festphasenextraktionen (SPE) umgangen und PFAS-Extraktionseffizienzen gesteigert werden. Die methodische Bestimmungsgrenze (LOQ) war mit 10,30 μg/kg (Fluor pro Bodenprobe) ausreichend für alle 9 untersuchten Realbodenproben. KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - PFAS KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction KW - Böden PY - 2022 UR - https://www.gdch.de/fileadmin/downloads/Netzwerk_und_Strukturen/Fachgruppen/Umweltchemie_Oekotoxikologie/mblatt/2022/Heft122.pdf SN - 1618-3258 VL - 28 IS - 1 SP - 12 EP - 15 PB - Gesellschaft Deutscher Chemiker AN - OPUS4-54417 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian T1 - Analytische Chemie Gusseisen, Gummi, Bodenproben N2 - Die BAM stellt seit über 100 Jahren Referenzmaterialien (RM) her. Seit damals haben sich die Anforderungen an RM stark verändert. Der Artikel gibt einen Einblick in Anforderungen und die Herstellungsweise von Referenzmaterialien. KW - Referenzmaterialien KW - ISO-Guide 35 KW - Boden PY - 2021 SP - 51 EP - 53 AN - OPUS4-53695 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - Meermann, Björn T1 - PFAS-Summenparameteranalytik - Neue analytische Methoden zum Nachweis von per- und polyfluorierten Verbindungen in der Umwelt N2 - Per- und polyfluorierte Alkylverbindungen (PFAS) sind sehr persistent und reichern sich in der Umwelt und im menschlichen Organismus in immer höheren Konzentrationen an. PFAS stellen deshalb eine große Gefährdung für Mensch und Umwelt dar. Eingesetzt werden sie u. a. als wasser- und fettabweisende Beschichtung in z. B. der Papier- und Textilindustrie und gelangen so während Produktion, Gebrauch und Entsorgung u. a. in den Wasserkreislauf. PFAS konnten sogar in der arktischen Umwelt in relevanten Konzentrationen detektiert werden und zählen somit zu den „emerging pollutants“. Ein prominenter Vertreter der PFAS stellt Perfluoroctansulfonsäure (PFOS) dar - die jedoch bereits im Anhang des Stockholmer Abkommen gelistet wurde und deren Einsatz somit stark eingeschränkt bzw. verboten ist. Im Hinblick auf die Vielzahl von Verbindungen werden neue analytische Methoden benötigt, die eine PFAS-Belastungssituation möglichst umfassend und nachweisstark widerspiegeln, um zukünftig mögliche Grenzwerte ableiten zu können. KW - PFAS KW - HR-CS-GFMAS KW - CIC KW - Fluor KW - Oberflächenwasser PY - 2021 UR - https://analyticalscience.wiley.com/do/10.1002/was.00080223 SN - 0016-3538 VL - 2021 IS - März SP - was.00080223, 2 EP - 4 PB - Wiley-VCH CY - Weinheim AN - OPUS4-52261 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meermann, Björn A1 - Lisec, Jan A1 - Jaeger, Carsten A1 - Saatz, Jessica A1 - Traub, Heike A1 - von der Au, Marcus T1 - Mehr Analyten, kleinere Proben N2 - Molekülmassenspektrometrie entwickelt sich weg von klassischer Target- hin zu Nontarget-Analytik. Elementmassenspektrometrie liefert hohe Ortsauflösung beim Element-Imaging und analysiert einzelne Zellen. Aufgrund der Fortschritte bei den Geräten für Timeof-Flight-Massenspektrometrie mit induktiv gekoppeltem Plasma (ICPToF-MS) lässt sich das gesamte Periodensystem der Elemente in kurzen transienten Signalen quasi-simultan massenspektrometrisch erfassen. KW - Massenspektrometrie KW - Non-target KW - ICP-ToF-MS KW - Laser Ablation/Imaging PY - 2021 VL - 69 IS - Juni SP - 64 EP - 67 PB - Wiley-VCH AN - OPUS4-52800 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cruz-Alonso, M. A1 - Fernandez, B. A1 - Alvarez, L. A1 - Gonzalez-Iglesias, H. A1 - Traub, Heike A1 - Jakubowski, Norbert A1 - Pereiro, R. T1 - Bioimaging of metallothioneins in ocular tissue sections by laser ablation-ICP-MS using bioconjugated gold nanoclusters as specific tags N2 - An immunohistochemical method is described to visualize the distribution of metallothioneins 1/2 (MT 1/2) and metallothionein 3 (MT 3) in human ocular tissue. It is making use of (a) antibodies conjugated to gold nanoclusters (AuNCs) acting as labels, and (b) laser ablation (LA) coupled to inductively coupled plasma – mass spectrometry (ICP-MS). Water-soluble fluorescent AuNCs (with an average size of 2.7 nm) were synthesized and then conjugated to antibody by carbodiimide coupling. The surface of the modified AuNCs was then blocked with hydroxylamine to avoid nonspecific interactions with biological tissue. Immunoassays for MT 1/2 and MT 3 in ocular tissue sections (5 μm thick) from two post mortem human donors were performed. Imaging studies were then performed by fluorescence using confocal microscopy, and LA-ICP-MS was performed in the retina to measure the signal for gold. Signal amplification by the >500 gold atoms in each nanocluster allowed the antigens (MT 1/2 and MT 3) to be imaged by LA-ICP-MS using a laser spot size as small as 4 μm. The image patterns found in retina are in good agreement with those obtained by conventional fluorescence immunohistochemistry which was used as an established reference method. KW - Nanocluster KW - Immunohistochemistry KW - Laser ablation KW - ICP-MS KW - Fluorescence KW - Bioimaging PY - 2018 DO - https://doi.org/10.1007/s00604-017-2597-1 SN - 1436-5073 SN - 0026-3672 VL - 185 IS - 1 SP - 64 EP - 72 PB - Springer CY - Vienna AN - OPUS4-44637 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Noureen, N. A1 - Shah, F. A. A1 - Lisec, Jan A1 - Usman, H. A1 - Khalid, M. A1 - Munir, R. A1 - Zaidi, N. T1 - Revisiting the Association between Human Leukocyte Antigen and End-Stage Renal Disease N2 - Multiple works have studied possible associations between human leukocyte antigen (HLA) alleles and end stage renal disease (ESRD). However, there are several contradictions in these previous works and no consistent HLA associations with ESRD itself have been identified. Most of these works have several limitations, for instance, the population size was too small, or only limited HLA loci were studied. The presented work aims to revisit the association between ESRD and HLA antigens while taking in to account the previously overlooked limitations. Here, we compared the HLA polymorphism (at HLA-A, -B, -C, -DRB1, -DQB1 and DQA1 loci) in ESRD patients (n=497) and controls (n=672). Our data identified several HLA alleles that displayed a significant positive or negative association with ESRD. We also determined whether heterozygosity or homozygosity of the ESRD-associated HLA alleles at different loci could modify the prevalence of the disease. Few HLA allele combinations displayed significant associations with ESRD among which HLA-A*3 –HLA-A*26 combination showed the highest strength of association (OR= 4.488, P≤ 0.05) with ESRD. However, the age of ESRD onset was not affected by HLA allele combinations at different loci. Most of the previous works have studied the association of HLA with ESRD in homogeneous ethnic groups and have interpreted their data accordingly. Here, we also performed an extensive literature analysis to determine whether the association of HLA to ESRD can be similar across different ethnic groups. This analysis showed that at least for certain alleles, the association of HLA to ESRD can be similar in different ethnic groups. For instance, HLA-A*11, HLA-DRB1*11, and HLA-DRB1*4 all showed significant positive associations with ESRD in different ethnic groups. The findings of our study will help in determining possible protective or susceptible roles of various HLA alleles in ESRD. KW - Mass-Spectrometry KW - HLA KW - Renal disease PY - 2020 DO - https://doi.org/10.1101/2020.03.18.996330 SP - 1 EP - 23 AN - OPUS4-50720 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittmann, Daniel A1 - Lucke, T. A1 - Ruhl, A. S. A1 - Winzenbacher, R. A1 - Jekel, M. A1 - Braun, Ulrike T1 - Untersuchungen zu biologischen, organischen und anorganischen Veränderungen granulierter Aktivkohlen während der Trinkwasseraufbereitung N2 - Untersuchungen zu biologischen, organischen und anorganischen Veränderungen granulierter Aktivkohlen während der Trinkwasseraufbereitung des Landeswasserversorgers Langenau. KW - Thermogravimetrie KW - Trinkwasser KW - Wasseraufbereitung KW - Aktivkohle PY - 2020 SN - 0083-6915 VL - 118 IS - 2 SP - 47 EP - 50 PB - Wiley-VCH Verlag GmbH & Co. KGaA AN - OPUS4-51434 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Silke A1 - Roethke, A. A1 - Rienitz, O. A1 - Matschat, Ralf A1 - Schiel, D. A1 - Jaehrling, R. A1 - Goerlitz, V. A1 - Kipphardt, Heinrich T1 - SI-traceable monoelemental solutions on the highest level of accuracy: 25 years from the foundation of CCQM to recent advances in the development of measurement methods N2 - Within the Working Group on Inorganic Analysis (IAWG) of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM) international key comparisons and pilot studies related to inorganic analysis are carried to ensure consistency in this field at the highest level. Some of these comparisons deal directly with the preparation and characterization of monoelemental solutions or with topics, closely related. The importance of monoelemental solutions lies in the fact that almost every measurement in inorganic analysis relies on the comparison with either a reference material, or references in form of solutions, usually (mono)elemental solutions. All quantitative measurement approaches, e.g. isotope dilution or standard addition, need an accurate reference solution made from a well characterized reference material, prepared under full gravimetric control. These primary (monoelemental) solutions do not only serve as arbitrary references/calibration solutions, but they also link up measurement results to the International System of units (SI), this way establishing the so-called metrological traceability to a measurement unit of the SI. Without such solutions on the highest possible level of accuracy and with the smallest possible associated uncertainties (for e.g. element content and/or impurities), an analysis itself can never be as good as it could be with appropriate reference solutions. This article highlights select key comparisons and pilot studies dealing with monoelemental solution related topics within the IAWG from the foundation of CCQM – 25 years ago – up to latest achievements in the field of inorganic analysis. KW - Metrology KW - SI Traceability KW - CCQM PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496080 DO - https://doi.org/10.1088/1681-7575/ab5636 SN - 0026-1394 SN - 1681-7575 SP - 1 EP - 23 PB - IOP CY - Bristol AN - OPUS4-49608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Von der Au, M. A1 - Borovinskaya, O. A1 - Büchel, C. A1 - Meermann, Björn T1 - Der Fingerabdruck der Kieselalge N2 - Elementanalytische Verfahren werden heute zu mehr eingesetzt als bloß zur Bestimmung von Metallgesamtgehalten in diversen Probenmatrizes. Sie stellen heute ein wichtiges Werkzeug zur Beantwortung lebenswissenschaftlicher Fragen aus Umwelt, Medizin und Biologie dar. In der vorliegenden Arbeit kommt die single-cell-ICP-Flugzeitmassenspektrometrie (single-cell-ICP-TOF-MS) zur Multielementanalytik in einzelnen Kieselalgen (Diatomeen) zum Einsatz und wird zukünftig ein wichtiges Werkzeug z.B. bei der Beantwortung ökotoxikologischer Fragestellung sein. KW - Diatomeenanalytik KW - Single cell-ICP-ToF-MS KW - Multielementanalytik in kurzen transienten Signalen PY - 2019 UR - https://q-more.chemie.de/q-more-artikel/299/der-fingerabdruck-der-kieselalge.html SP - 1 EP - 3 PB - LUMITOS AN - OPUS4-49749 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Von der Au, M. A1 - Meermann, Björn T1 - Screening von Organofluorverbindungen im Oberflächenwasser N2 - Organofluorverbindungen kommen in vielen Bereichen zum Einsatz und gelangen in die aquatische Umwelt. Die Belastungssituation der Gewässer ist bisher wenig untersucht – hier kommt die HR-CS GF MAS als leistungsstarkes Screeningtool zum Einsatz. KW - HR-CS-GFMAS KW - Extrahierbar organisch gebundenes Fluor (EOF) KW - Oberflächengewässer PY - 2019 UR - https://analytik.news/Fachartikel/Volltext/bam5.pdf SP - 1 EP - 3 PB - Dr. Beyer Internet-Beratung AN - OPUS4-49750 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meermann, Björn A1 - Faßbender, Sebastian T1 - Antifoulingmittel im Wasser N2 - Für das Biozid Zink-Pyrithion, das in Schiffsanstrichen weit verbreitet ist, fehlten bisher die analytischen Methoden, um den Komplex und seine Abbauprodukte in der Umwelt nachzuweisen. Kapillarelektrophorese, gekoppelt mit komplementärer Massenspektrometrie könnte dieses Problem lösen. KW - Antifouling-Biozide KW - Kapillarelektrophorese-Massenspektrometrie KW - Komplementäre Massenspektrometrie KW - Umwelt-Speziation PY - 2019 DO - https://doi.org/10.1002/nadc.20194088793 SN - 1439-9598 SN - 1868-0054 VL - 67 IS - 12 SP - 56 EP - 58 PB - Wiley-VCH CY - Weinheim AN - OPUS4-49789 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moldenhauer, Laura A1 - Helmerich, Rosemarie A1 - Köppe, E. A1 - Wittmann, H.-J. T1 - Experimental modeling approach for determining the moisture damping exponent of a bluetooth low energy signal in moist building material N2 - The presented development of a damping model is a research component of an experimental feasibility study about moisture in building materials measured with Bluetooth® Low Energy (BLE) signals. This study may be part of a structural health- and long-term monitoring aiming at early damage detection in the built infrastructure and is increasingly focusing on wireless sensor network technology. It is investigated, how the Received Signal Strength Indicator (RSSI) of a BLE signal, transmitted from the BLE-module embedded in building materials with changing moisture content is damped. The aim of the modelling is the derivation of a damping equation for the formal model to determine the moisture damping exponent to finding a correlation. T2 - 34th Danubia Adria Symposium on Advances in Experimental Mechanics CY - Trieste, Italy DA - 19.09.2017 KW - BLE Bluetooth low energy KW - Sensor network KW - RSSI Received Signal Strength Indicator KW - Structural Health Monitoring KW - Moisture measurements PY - 2018 DO - https://doi.org/10.1016/j.matpr.2018.08.124 SN - 2214-7853 VL - 5 IS - Issue 13, Part 2 SP - 26469 EP - 26792 PB - Elsevier Ltd. CY - Radarweg 29, 1043 NX Amsterdam, The Netherlands AN - OPUS4-47171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duewer, D. L. A1 - Sander, L. C. A1 - Wise, S. A. A1 - Philipp, Rosemarie A1 - Hein, Sebastian A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Chan, P. A1 - Lee, H. A1 - Tang, H. A1 - Tang, P. A1 - Yip, Y. A1 - Lu, T. A1 - Cheow, P. S. A1 - Teo, T. L. A1 - Sega, M. A1 - Rolle, F. A1 - Baek, S. A1 - Kim, B. A1 - Lee, S. A1 - Cabillic, J. A1 - Fallot, C. A1 - Hua, T. A1 - Dazhou, C. A1 - Changjun, Y. A1 - Chunxin, L. A1 - Hongmei, L. A1 - Lippa, K. A1 - Itoh, N. A1 - Quinn, L. A1 - Prevoo-Franzsen, D. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. A1 - Gündüz, S. A1 - Krylov, A. A1 - Mikheeva, A. A1 - Baldan, A. A1 - van der Hout, J. W. A1 - van der Veen, A. M. H. T1 - CCQM-K131 Low-polarity analytes in a multicomponent organic solution: Polycyclic aromatic hydrocarbons (PAHs) in acetonitrile N2 - Solutions of organic analytes of known mass fraction are typically used to calibrate the measurement processes used to determine these compounds in matrix samples. Appropriate value assignments and uncertainty calculations for calibration solutions are critical for accurate measurements. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2015 the Organic Analysis Working Group (OAWG) sponsored CCQM-K131 "Low-Polarity Analytes in a Multicomponent Organic Solution: Polycyclic Aromatic Hydrocarbons (PAHs) in Acetonitrile". Polycyclic aromatic hydrocarbons (PAHs) result from combustion sources and are ubiquitous in environmental samples. The PAH congeners, benz[a]anthracene (BaA), benzo[a]pyrene (BaP), and naphthalene (Nap) were selected as the target analytes for CCQM-K131. These targets span the volatility range of PAHs found in environmental samples and include potentially problematic chromatographic separations. Nineteen NMIs participated in CCQM-K131. The consensus summary mass fractions for the three PAHs are in the range of (5 to 25) μg/g with relative standard deviations of (2.5 to 3.5) %. Successful participation in CCQM-K131 demonstrates the following measurement capabilities in determining mass fraction of organic compounds of moderate to insignificant volatility, molar mass of 100 g/mol up to 500 g/mol, and polarity pKow < −2 in a multicomponent organic solution ranging in mass fraction from 100 ng/g to 100 μg/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, and (3) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Naphthalene (Nap) KW - Organic calibration solution KW - Polycyclic aromatic hydrocarbon (PAH) PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471442 DO - https://doi.org/10.1088/0026-1394/56/1A/08003 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1A SP - 08003, 1 EP - 102 PB - IOP Science AN - OPUS4-47144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Jaeger, C. A1 - Zaidi, Nousheen T1 - Cancer cell lipid class homeostasis is altered under nutrient-deprivation but stable under hypoxia N2 - Under oxygen/nutrient deprivation cancer cells modify the Balance between fatty acid (FA) synthesis and uptake, which alters the levels of individual triglyceride or phospholipid sub-species. These modifications may affect survival and drug-uptake in cancer cells. Here, we aimed to attain a more holistic overview of the lipidomic profiles of cancer cells under stress and assess the changes in Major lipid-classes. First, expressions of markers of FA synthesis/uptake in cancer cells were assessed and found to be differentially regulated under metabolic stress. Next, we performed a broad lipidomics assay, comprising 244 lipids from six major classes, which allowed us to investigate robust stress induced changes in median levels of different lipid classes -additionally stratified by fatty acid side chain saturation status. The lipidomic profiles of cancer cells were predominantly affected by nutrient-deprivation. Neutral lipid compositions were markedly modified under serum-deprivation and, strikingly, the cellular level of triglyceride subspecies decreased with increasing number of double bonds in their fatty acyl chains. In contrast, cancer cells maintained lipid class homeostasis under hypoxic stress. We conclude that although the levels of individual lipid moieties alter under hypoxia, the robust averages of broader lipid class remain unchanged. KW - Mass-Spectrometry KW - Tumor metabolism KW - Fatty acid metabolism KW - Lipidomic profile KW - Metabolic stress PY - 2018 DO - https://doi.org/10.1101/382457 SP - 1 EP - 25 PB - Cold Spring Harbor Laboratory CY - Cold Spring Harbor, NY AN - OPUS4-46814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tjaden, B. A1 - Baum, K. A1 - Marquardt, V. A1 - Simon, M. A1 - Trajkovic-Arsic, M. A1 - Kouril, T. A1 - Siebers, B. A1 - Lisec, Jan A1 - Siveke, J. T. A1 - Schulte, J. H. A1 - Benary, U. A1 - Remke, M. A1 - Wolf, J. A1 - Schramm, A. T1 - MYCN-induced metabolic rewiring creates novel therapeutic vulnerabilities in neuroblastoma N2 - MYCN is a transcription factor that is aberrantly expressed in many tumor types and is often correlated with poor patient prognosis. Recently, several lines of evidence pointed to the fact that oncogenic activation of MYC family proteins is concomitant with reprogramming of tumor cells to cope with an enhanced need for metabolites during cell growth. These adaptions are driven by the ability of MYC proteins to act as transcriptional amplifiers in a tissue-of-origin specific manner. Here, we describe the effects of MYCN overexpression on metabolic reprogramming in neuroblastoma cells. Ectopic expression of MYCN induced a glycolytic switch that was concomitant with enhanced sensitivity towards 2-deoxyglucose, an inhibitor of glycolysis. Moreover, global metabolic profiling revealed extensive alterations in the cellular metabolome resulting from overexpression of MYCN. Limited supply with either of the two main carbon sources, glucose or glutamine, resulted in distinct shifts in steady-state metabolite levels and significant changes in glutathione metabolism. Interestingly, interference with glutamine-glutamate conversion preferentially blocked proliferation of MYCN overexpressing cells, when glutamine levels were reduced. Thus, our study uncovered MYCN induction and nutrient levels as important metabolic master switches in neuroblastoma cells and identified critical nodes that restrict tumor cell proliferation. KW - Mass-spectrometry KW - Tumor metabolism KW - MYCN PY - 2018 DO - https://doi.org/10.1101/423756 SP - 1 EP - 21 PB - Cold Spring Harbor Laboratory CY - Cold Spring Harbor, NY AN - OPUS4-46815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keller, Julia A1 - Borzekowski, Antje A1 - Koch, Matthias T1 - Mykotoxine in Lebensmitteln - Zearalenon und seine Transformationsprodukte N2 - Mykotoxine in Lebensmitteln stellen weltweit Probleme dar, Zearalenon in Speiseöl ist ein solches. Neue Hydrazinbasierte Analyseverfahren können jetzt helfen, den EU-Grenzwert besser zu kontrollieren. Aber auch die Strukturaufklärung von Transformationsprodukten und verlässliche Kalibrierstandards sind aktuelle Herausforderungen. KW - Analyseverfahren KW - Hydrazin KW - Speiseöle KW - Transformationsprodukte PY - 2019 IS - 03 SP - 34 EP - 36 AN - OPUS4-47858 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Silke T1 - Plasmaspectrochemistry in material sciences N2 - Plasmas as atomization and ionization/excitation sources have been used for more than 50 years. The term plasma spectrochemistry was introduced in the 1980s and is nowadays a topic of annual reviews and different conferences such as the Winter Conference on Plasma Spectrochemistry (held in USA), the European Winter Conference on Plasma Spectrochemistry, and The Nordic conference on Plasma Spectrochemistry. The development of advanced materials is inherently connected with improvements in analytical chemistry, and often is the driving force for method development in plasma-based spectrometry. Besides the determination of physical characteristics such as tensile strength, density, and conductivity, the investigation of their chemical constituents down to the trace and ultra-trace levels becomes more and more important and, therefore, the demand of sensitive and precise analytical methods is growing. In some cases, the determination of the average content is a sufficient result, for instance for the characterisation of raw material or waste management. However, lately laterally resolved analysis, depth profiling of layered materials and characterization of high purity materials are of growing importance. The aim of this article is to give an introduction into plasma spectrometry and its application in materials science. A theoretical overview of the used plasma techniques and a review on applications with a special focus on direct solid sampling will be presented. KW - Material Science KW - Plasma KW - Plasmaspectrochemistry PY - 2019 DO - https://doi.org/10.1002/9780470027318.a9341.pub2 SP - 1 PB - John Wiley & Sons CY - Hoboken, New Jersey AN - OPUS4-47840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Noeller, Renate A1 - Feldmann, Ines A1 - Kasztovszky, Z. A1 - Szőkefalvi-Nagy, Z. A1 - Kovács, I. T1 - Characteristic Features of Lapis Lazuli from Different Provenances, Revised by µXRF, ESEM, PGAA and PIXE N2 - The objective of this study is to find out, to what extent the geochemical characteristics of lapis lazuli can be utilized in respect to its provenance. A wide range of variables is taken into consideration depending on the quantity of samples analysed from a specific geological region and the methods applied. In order to provide evidence, a multi-technique analytical approach using µXRF, ESEM, PGAA and PIXE is applied to samples from the most famous deposits of lapis lazuli. Special elements determined as fingerprints are compared in relation to the forming conditions obvious in textural features. The results and statistical output allow a differentiation that enables an optimized local classification of the blue stone. An absolute requirement for all geo-tracing performed on blue colored cultural objects of unknown provenance is awareness of the limits of analysis. The possible sources of lapis lazuli are tested by analysing the blue pigment used as paint on murals and ink on manuscripts from the Silk Road. KW - Provenance studies KW - Micro-XRF KW - Lapis lazuli KW - ESEM KW - PGAA KW - PIXE KW - Pigment analyses PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-480048 DO - https://doi.org/10.17265/2328-2193/2019.02.003 VL - 7 IS - 2 SP - 57 EP - 69 PB - David Publishing AN - OPUS4-48004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - El-Athman, Rukeia A1 - Bresch, Harald A1 - Muth, Thilo A1 - Rädler, Jörg A1 - Rühle, Bastian T1 - Datenmanagement im Nanomaterial-Labor: Einsatz von ELN-Software zur digitalen Transformation des Laboralltags N2 - Angesichts der zunehmenden Digitalisierung und dem Einsatz datenintensiver Methodiken in der Wissenschaft stehen Forschende vor der Herausforderung, stetig wachsende Datenmengen nachvollziehbar zu dokumentieren, langfristig zu speichern und für Dritte nachnutzbar zu machen. Um diesen Anforderungen gerecht zu werden, bietet sich die Nutzung von Software-Lösungen an, welche Forschungsdatenmanagement mit der digitalen Dokumentation von Laborinventar und Experimenten in elektronischen Laborbüchern (engl. electronic lab notebooks (ELN)) verknüpfen. KW - NanoPlattform KW - BAM Data Store KW - OpenBIS KW - Forschungsdatenmanagement KW - Research data management KW - Elektronisches Laborbuch KW - Electronic lab notebook (ELN) PY - 2023 UR - https://analyticalscience.wiley.com/content/article-do/datenmanagement-im-nanomaterial-labor SN - 0016-3538 IS - 9 SP - 24 EP - 26 PB - Wiley Analytical Science CY - Weinheim AN - OPUS4-59600 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - El-Athman, Rukeia A1 - Rädler, Jörg A1 - Löhmann, Oliver A1 - Ariza, Angela A1 - Muth, Thilo T1 - The BAM Data Store N2 - As a partner in several NFDI consortia, the Bundesanstalt für Materialforschung und -prüfung (BAM, German federal institute for materials science and testing) contributes to research data standardization efforts in various domains of materials science and engineering (MSE). To implement a central research data management (RDM) infrastructure that meets the requirements of MSE groups at BAM, we initiated the Data Store pilot project in 2021. The resulting infrastructure should enable researchers to digitally document research processes and store related data in a standardized and interoperable manner. As a software solution, we chose openBIS, an open-source framework that is increasingly being used for RDM in MSE communities. The pilot project was conducted for one year with five research groups across different organizational units and MSE disciplines. The main results are presented for the use case “nanoPlattform”. The group registered experimental steps and linked associated instruments and chemicals in the Data Store to ensure full traceability of data related to the synthesis of ~400 nanomaterials. The system also supported researchers in implementing RDM practices in their workflows, e.g., by automating data import and documentation and by integrating infrastructure for data analysis. Based on the promising results of the pilot phase, we will roll out the Data Store as the central RDM infrastructure of BAM starting in 2023. We further aim to develop openBIS plugins, metadata standards, and RDM workflows to contribute to the openBIS community and to foster RDM in MSE. T2 - 1st Conference on Research Data Infrastructure DA - 12.09.2023 KW - Research Data Infrastructure KW - Electronic Lab Notebook (ELN) KW - openBIS KW - Research Data Management PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596032 DO - https://doi.org/10.52825/CoRDI.v1i.229 VL - 1 SP - 1 EP - 5 AN - OPUS4-59603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Scharf, Holger A1 - Lkhagvasuren, B. A1 - Oyuntungalag, U. A1 - Rausch, J. T1 - Certified reference material for determination of total cyanide in soil [BAM-U116/CGL306] N2 - CRM (Certified Reference Material) BAM-U116/CGL306 “Cyanide in soil” was produced within a framework of cooperation between CGL (Central Geological Laboratory) of Mongolia and Federal Institute for Materials Research and Testing (BAM) of Germany in 2013-2017. The CRM BAM-U116/CGL306 represents a mixture of a sandy soil collected from a contaminated former gasworks area in the Berlin region (Germany) and an unpolluted sandy soil from Nalaikh region (Mongolia). The bulk candidate material for this reference material was prepared at CGL CRM Laboratory exclusively destined to the preparation of reference materials and equipped with modern technical equipment. Homogeneity, stability and shelf life were studied in full compliance with ISO Guide 35. The CRM was evaluated as sufficiently homogeneous. Statistical evaluation of certification analysis was software packages SoftCRM and ProLab Plus. Certified value of total cyanide of the CRM is 12.0 mg/kg and expanded uncertainty was assigned as 0.8 mg/kg. The intended purpose of this material is the verification of analytical results obtained for the mass fraction of total cyanide in soils and soil-like materials applying the standardized procedure ISO 11262:2011. As any reference material, it can also be used for routine performance checks (quality control charts) or validation studies. KW - CRM KW - Cyanide in soil KW - Total cyanide PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-469694 DO - https://doi.org/10.17265/2162-5263/2018.04.004 SP - 149 EP - 161 PB - David Publishing AN - OPUS4-46969 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jakubowski, N. A1 - Borrmann, S. A1 - Recknagel, Sebastian A1 - Roik, Janina A1 - Rickert, F. T1 - Comparison of peristaltic pumps used for sample introduction in Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) N2 - In this investigation, two conventional peristaltic pumps are compared with a new pump based on the “easy click” principle using a simultaneous ICP-AES instrument with standard operating conditions. It is found that the figures of merit achieved are quite comparable for all three pumps. Relative standard deviations (RSDs) range between 0.2% and 1.8%, and limits of detection as low as 0.1 μg/L have been achieved , demonstrating that the easy click principle of the new pump does not compromise the analytical figures of merit. KW - ICP-AES KW - Peristaltic pumps KW - ICP-MS PY - 2020 IS - 35 / S4 SP - 6 AN - OPUS4-52020 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael A1 - Klaer, R.-H. A1 - Wagner, A. T1 - 100 % Digital in der Prozessindustrie - Tutzing-Symposion Teil 3: Intelligente Nutzung von Daten und Bausteinen der Digitalisierung N2 - Digitalisierung und Industrie 4.0 verändern komplette Geschäftsmodelle, heben neue Effizienzpotenziale und stärken die Wettbewerbsfähigkeit. Auf dem 57. Tutzing-Symposion vom 15.–18.04.2018 wurde mit Vorträgen und Kreativworkshops erkundet, welche speziellen Anforderungen die Prozessindustrie hat, welche digitalen Innovationen bereits umgesetzt wurden und wo noch Handlungsbedarf besteht. Ein Workshop befasste sich mit den Themenfeldern Datenkonzepte, Datenanalyse, Big Data und künstliche Intelligenz. Es geht nicht um die Digitalisierung von heute. Im Angesicht der wachsenden Digitalisierung unserer Prozesse stellt sich die Frage, ob wir den Prozess wirklich gut kennen. Ob alle Verfahrensschritte detailliert hinterlegt wurden. Nur mit einem heuristischen Ansatz kann das vorhandene Wissen nicht digitalisiert werden. Sehr schnell werden die Mechanismen eines Massenmarktes mit denen einer Nische verwechselt. Nicht jeder Mechanismus, den wir von großen Suchmaschinen oder Einkaufsportalen kennen, gibt uns einen Hinweis auf Nutzen und Verfügbarkeit für die Prozess- oder pharmazeutische Industrie. Eine gute Analyse der Anforderungen in der Zukunft mit einem Abgleich der derzeitigen technischen Möglichkeiten ist Voraussetzung für eine Verbesserung der derzeitigen digitalen Umsetzung. Dabei ist es sinnvoll unkonventionelle Methoden einzusetzen. KW - Digitalisierung KW - Prozessindustrie KW - Tutzing-Symposion KW - Datenkonzepte KW - Datenanalyse KW - Big Data KW - Künstlicher Intelligenz PY - 2018 UR - https://www.chemanager-online.com/themen/produktion/100-digital-der-prozessindustrie SN - 1436-2597 VL - 21 IS - 9 SP - 6 EP - 9 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-45861 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Metrologie für fortschrittliche Wasserstoffspeicherlösungen – Das EU-Projekt MefHySto T1 - Metrology for advanced hydrogen storage solutions – The EU project MefHySto N2 - Das europäische Projekt MefHySto befasst sich mit dem Bedarf an großmaßstäblichen Energiespeichern, die für eine Umstellung der Energieversorgung auf erneuerbare Energien erforderlich sind. Eine solche Speicherung ist entscheidend, um Energie zu Spitzenzeiten zu liefern, wenn die erneuerbaren Energiequellen schwanken. Eine mögliche Lösung für die Energiespeicherung ist der großtechnische Einsatz von Wasserstoff. Die messtechnische Rückführbarkeit in der Energieinfrastruktur für die Wasserstoffspeicherung ist dann von entscheidender Bedeutung und eine bessere Kenntnis der chemischen und physikalischen Eigenschaften von Wasserstoff sowie rückführbare Messungen und validierte Techniken unverzichtbar. N2 - The European project MefHySto addresses the need of large-scale energy storage, which is required for a shift to renewable energy supply. Such storage is mandatory to supply energy at peak times when renewable sources fluctuate. A possible solution for energy storage is large-scale use of hydrogen. Metrological traceability in the energy infrastructure for hydrogen storage is then crucial and a better knowledge of the chemical and physical properties of hydrogen as well as traceable measurements and validated techniques are indispensable. KW - Wasserstoff KW - Wasserstoffspeicher KW - Infrastruktur KW - Metrologie KW - PEM-Wasserelektrolyse KW - Rückverstromung KW - Lastwechsel KW - Wasserstoff-Qualität PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556451 UR - https://gwf-gas.de/forschung-entwicklung/metrologie-fuer-fortschrittliche-wasserstoffspeicherloesungen-das-eu-projekt-mefhysto/ SN - 2366-9594 VL - 163 IS - 9 SP - 38 EP - 45 PB - Vulkan Verlag CY - Essen AN - OPUS4-55645 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - The internet of things in the lab and in process - The digital transformation challenges for the laboratory 4.0 T1 - Das Internet of Things in Labor und Prozess - Herausforderungen des digitalen Wandels für das Labor 4.0 N2 - It is a fact that much of the time spent on analytical laboratory instrumentation these days goes into system maintenance. Digital transformation could give us more time again for creativity and our actual laboratory work – if we shape it the right way. N2 - Fakt ist: Einen Großteil der Zeit, der an analytischen Laborgeräten verbracht wird, nimmt heute die Systempflege in Anspruch. Der digitale Wandel kann uns endlich wieder mehr Zeit für Kreativität und die eigentliche Laborarbeit geben – wenn wir ihn richtig gestalten. KW - Lab of the Future KW - Digitalisation KW - Automation KW - Data Analysis KW - Instrument Communication KW - Labor der Zukunft KW - Digitale Transformation KW - Automatisierung KW - Gerätekommunikation PY - 2020 IS - 4 SP - 1 EP - 3 PB - Lumitos AG CY - Darmstadt AN - OPUS4-50618 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - On the way to the cyber-physical lab T1 - Auf dem Weg zum cyber-physical Lab N2 - Laboratories tend to be central hubs for chemical, biotechnological, pharmaceutical or foodstuff production. They play a key role in research and development, chemical analysis, quality assurance, maintenance and process control. For process development and optimization, process analytical technology (PAT) has proven to be a powerful tool to improve our understanding of processes, increase productivity, reduce waste and costs and shorten processing times. N2 - Im Allgemeinen sind Laboratorien zentrale Drehscheiben für die chemische, biotechnologische, pharmazeutische oder Lebensmittelproduktion. Sie spielen eine Schlüsselrolle in Forschung und Entwicklung, chemischer Analytik, Qualitätssicherung, Instandhaltung und Prozesskontrolle. Für die Prozessentwicklung und -Optimierung hat sich die Prozessanalysentechnik (PAT) als leistungsfähiges Werkzeug erwiesen, um das Prozessverständnis zu verbessern, die Produktivität zu steigern, Abfall und Kosten zu reduzieren und die Prozesszeit zu verkürzen. KW - Lab of the Future KW - Digitalisation KW - Cyber-physical Lab KW - Smart Laboratoy PY - 2020 SP - 1 EP - 3 PB - Lumitos AG CY - Darmstadt AN - OPUS4-51036 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Klas T1 - Atomkerne zählen - Quantitative NMR-Spektroskopie als vielseitige Methode in Labor und Prozess N2 - Meist präsentieren sich Laboratorien für NMR-Spektroskopie auf den ersten Blick von außen nur wenig einladend. Es lohnt sich aber einen Blick hinein zu riskieren, denn die Methode ist heute unverzichtbar für die analytische Chemie. Die quantitativen Möglichkeiten werden häufig unterschätzt, erfahren allerdings durch den aufstrebenden Markt kompakter Benchtop-NMR-Spektrometer verstärktes Interesse für Anwendungen von der Laborbank bis hin zum Industrieprozess. KW - NMR-Spektroskopie KW - Benchtop-NMR KW - qNMR PY - 2020 UR - https://analyticalscience.wiley.com/do/10.1002/was.000600052 SN - 0016-3538 VL - 64 IS - 10 SP - 28 EP - 30 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-51464 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Klas T1 - Flexible Prozessanalytik für die pharmazeutische Produktion - Benchtop-NMR-Spektroskopie im industriellen Einsatz N2 - Im Rahmen des EU-Projekts „CONSENS – Integrated Control and Sensing“ wurde ein vollautomatisiertes, gemäß Atmosphère-Explosibles(ATEX)-Regeln zertifiziertes Analysatormodul auf Basis eines kommerziellen Benchtop-Kernspinresonanzspektrometers (Engl. nuclear magnetic resonance, NMR) entwickelt und im Umfeld einer modularen containerbasierten Produktionsanlage validiert. Auf Basis der gewonnenen Daten konnten sowohl eine iterative Optimierung der Prozessparameter erfolgen als auch Referenzdaten für die Kalibrierung eines Nahinfrarot-Spektrometers gewonnen werden. KW - Prozessanalytik KW - NMR-Spektroskopie KW - Modulare Produktion KW - Kalibriertransfer PY - 2022 VL - 12 IS - 3 SP - 122 EP - 129 PB - Editio Cantor Verlag CY - Aulendorf AN - OPUS4-55402 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weigel, Sandra A1 - Sielaff, S. A1 - Kunsic-Nowak, T. A1 - Nytus, N. A1 - Schwettmann, K. A1 - Schulze, C. A1 - Wetekam, J. T1 - Die FTIR-Untersuchung von Bitumen: Chancen, Durchführung und Präzision N2 - Die Fourier-Transformations-Infrarot-Spektroskopie (FTIR-Spektroskopie) stellt eine innovative und wirkungsvolle Methode zur Charakterisierung von Bitumen und bitumenhaltigen Bindemitteln dar. So erlaubt die FTIRCharakterisierung nicht nur eine Bewertung des Alterungsfortschritts eines Bindemittels, sondern zudem auch die Identifizierung von im Bitumen enthaltenen Additiven und Schadstoffen wie z. B. polyzyklischen aromatischen Kohlenwasserstoffen (PAK), die Ableitung verschiedener physikalischer und chemischer Kennwerte sowie weiterhin eine Klassifizierung von Bindemitteln nach verschiedenen übergeordneten Eigenschaften wie der Raffinerie, dem Alterungszustand und auch der Alterungsempfindlichkeit. KW - Bitumen und bitumenhaltige Bindemittel KW - FTIR-Spektroskopie KW - Anwendungsmöglichkeiten KW - Vergleichuntersuchung KW - Arbeitsanleitung KW - Präzision PY - 2023 UR - https://www.kirschbaum.de/fachzeitschriften/strasse-und-autobahn/strasse-und-autobahn/aktuelles-heft-17.html DO - https://doi.org/10.53184/STA8-2023-4 VL - 74/8 SP - 630 EP - 642 PB - KIRSCHBAUM VERLAG GmbH CY - Bonn AN - OPUS4-59049 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Dierckes, G. A1 - Göckener, B. A1 - Koschorreck, J. A1 - Meermann, Björn T1 - Analyse von PFAS mittels (Non-)Target HRMS, dTOPA und EOF in Schwebstoff-Proben aus Zeitreihen der Umweltprobenbank N2 - Per- und polyfluorierte Alkylverbindungen (PFAS) sind eine Substanzklasse bestehend aus mehreren tausenden Einzelverbindungen. Unter PFAS zählen alle Verbindungen, die mindestens eine perfluorierte Methyl- (-CF3) oder Methylen-Gruppe (-CF2-) besitzen. Somit zählt auch ein großer Teil der fluorierten Medikamente, Pflanzenschutzmittel oder Biozide in die PFAS-Substanzklasse. Aufgrund der Persistenz, Bioakkumulation in Nahrungsketten, Toxizität und der ubiquitären Verbreitung von PFAS zählen sie zu den „emerging pollutants“. Die PFAS-Analytik ist wegen ihrer vielfältigen physikalisch-chemischen Eigenschaften und der sehr hohen Anzahl an PFAS eine große Herausforderung. Da es für viele Anwendungen noch ungewiss ist, welche PFAS verwendet werden, wie sie in die Umwelt gelangen und welche Transformations- bzw. Abbauprodukte entstehen, stoßen analytische Ansätze, die nur auf Einzelsubstanzen abzielen, hier an ihre Grenzen. PFAS-Summenparameter-Methoden, die darauf abzielen ein möglichst vollständiges Abbild der PFAS-Belastungssituation widerzuspiegeln, werden daher immer wichtiger. KW - PFAS KW - HR-CS-GFMAS KW - Fluorine KW - SPM KW - LC-MS/MS KW - Schwebstoffe PY - 2023 VL - 5 SP - 1 EP - 6 AN - OPUS4-57544 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, X.Q. A1 - Li, H.M. A1 - Jiao, H. A1 - Guo, Z.H. A1 - Zhang, Q.H. A1 - Kneeteman, L.E. A1 - Lewin, M. A1 - Pires do Rego, E.C. A1 - Leal, R.V. A1 - Violante, F.G.M. A1 - Riedel, Juliane A1 - Koch, Matthias T1 - CCQM Key Comparison track A CCQM-K168: Non-polar analytes in high carbohydrate food matrix: trans-zearalenone in maize powder N2 - Demonstrating competency and equivalence for the measurement capacity of contaminants and nutrients in primary foodstuffs is a priority of the OAWG 10-year strategy for Track A core comparisons. Such measurements have posed significant challenges for reference material producers and calibration service providers. This key comparison (KC), under the topic of “non- polar analyte in high carbohydrate food matrix: trans-Zearalenone (trans-ZEN) in maize powder” , was a sector of the model system selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to demonstrate the Calibration and Measurement Capabilities (CMCs) of national metrology institutes (NMIs) and designated institutes (DIs). 17 NMIs and DIs participated in the Track A KC CCQM- 168 “non-polar analyte in high carbohydrate food matrix: trans-ZEN in maize powder” . Participants were requested to evaluate the mass fraction (μg/kg) of trans-ZEN in maize powder material. Methods like liquid-liquid extraction and SPE were applied in the pre-treatment, and HPLC-MS/MS and HPLC-FLD were used for detection by the participants. The mass fractions for trans-ZEN were in the range of (91.8 to 169) μg/kg with standard uncertainties of (1.5 to 24.7) μg/kg, and corresponding relative standard uncertainties from 1.5% to 14.6%. Two labs, INTI and BAM were excluded from the KCRV evaluation. INTI result was identified as an outlier and confirmed their method had insufficient specificity. For BAM the calibration approach they used does not meet the CIPM traceability requirements. The other 15 labs included in the calculation of the consensus KCRV all agreed within their standard uncertainties. Hierarchical Bayes was used as estimators in calculating KCRV and standard uncertainty. Successful participation in CCQM-K168 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 1 μg/kg to 1000 μg/kg in a high carbohydrate food matrix. KW - Metrology KW - Quality Assurance KW - Mycotoxin Analysis KW - Sustainable Food Safety PY - 2023 DO - https://doi.org/10.1088/0026-1394/60/1A/08021 VL - 60 IS - 1a SP - 08021 AN - OPUS4-59059 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bilsel, M. A1 - Gökçen, T. A1 - Binici, B. A1 - Isleyen, A. A1 - Piechotta, Christian A1 - Kar-wai, A. A1 - Krylov, A. A1 - Miheeva, A. A1 - Beliakov, M. A1 - Palagina, M. A1 - chenko, Irina Tka A1 - Perkola, N. A1 - Lewin, M. A1 - Hua, T. T1 - High polarity analyte(s) in aqueous media: determination of L-PFOA and L-PFOS in ground water N2 - The CCQM-K156 comparison was coordinated by TUBITAK UME on behalf of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) for National Measurement Institutes (NMIs) and Designated Institutes (DIs) which provide measurement services in organic analysis under the 'Comité International des Poids et Mesures' Mutual Recognition Arrangement (CIPM MRA). Perfluoro alkyl substances (PFAS) such as PFOS and PFOA have been used in numerous industrial applications and products. Because of their high stability and resistance to biodegradation, atmospheric photooxidation, direct photolysis and hydrolysis, they are extremely persistent in the environment. The European Union (EU) Water Framework Directive lists PFOS as a priority hazardous substance that poses a significant risk to the aquatic environment. The use of PFOS-containing Aqueous Film-Forming Foams (AFFFs) has been banned since June 2011 in the EU. As relatively water-soluble, effectively non-degradable compounds, PFOS and PFOA migrate to ground water. They are not removed in the conventional drinking water treatment, and therefore cause health risks in polluted areas. The EU Drinking Water Directive and the European Commission has proposed a limit value of 100 ng/L for the sum of 20 PFAS, including PFOS and PFOA. This study provides the means for assessing measurement capabilities for determination of high polarity measurands in a procedure that requires extraction, clean-up, analytical separation and detection. Successful participation in CCQM-K156 demonstrates measurement capabilities in determining mass fraction of organic compounds, with a molecular mass of 200 g/mol to 700 g/mol, having high polarity pKow -2, in a mass fraction range from 0.5 ng/kg to 500 ng/kg in aqueous media. Nine NMIs and DIs participated in the CCQM-K156 key comparison. Seven institutes reported their results. SPE was applied in the sample pre-treatment and LC-MS was applied for detection. All participating laboratories applied isotope dilution mass spectrometry (IDMS) techniques for quantification. Participants established the metrological traceability of their results using certified reference materials (CRMs) from NMIs with stated traceability; where commercially available high purity materials were used the purity was determined in-house. The CCQM-K156 results for L-PFOA and L-PFOS range from 2.75 ng/kg to 5.50 ng/kg with a % RSD of 19.5 % for L-PFOA and from 2.04 ng/kg to 4.45 ng/kg with a % RSD of 21.3 % for L-PFOS. The KCRV was assigned using a Hierarchical Bayesian Random Effects Model (HB REM) estimator from the values reported by six of the participants. One participant result of L-PFOS and one result of L-PFOA were excluded from the KCRV for technical reasons. The KCRV was 4.9 ng/kg ± 0.4 ng/kg for L-PFOA and 3.8 ng/kg ± 0.4 ng/kg for L-PFOS. The six institutes that were included in the assignment of consensus KCRV all agreed within their standard uncertainties. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - PFAS KW - Surface water KW - ILC KW - CCQM PY - 2022 DO - https://doi.org/10.1088/0026-1394/59/1A/08016 VL - 59 IS - 1A SP - 1 EP - 3 PB - IOP Publishing AN - OPUS4-58941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiesner, Yosri A1 - Altmann, Korinna A1 - Braun, U. T1 - Determination of Microplastic Mass Content by Thermal Extraction Desorption Gas Chromatography– Mass Spectrometry N2 - The scientific and practical challenge of detecting microplastics (MPs) in the environment in a targeted and rapid manner is solved by innovative coupling of thermogravimetric analysis with mass spectrometric methods. Fast identification and quantitative determination of most thermoplastic polymers and elastomers is possible by using thermal extraction Desorption gas chromatography–mass spectrometry (TED-GC–MS). KW - Microplastics KW - Mikroplastik KW - TED-GC/MS KW - Microplastics analytic KW - Mikroplastik Massegehalt PY - 2021 VL - 17 IS - 3 SP - 2 EP - 7 PB - MultiMedia (UK) LLC CY - Cranbury AN - OPUS4-52570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Alfeld, M. A1 - Eckhardt, H.-S. A1 - Kraft, J. A1 - Maiwald, Michael A1 - Meermann, Björn A1 - Merz, K. A1 - Prikler, S. A1 - Richert, J. A1 - Steiner, G. A1 - von Tümpling, W. T1 - Trendbericht Analytische Chemie N2 - Zusätzlich zu Methodenentwicklung, Miniaturisierung und Kopplungsverfahren zeigen sich die Hyperspektroskopie zusammen mit Imaging‐Verfahren, der Einzelmolekülnachweis und der Einsatz von 3‐D‐Druckern als neue Schwerpunkte. Hinzu kommen künstliche Intelligenz bei Sensoren, Bildgebungsverfahren und Prozesssteuerung sowie die Vernetzung von Analyse‐ und Laborgeräten. Trends und Forschungsthemen aus der analytischen Chemie, zusammengestellt von elf Autoren, koordiniert von Günter Gauglitz. KW - Multielementanalytik KW - Multimodale Analytik KW - Kristallolgraphie KW - Prozessanalytik KW - Prozessindustrie KW - Industrielle Analytik KW - Chemometrik KW - Chemometrie PY - 2020 DO - https://doi.org/10.1002/nadc.20204095786 SN - 1868-0054 VL - 68 IS - 4 SP - 52 EP - 60 PB - Wiley CY - Weinheim AN - OPUS4-50609 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Goedecke, Caroline A1 - Bannick, C.-G. A1 - Abusafia, A. A1 - Scheid, C. A1 - Steinmetz, H. A1 - Paul, Andrea A1 - Beleites, C. A1 - Braun, U. T1 - Identification of microplastic pathways within a typical European urban wastewater system N2 - In recent years, thermoextraction/desorption-gas chromatography/mass spectrometry (TED-GC/MS) has been developed as a rapid detection method for the determination of microplastics (MP) mass contents in numerous environmentally relevant matrices and, in particular, for the measurement of polymers in water samples without time-consuming sample preparation. The TED-GC/MS method was applied to investigate a typical European municipal wastewater system for possible MP masses. Such investigations are important in view of the recent revision of the Urban Wastewater Treatment Directive. Four different representative sampling sites were selected: greywater (domestic wastewater without toilet), combined sewer, and influent and effluent of a wastewater treatment plant (WWTP). All samples were collected by fractional filtration. Filtration was carried out over mesh sizes of 500, 100, 50, and in some cases, 5 µm. Polyethylene (PE), polypropylene (PP), and polystyrene (PS) were detected in all samples, with the PE fraction dominating in all cases. Styrene-butadiene rubber which serves as an indication of tire abrasion, was only found in the influent of the WWTP. The highest MP mass contents were found in the combined sewer, so MP can become a source of pollution during heavy rain events when the capacity limits of the effluent are reached, and the polluted effluent is released uncontrolled into the environment. Based on the studies, MP retention from the WWTP could be estimated to be approximately 96%. Few trends in polymer type or mass contents were detected within the different fractions of the samples or when comparing samples to each other. KW - Microplastics KW - Microplastic analysis KW - TED-GC/MS KW - Microplastic pathways KW - Mass contents PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568289 DO - https://doi.org/doi.org/10.1002/appl.202200078 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eisentraut, Paul A1 - Altmann, Korinna T1 - Repräsentative Mikroplastik-Detektion in Umweltproben - Weiterentwicklung der TED-GC/MS N2 - Die große Herausforderung in der Detektion von Mikroplastik (MP)‑Partikeln (1-1000 µm) besteht darin, sie neben Millionen von natürlichen Partikeln in Umweltproben nachzuweisen. Zum Aufspüren von Senken, Eintragspfaden und für Monitoring-Kampagnen ist ein schnelles, automatisiertes Verfahren unerlässlich. Ein solches Verfahren wurde an der Bundesanstalt für Materialforschung und -prüfung (BAM) mit der ThermoExtraktion/Desorption-Gaschromatographie-Massenspektrometrie (TED-GC/MS) in den letzten Jahren entwickelt. KW - Mikroplastik KW - TED-GC/MS PY - 2021 UR - https://analyticalscience.wiley.com/do/10.1002/was.0004000195 SN - 0016-3538 SP - 2 EP - 5 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54266 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ogrinc, N. A1 - Rossi, A. M. A1 - Durbiano, F. A1 - Becker, Roland A1 - Milavec, M. A1 - Bogozalec Kosir, A. A1 - Kakoulides, E. A1 - Ozer, H. A1 - Akcadag, F. A1 - Goenaga-Infante, H. A1 - Quaglia, M. A1 - Mallia, S. A1 - Umbricht, G. A1 - O'Connor, G. A1 - Guettler, B. T1 - Support for a European metrology network on food safety Food-MetNet N2 - This paper describes Food-MetNet, a coordinated preparatory initiative to establish the European Metrology Network on Food Safety (EMN-FS). Food-MetNet aims to establish a long-term ongoing dialogue between the metrology community and relevant stakeholders, in particular, European Union Reference Laboratories (EURLs), National Reference Laboratories (NRLs) and the Joint Research Centre (JRC). This dialogue is meant to support the collection of needs from stakeholders, the take-up of metrological research output and the development of the roadmaps needed to navigate future research. KW - Network KW - Metrology KW - Food KW - Safety KW - Stakeholders PY - 2021 DO - https://doi.org/10.1016/j.measen.2021.100285 VL - 18 SP - 1 EP - 4 PB - Elsevier AN - OPUS4-53740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ecke, Alexander A1 - Bohm, Konrad A1 - Schneider, Rudolf T1 - Magnetpartikelbasierte Immunoassays als vielseitiges Werkzeug für die Umweltanalytik N2 - Der Bedarf nach schnellen und kostengünstigen Analysemethoden in der (Trink-)Wasseranalytik steigt mit dem zunehmenden Eintrag pharmazeutisch aktiver Substanzen in die Umwelt. Insbesondere die Kontamination mit Antibiotika erscheint neben ökotoxikologischen Effekten vor allem in Hinblick auf die Evolution resistenter Keime im Wasser besorgniserregend. Wir berichten hier über die Entwicklung eines magnetpartikelbasierten Immunoassays (MBBA) zur Detektion des Breitbandantibiotikums Amoxicillin (AMX) in Wasserproben, der im Vergleich zum entsprechenden Enzyme-linked Immunosorbent Assay (ELISA) eine wesentlich kürzere Analysendauer sowie einen breiteren Messbereich mit niedrigerer Nachweisgrenze aufweist. Das angewendete Assayprinzip ist dabei leicht auf weitere Analyten übertragbar und ermöglicht die Implementierung in einen Immunosensor. KW - Magnetpartikel KW - Amoxicillin KW - Immunoassay KW - Wasser KW - Antikörper PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527366 UR - https://www.gdch.de/netzwerk-strukturen/fachstrukturen/umweltchemie-und-oekotoxikologie/publikationen/mitteilungen/archiv/2021.html SN - 1618-3258 VL - 27 IS - 2 SP - 48 EP - 51 PB - Gesellschaft Deutscher Chemiker (GDCh) CY - Frankfurt/Main AN - OPUS4-52736 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fernández, L. A1 - Lin, Z. A1 - Schneider, Rudolf A1 - Esteves, V. I. A1 - Cunha, Â. A1 - Tomé, J. P. C. T1 - Antimicrobial Photodynamic Activity of Cationic Nanoparticles Decorated with Glycosylated Photosensitizers for Water Disinfection N2 - The antimicrobial photodynamic approach has been demonstrated as an efficient and sustainable process for the eradication of microbial pathogens. In this work, silica-coated Magnetite nanoparticles (NPs) were used as carriers of glycosylated porphyrins and phthalocyanines. Their subsequent cationization resulted in the production of stable antimicrobial photosensitizing materials, effective against E. coli. Suspensions of the photocatalysts in water present bimodal size distributions formed by big clusters and small NPs with hydrodynamic diameters between 8 and 38 nm. The presence of small NPs in the suspensions is related to an effective photodynamic inactivation (PDI) of E. coli cells. Glycosylation of the PS showed a positive effect on the PDI performance, which could be related to a higher accumulation of the photocatalyst over the bacterial cell membrane. In addition, these biocidal agents proved to be photostable and their photoactive performance decreased only between 23% and 28% upon 5 PDI cycles, mostly because of the loss of material between cycles, which makes them promising materials for water disinfection purposes. KW - Photodynamische Inaktivierung KW - E. coli KW - Photokatalyse KW - Bakterien KW - Nanopartikel KW - Photosensibilisator KW - Porphyrin KW - Phthalocyanin PY - 2018 DO - https://doi.org/10.1002/cptc.201700169 SN - 2367-0932 VL - 2 IS - 7 SP - 596 EP - 605 PB - Wiley VHC CY - Weinheim AN - OPUS4-45684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Löhr, Konrad A1 - Traub, Heike A1 - Wanka, Antje Jutta A1 - Panne, Ulrich A1 - Jakubowski, Norbert T1 - Quantification of metals in single cells by LA-ICP-MS: Comparison of single spot analysis and imaging N2 - LA-ICP-MS is increasingly used for single cell analysis in two different detection modes using either the imaging mode with subcellular resolution or alternatively single spot analysis of cells with a larger laser spot size. This study compares the analytical figures of merit of both detection modes (signal to noise, precision, accuracy, throughput), as well as ease of operation and data evaluation. Adherent 3T3 fibroblast cells were stained with two metal dyes (mDOTA-Ho, Ir-DNA-intercalator) and several dozen cells were measured using both modes. We found a ten times higher throughput for single spot analysis, which has as well a straightforward data analysis, shortening the total analysis time further. The signal to noise ratio for single spot analysis was found to be slightly better compared to the signal to noise of pixels in imaging. The mean metal intensity per single cell differed by only 10% between both modes and obtained distributions were found to show no statistically significant differences. Using matrix matched calibration based on standards spotted onto nitrocellulose membrane, we achieved detection limits (10s) of 12 fg for Ir and 30 fg for Ho and quantified 57 +/-35 fg Ir and 1192 +/- 707 fg Ho per single cell. Compared to a conventional ICP-MS measurement of a digest of about 60000 cells, 54% of Ir content and 358% Ho content was found using quantitative LA-ICP-MS. The difference might be a consequence of the two metal dyes binding to different structures of the cell and therefore might behave differently in sample preparation for conventional and LA-ICP-MS. KW - Cells KW - Laser ablation KW - ICP-MS KW - Metals KW - Quantification PY - 2018 DO - https://doi.org/10.1039/c8ja00191j SN - 0267-9477 VL - 33 IS - 9 SP - 1579 EP - 1587 PB - RSC Royal Society of Chemistry CY - London AN - OPUS4-46441 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hill, Sarah A1 - Infante, Heidi Goenaga A1 - Entwisle, John A1 - Strekopytov, Stanislav A1 - Ward-Deitrich, Christian A1 - Cowen, Simon A1 - Rienitz, Olaf A1 - Roethke, Anita A1 - Goerlitz, Volker A1 - Schulz, Ursula A1 - Pape, Carola A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Jacimovic, Radojko A1 - Fisicaro, Paola A1 - Ren, Tongxiang A1 - Wang, Song A1 - Song, Panshu A1 - Li, Haifeng A1 - Linsky, Maré A1 - Sobina, Egor A1 - Lozano, Hernán Ezequiel A1 - Puelles, Mabel A1 - Yamani, Randa A1 - Haraldsson, Conny T1 - CCQM-K160: platinum group elements in automotive catalyst N2 - The platinum group elements (PGEs) play an important role in reducing emissions from automotive vehicles through their use in catalytic convertors but also for catalysis in the pharmaceutical industry. The immense economic value of platinum (Pt), palladium (Pd) and rhodium (Rh) highlights the importance of highly accurate measurements. Therefore, there is a need for National Metrology Institutes (NMIs) and Designated Institutes (DIs) to demonstrate measurement capability in this space. A pilot comparison (CCQM-P63) for precious metals in automotive catalyst took place in 2006, but with a limited number of institutes participating. Furthermore, this study was performed over 17 years ago. Therefore, there was a need to maintain existing capability and demonstrate new capability in a key comparison, in order to claim calibration and measurement capability claims (CMCs). With the core capability matrix, this study falls into the "Difficult to dissolve metals/metal oxides" which will support CMC categories 8 (Metal and metal alloys), 9 (Advanced materials) and 14 (Other materials). Eleven NMIs and DIs participated in the Key Comparison CCQM-K160 Platinum Group Elements in Automotive Catalyst. Participants were requested to evaluate the mass fractions of Pt, Pd and Rh in mg/kg in an unused autocatalyst material (cordierite ceramic base). The Key Comparison Reference Values (KCRVs) and Degrees of Equivalence (DoEs) were calculated utilising the NIST Decision Tree for the measurands. The participants utilised a number of sample preparation and analytical methods including hot plate digestion, microwave digestion and sodium fusion, followed by either atomic absorption spectroscopy (AAS), inductively coupled plasma optical emission spectroscopy (ICP-OES) or inductively coupled plasma mass spectrometry (ICP-MS) detection. Several calibration techniques were used, namely external calibration, standard addition, isotope dilution mass spectrometry (IDMS) and an exact matching procedure. Additionally, one participant employed instrumental neutron activation analysis (INAA) with k0 standardisation which is a direct solid analysis method. The majority of participants claimed traceability to NIST primary calibrants or their own CRMs. Furthermore, several matrix CRMs were included or spiked samples for quality control. All institutes were required to determine the dry mass fraction using the stipulated protocol. The NIST decision tree was implemented for the calculation of the KCRVs and DoEs. The participant results overall showed good agreement with the KCRV, despite the variety of dissolution procedures and measurement techniques for this highly complex matrix and challenging measurands. Successful participation in CCQM-K160 demonstrated measurement capabilities for the determination of mass fraction of Pt, Pd and Rh in the mg/kg range and will support broad scope CMC claims for a wide range of challenging matrices. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - Metrology in Chemistry KW - Traceability KW - Uncertainty PY - 2024 DO - https://doi.org/10.1088/0026-1394/61/1A/08011 VL - 61 IS - 1A SP - 1 EP - 39 PB - IOP Publishing AN - OPUS4-60524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Küttenbaum, Stefan T1 - Zur Visualisierung von Schäden in Betonschwellen durch zerstörungsfreie Ultraschallprüfung N2 - Die bildgebende Ultraschalltechnik liefert Hinweise auf verdeckte Schäden in Spannbetonschwellen. Dieses zerstörungsfreie Prüfverfahren schafft eine objektive und vergleichbare Basis für die Zustandsbestimmung der Schwellen und ermöglicht die Optimierung von baulichen Erhaltungsstrategien. KW - Betonschwellen KW - Ultraschall KW - Schieneninfrastruktur KW - Gleisoberbau KW - Spannbetonschwelle PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591889 UR - https://www.eurailpress.de/etr SN - 0013-2845 IS - 12 SP - 26 EP - 31 PB - DVV Media Group, Eurailpress CY - Hamburg AN - OPUS4-59188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kornev, Roman A1 - Gornushkin, Igor B. A1 - Shabarova, Lubov A1 - Kadomtseva, Alena A1 - Mochalov, Georgy A1 - Rekunov, Nikita A1 - Romanov, Sergey A1 - Medov, Vitaly A1 - Belousova, Darya A1 - Maleev, Nikita T1 - Plasma-Chemical Disposal of Silicon and Germanium Tetrachlorides Waste by Hydrogen Reduction N2 - The processes of hydrogen reduction of silicon and germanium chlorides under the conditions of high-frequency (40.68 MHz) counteracted arc discharge stabilized between two rod electrodes are investigated. The main gas-phase and solid products of plasma-chemical transformations are determined. Thermodynamic analysis of SiCl4 + H2 and GeCl4 + H2 systems for optimal process parameters was carried out. Using the example of hydrogen reduction of SiCl4 by the method of numerical modeling, gas-dynamic and thermal processes for this type of discharge are investigated. The impurity composition of gas-phase and solid reaction products is investigated. The possibility of single-stage production of high-purity Si and Ge mainly in the form of compact ingots, as well as high-purity chlorosilanes and trichlorogermane, is shown. KW - High-frequency arc discharge KW - Hydrogen reduction KW - Silicon chlorides KW - Germanium chlorides PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594454 DO - https://doi.org/10.3390/sci6010001 VL - 6 IS - 1 SP - 1 EP - 12 PB - MDPI AG AN - OPUS4-59445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Gornushkin, Igor B. A1 - Griesche, Axel A1 - Kannengiesser, Thomas A1 - Treutler, Kai A1 - Wesling, Volker T1 - In situ chemical analysis of duplex stainless steel weld by laser induced breakdown spectroscopy N2 - The high corrosion resistance and good mechanical properties of duplex stainless steel (DSS) are due to its special chemical composition, which is a balanced phase ratio of ferrite (α) and austenite (γ). Many industrial applications require the integration of DSS components. For this, Gas tungsten arc welding (GTAW) is an excellent choice, as it allows an automated operation with high reproducibility. However, when the weld pool solidifies, critical ratios of α- and γ- phases can occur, which lead to solidification cracking, increased susceptibility to corrosion, and a decrease in ductility and critical strength. Previous studies have shown that these defects can be caused by the accumulation of manganese and chromium in the heat affected zone (HAZ), requiring ongoing monitoring of this accumulation. A suitable method for such monitoring is laser-induced breakdown spectroscopy (LIBS), which can be used in two operating modes: calibration using standard reference samples and calibration-free. Unlike conventional quantitative LIBS measurements, which require reference samples to generate a calibration curve, calibration-free LIBS (CF-LIBS) allows chemical compositions to be determined solely from the emission spectrum of the plasma. Numerous publications show that CF-LIBS is a fast and efficient analytical method for the quantitative analysis of metal samples. In this work, CF-LIBS is applied to spectra obtained during GTAW DSS welding and the result is compared with those obtained by PLS analysis. A good correlation was found between both types of analysis, demonstrating the suitability of the CF-LIBS method for this application. The CF-LIBS method has a significant advantage over conventional LIBS due to the rapid in situ measurement of concentrations of major alloying elements without calibration procedure. This, combined with fast feedback and appropriate adjustment of welding parameters, helps prevent welding defects. KW - Duplex stainless steels KW - In situ measurement KW - LIBS KW - GMAW PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597940 DO - https://doi.org/10.1016/j.sab.2024.106899 SN - 0584-8547 VL - 214 SP - 1 EP - 7 PB - Elsevier B.V. AN - OPUS4-59794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mi, W. A1 - Josephs, R. D. A1 - Melanson, J. E. A1 - Dai, X. A1 - Wang, Y. A1 - Zhai, R. A1 - Chu, Z. A1 - Fang, X. A1 - Thibeault, M.-P. A1 - Stocks, B. B. A1 - Meija, J. A1 - Bedu, M. A1 - Martos, G. A1 - Westwood, S. A1 - Wielgosz, R. I. A1 - Liu, Q. A1 - Teo, T. L. A1 - Liu, H. A1 - Tan, Y. J. A1 - Öztuğ, M. A1 - Saban, E. A1 - Kinumi, T. A1 - Saikusa, K. A1 - Schneider, Rudolf A1 - Weller, Michael G. A1 - Konthur, Zoltán A1 - Jaeger, Carsten A1 - Quaglia, M. A1 - Mussell, C. A1 - Drinkwater, G. A1 - Giangrande, C. A1 - Vaneeckhoutte, H. A1 - Boeuf, A. A1 - Delatour, V. A1 - Lee, J. E. A1 - O'Connor, G. A1 - Ohlendorf, R. A1 - Henrion, A. A1 - Beltrão, P. J. A1 - Naressi Scapin, S. M. A1 - Sade, Y. B. T1 - PAWG Pilot Study on Quantification of SARS-CoV-2 Monoclonal Antibody - Part 1 N2 - Under the auspices of the Protein Analysis Working Group (PAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a pilot study, CCQM-P216, was coordinated by the Chinese National Institute of Metrology (NIM), National Research Council of Canada (NRC) and the Bureau International des Poids et Mesures (BIPM). Eleven Metrology Institutes or Designated Institutes and the BIPM participated in the first phase of the pilot study (Part 1). The purpose of this pilot study was to develop measurement capabilities for larger proteins using a recombinant humanized IgG monoclonal antibody against Spike glycoprotein of SARS-CoV-2 (Anti-S IgG mAb) in solution. The first phase of the study was designed to employ established methods that had been previously studies by the CCQM Protein Analysis Working Group, involving the digestion of protein down to the peptide or amino acid level. The global coronavirus pandemic has also led to increased focus on antibody quantitation methods. IgG are among the immunoglobulins produced by the immune system to provide protection against SARS-CoV-2. Anti-SARS-CoV-2 IgG can therefore be detected in samples from affected patients. Antibody tests can show whether a person has been exposed to the SARS-CoV-2, and whether or not they potentially show lasting immunity to the disease. With the constant spread of the virus and the high pressure of re-opening economies, antibody testing plays a critical role in the fight against COVID-19 by helping healthcare professionals to identify individuals who have developed an immune response, either via vaccination or exposure to the virus. Many countries have launched large-scale antibody testing for COVID-19. The development of measurement standards for the antibody detection of SARS-CoV-2 is critically important to deal with the challenges of the COVID-19 pandemic. In this study, the SARS-CoV-2 monoclonal antibody is being used as a model system to build capacity in methods that can be used in antibody quantification. Amino acid reference values with corresponding expanded uncertainty of 36.10 ± 1.55 mg/kg, 38.75 ± 1.45 mg/kg, 18.46 ± 0.78 mg/kg, 16.20 ± 0.67 mg/kg and 30.61 ± 1.30 mg/kg have been established for leucine, valine, phenylalanine, isoleucine and proline, respectively. Agreement between nearly all laboratories was achieved for the amino acid analysis within 2 to 2.5 %, with one participant achieving markedly higher results due to a technical issue found in their procedure; this result was thus excluded from the reference value calculations. The relatively good agreement within a laboratory between different amino acids was not dissimilar to previous results for peptides or small proteins, indicating that factors such as hydrolysis conditions and calibration procedures could be the largest sources of variability. Peptide reference values with corresponding expanded uncertainty of 4.99 ± 0.28 mg/kg and 6.83 ± 0.65 mg/kg have been established for ALPAPIEK and GPSVFPLAPSSK, respectively. Not surprisingly due to prior knowledge from previous studies on peptide quantitation, agreement between laboratories for the peptide-based analysis was slightly poorer at 3 to 5 %, with one laboratory's result excluded for the peptide GPSVFPLAPSSK. Again, this level of agreement was not significantly poorer than that achieved in previous studies with smaller or less complex proteins. To reach the main text of this paper, click on Final Report. KW - Antibody quantification KW - Amino acid analysis KW - Peptide analysis KW - Round robin test PY - 2021 DO - https://doi.org/10.1088/0026-1394/59/1a/08001 VL - 59 IS - 1A SP - 08001 AN - OPUS4-54972 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Hampel, S. A1 - Fittschen, UEA A1 - Streli, C. A1 - Radtke, Martin T1 - Reconstruction for coded aperture full-field x-ray fluorescence imaging N2 - X-ray fluorescence imaging is a well-established tool in materials characterization. In this work, we present the adaption of coded aperture imaging to full-field X-ray fluorescence imaging at the synchrotron. Coded aperture imaging has its origins in astrophysics, and has several advantages: Coded apertures are relatively easy to fabricate, achromatic, allow a high photon throughput, and high angular acceptance. Coded aperture imaging is a two-step-process, consisting of the measurement process and a reconstruction step. Different programs have been written, for the raytracing/forward projection and the reconstruction. Experiments with coded aperture in combination with a Color X-ray Camera and an energy-dispersive area detector, have been conducted at the BAMline. Measured samples were successfully reconstructed, and gave a 9.1-fold increase in count rate compared to a polycapillary optic. KW - Synchrotron KW - BAMline KW - Coded Aperture PY - 2022 SN - 1097-0002 VL - 65 SP - 57 EP - 70 PB - Cambridge University Press CY - Cambridge AN - OPUS4-56350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fittschen, U.E.A. A1 - Möckel, R. A1 - Schreiner, M. A1 - klinger, M. A1 - Radtke, Martin A1 - Meyer, B. A1 - Guhl, S. A1 - Renno, A. A1 - Godinho, J. A1 - Gloaguen, R. A1 - Gutzmer, J. T1 - Bundling analytical capacities to understand phase formation in recycling of functional materials N2 - Transitioning from combustion engine-driven transportation to e-mobility demands a paradigm shift – from a system geared to maximize energy efficiency (i.e. fuel consumption) to a system that may be constrained by the availability of high technology (critical) metals required for electrical energy storage systems and drives. In the wake of these developments efforts in securing new resources of these metals from recycling of end-of-life products are increasing steadily. Recycling of Li-Ion batteries has recently been evaluated. The results pinpoint to a critical need for understanding slag Formation and its dependence on metal components like Mn under extreme conditions. This will allow researchers to predict optimal Operation setting and to react quickly to changing market demands (which may be Li or Co at one point but may also shift to Ni or rare earth elements (REE)). The long-term goal is to control the formation of specific phases in slags allowing for a Maximum yield of elements of interest and optimal recovery in the separation processes that follows. The combination of data on the physical micro structure and local chemistry of the multi-Phase products during and after processing will help to understand and derive thermodynamic and kinetic data on its formation. In this paper we are giving an overview on the analytical challenges and approaches to provide robust data on local element concentration and species (especially Mn which is a common component of next generation Li-ion batteries cathodes), spanning the dimensions from the nanometer scale to the bulk material. The complementary interactions of X-rays and electrons make them ideal probes to collect Interface and “in-depth” information. Before- and -after studies as well as in situ structural changes and Phase (trans)formation, changes in elemental and elemental species (e.g. oxidation state) distribution may be tracked by X-ray diffraction (XRD), X-ray fluorescence microscopy and X-ray Absorption spectroscopy. The application of such advanced analytical tools will not only provide essential clues during early lab-based experiments towards the development of new recycling technologies, but may also be deployed for on-line and in-line monitoring of industrial processes. KW - Synchrotron KW - XANES KW - Slags KW - Battery PY - 2019 DO - https://doi.org/10.4028/www.scientific.net/MSF.959.183 SN - 1662-9752 VL - 959 SP - 183 EP - 190 PB - Trans Tech Publ. AN - OPUS4-48900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lutz, C. A1 - Hampel, S. A1 - Beuermann, S. A1 - Turek, T. A1 - Kunz, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Fittschen, U. E. A. T1 - Investigation on Vanadium Species Distribution in Nafion™ 117 after Cyclization in a Vanadium Redox Flow Battery N2 - The vanadium redox flow battery (VRFB) is currently a potential candidate for stationary energy storage. A major challenge is the unintended vanadium transport through the separator, which results in a fade of capacity. To overcome this issue, it is necessary to understand the transport processes in the membrane on a more fundamental level. In this work, the vanadium species distribution in Nafion™ 117 after cyclization was investigated. Two membranes, one from a charged VRFB and another from a discharged VRFB, were analyzed using ultraviolet–visible spectroscopy (UV/VIS) and X-ray absorption near edge structure spectroscopy (XANES). Little difference between the two membranes was recognizable according to the UV/VIS results. In comparison, the XANES results showed that the membrane from the charged VRFB contains more V3+ than VO2+, whereas for the discharged case, more VO2+ is present in the membrane. KW - Synchrotron KW - BAMline KW - XANES KW - Vanadium redox flow battery PY - 2021 VL - 64 SP - 1 EP - 8 AN - OPUS4-54144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Rakotondrajoa, A. T1 - Machine learning based quantification of synchrotron radiation-induced X-ray fluorescence measurements - a case study N2 - In this work, we describe the use of artificial neural networks for the quantification of X-ray fluorescence measurements. The training data were generated using Monte Carlo simulation, which avoided the use of adapted reference materials. The extension of the available data set by means of an ANN to generate additional data was demonstrated. Particular emphasis was put on the comparability of simulated and experimental data and how the influence of deviations can be reduced. The search for the optimal hyperparameter, manual and automatic, is also described. For the presented case, we were able to train a network with a mean absolute error of 0.1 weight percent for the synthetic data and 0.7 weight percent for a set of experimental data obtained with certified reference materials. KW - Machine learning KW - BAMline KW - XRF KW - Synchrotron KW - Neural network PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519008 DO - https://doi.org/10.1088/2632-2153/abc9fb SP - 1 EP - 16 PB - IOP Publishing AN - OPUS4-51900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -