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 - GEN A1 - Recknagel, Sebastian T1 - Certified reference materials for the determination of cadmium (Cd) in cocoa N2 - BAM has produced three cocoa CRMs certified for cadmium (ERM-BD513 – 515) as tools for checking analytical methods for Cd-determination. KW - Certified reference material KW - Cocoa KW - Cadmium PY - 2021 SP - 4 EP - 4 AN - OPUS4-53694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Tanz der Moleküle: Herkunftsbestimmung mittels optischer Spektroskopie N2 - Wie lässt sich die Herkunft von Rohstoffen, Lebensmitteln oder Umweltschadstoffen einfacher, schneller und kostengünstiger als mit bisherigen Methoden bestimmen? Die Dissertation zeigt auf, dass man das grundlegende physikalische Prinzip einer Isotopverschiebung mit in Adlershof entwickelten Optik-Instrumenten für die Herkunftsbestimmung nutzen kann. Die entwickelte Methode ermöglicht es in Zukunft den Ursprung von Rohstoffen, Lebensmitteln oder Umweltschadstoffen kostengünstiger und wesentlich schneller bestimmen, als dies mit bisherigen Methoden möglich ist. Kann man das grundlegende physikalische Prinzip einer Isotopieverschiebung mit einem Optik-Instrument für die Herkunftsbestimmung nutzen? Carlos Abad hat eine wegweisende Methode entwickelt, die es in Zukunft ermöglicht den Ursprung von Rohstoffen, Lebensmitteln oder Umweltschadstoffen kostengünstiger und wesentlich schneller bestimmen, als dies mit bisherigen Techniken möglich ist. T2 - Dissertationspreis Adlershof 2019 CY - Berlin, Germany DA - 12.02.2020 KW - Herkunftsbestimmung KW - Isotopenanalyse KW - Isotope KW - Optischer Spektroskopie KW - Coltan PY - 2020 AN - OPUS4-51993 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Isotopic analysis by high-resolution optical spectroscopy N2 - Isotope analysis can be used to determine the age and provenance of geological samples or to study dynamic systems like Li-ion batteries. Modern techniques in optical spectrometry allow us a fast and slow-cost isotope analysis. These techniques include high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS) and laser ablation molecular isotopic spectrometry. This seminar will discuss our recent work on precise and accurate isotope analysis of boron, magnesium, and lithium with geology, climate, and energy research applications. T2 - Recent Trends in Chemical Science and Technology, Christian College Chengannur, India CY - Online meeting DA - 29.09.2020 KW - Isotopes KW - Optical spectrometry KW - Machine learning PY - 2020 AN - OPUS4-51997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Isotope analysis by high-resolution optical spectroscopy: a tool for planetary science N2 - Isotope analysis can be used to determine the age and provenance of geological samples. Modern techniques in optical spectrometry allow us a stand-off isotope analysis. This seminar will discuss how planetary science with the next Moon and Mars missions drive optical spectrometry into precise and accurate isotope analysis and how BAM will contribute. T2 - Adlershofer Kolloquium CY - Online meeting DA - 19.05.2020 KW - Provenance KW - Dating KW - Isotopes KW - Optical spectroscopy KW - Isotopic shift KW - Planetary science PY - 2020 AN - OPUS4-51995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Advances and Applications of Molecular Absorption Spectrometry: from Non-Metals to Isotope Analysis N2 - Wie kann Nicht-Messbares messbar gemacht werden? Die Antwort der Dissertation auf diese zentrale Frage der analytischen Chemie lautet: die Anwendung der hochauflösenden optischen Spektroskopie der diatomischen Moleküle. In der Arbeit wird in einem ersten Schritt in Grafitöfen, die wie Chemiereaktoren funktionieren, und durch die Anwendung verschiedener analytischer Methoden die diatomische Molekülbildung nachvollzogen. In einem zweiten Schritt werden die aufgedeckten Mechanismen auf die Bestimmung von Nichtmetallen und die Analyse von Isotopen angewendet. Die Isotopenanalytik ist das zukunftsweisendes Herzstück der Dissertation und von alltäglicher und politischer Relevanz: Mittels dieser Technik lässt sich die Herkunft von Lebensmitteln aber auch Chemiewaffen kostengünstiger und wesentlich schneller bestimmen als mit bisherigen Methoden der Massenspektrometrie. Möglich ist die Bestimmung, da alles um uns herum aus Atomen verschiedener Elemente besteht und die meisten Elemente mehrere Isotope haben. Isotope unterscheiden sich hinsichtlich ihres Gewichts, da sie über eine unterschiedliche Anzahl an Neutronen verfügen. Die Informationen über das Verhältnis von schweren und leichten Isotopen lässt sich nutzen, um zu bestimmen wo etwas entstanden ist. Jeder Ort auf unserem Planeten hat seinen persönlichen Element- und Isotopenanteil (Isotopenfingerabdruck). Das in der Arbeit angewandte Instrument misst das Verhältnis indirekt und nutzt hierzu die Interaktion zwischen Licht und Materie. Für das schwerere Isotop wird mehr Licht/Energie benötigt, um es in Bewegung zu bringen, als für das leichtere. Diese kleinen Unterschiede an Energie, die wir dafür aufwenden müssen, werden gemessen und ermöglichen die Herkunftsbestimmung. Damit leistet die Arbeit nicht nur einen wichtigen Beitrag zur Grundlagenforschung in der analytischen Chemie, sondern kann mit den aufgezeigten Ergebnissen auch Anwendung in den Bereichen Verbraucherschutz, Umweltforschung und Waffenkontrolle finden. N2 - The present work covers two main aspects of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS), an analytical technique for elemental trace analysis. First, a comprehensive mechanistic study of molecule formation in graphite furnaces is presented, which is a key step into the recovery of analytical signals. For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in HR-CS-GFMAS. A zirconium coating catalyzes the CaF formation, and its structure was investigated. The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. Here a mechanism is proposed, where ZrO2 works as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. Second, analytical methods were developed by using HR-CS-MAS as detector for non-metals and isotope analysis. Therefore, the determination of organic absorbable chlorine in water, the quantification of fluorine in consume care products with declared perfluorinated ingredients, and the determination of sulfur content in crude oils were investigated. Finally, the high resolution of the instrumentation allows to measure isotopic shifts with high precision in some observed molecular spectra. Consequently, the molecular spectra of enriched isotopes of boron and magnesium were investigated, establishing so the potential of HR-CS-MAS for the accurate and precise determination of isotopic amount ratios. T2 - Applied Photonics Award 2020 CY - Jena, Germany DA - 22.09.2020 KW - Herkunftsbestimmung KW - Isotopenanalyse KW - Isotope KW - Optischer Spektroskopie PY - 2020 AN - OPUS4-51996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - Recent Trends in Inexpensive Lithium Isotopic Analysis N2 - Lithium exists in two stable isotopes, 6Li and 7Li. The ratio of these in every ore varies depending on the geological history of the sample, thus providing a tool for fingerprinting the distinct origin of Li containing samples. Determination of the exact isotope ratio for e.g. designation of provenance today relies on expensive and bulky instrumentation such as multi `collector inductively coupled plasma mass spectrometry` (MC-ICP-MS). These instruments, however, are known to bear pitfalls in the characterization of particular elements including Lithium. BAM recently developed two alternative analytical devices for this task, solely relying on inexpensive optical spectroscopy in combination with state-of-the-art multivariate data analysis such as Machine learning algorithms. Both techniques have been comprehensively studied using certified reference materials and comparing the results to MC-ICP-MS results and could be shown to result in comparable figures of merit, paving the way for a more general accessibility to provenance determination instrumentation. The results also pave the way towards even further simplification of the laboratory infrastructure demands and to further include additional elements into the isotopic fingerprinting methodology. T2 - Lithium-Days CY - Halle, Germany DA - 06.12.2021 KW - Lithium KW - Isotopes KW - Optical Spectroscopy PY - 2021 AN - OPUS4-53966 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - ISO-Guide 35 in der Praxis eines RM-Herstellers N2 - Der ISO-Guide 35 beschreibt die notwendigen Schritte zur Herstellung von zertifizierten Referenzmaterialien. Anhand praktischer Beispiele wird die Umsetzung des Guide 35 in der BAM dokumentiert. T2 - DAkkS-Begutachterschulung Modul E zur Akkreditierung von Eignungsprüfungsanbietern und Referenzmaterialherstellern CY - Online meeting DA - 04.02.2021 KW - ISO-Guide 35 KW - Referenzmaterial-Herstellung KW - ZRM PY - 2021 AN - OPUS4-52099 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, V. A1 - Uhlemann, M. A1 - Richter, Silke A1 - Pfeifer, jens T1 - Calibration capacity of hot-pressed hydrogen standards for glow discharge optical emission and mass spectrometry N2 - Mixed copper and titanium hydride powder was hot-pressed and characterized by Carrier Gas Hot Extraction, XRay Diffraction, Thermal Gravimetric Analysis coupled with Mass Spectrometry, and Scanning Electron Microscopy. The hot-pressed and five conventional samples were applied for calibration of hydrogen in Glow Discharge Optical Emission and Mass Spectrometry. Up to the introduction of 15 ng/s hydrogen the Emission yield model is useful in Glow Discharge Optical Emission Spectrometry. A correlation between saturation and even reversal of the emission yield of the spectral lines H121, H486 and H656 and low sputtering rates was found. Hydrogen effects exist for the spectral lines of Cu(II) 219 and Ti(I) 399. In Glow Discharge Mass Spectrometry, a linear dependency of the 1H ion current on the sputtered mass per time exists over the total range of hydrogen content investigated. Hydrogen effects also exist for the sensitivity of 48Ti and 63Cu. The sputtering rate of two-phase materials depends linearly on the sputtered mass per time of one phase, which allows the sputtering rate of two-phase materials with known composition to be predicted. KW - Hot-pressing KW - GD-OES KW - GD-MS KW - Calibration KW - Hydrogen KW - Titanium hydride KW - Sputtering KW - Two-phase system PY - 2021 DO - https://doi.org/10.1016/j.sab.2020.106039 VL - 176 SP - 106039 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-52074 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Soba, L. A1 - Tuma, Dirk T1 - Messung der Schallgeschwindigkeit in Neopentan bei Temperaturen von (263 bis 373) K und Drücken bis 20 MPa N2 - Alkan-Isomere haben signifikanten Einfluss als Spurenstoffe auf thermodynamische Eigenschaften von Erdgasgemischen. In Erdgas sind bis zu 0.35 mol-% Neopentan enthalten. Gemischmodelle basieren auf Reinstoffzustandsgleichungen der beteiligten Komponenten. Die hier untersuchte Schallgeschwindigkeit ist von besonderer Bedeutung für die Entwicklung hochgenauer Gleichungen. T2 - Thermodynamik-Kolloquium 2025 CY - Hamburg, Germany DA - 22.09.2025 KW - Neopentan KW - Schallgeschwindigkeit KW - Zustandsgleichung PY - 2025 AN - OPUS4-64226 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winckelmann, Alexander A1 - Morcillo Garcia-Morato, Dalia A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Riedel, Jens A1 - Vogl, Jochen A1 - Panne, Ulrich A1 - Abad Andrade, Carlos Enrique T1 - Determination of lithium in human serum by isotope dilution atomic absorption spectrometry N2 - The therapeutic dose of lithium (Li) compounds, which are widely used for the treatment of psychiatric and hematologic disorders, is close to its toxic level; therefore, drug monitoring protocols are mandatory. Herein, we propose a fast, simple, and low-cost analytical procedure for the traceable determination of Li concentration in human serum, based on the monitoring of the Li isotope dilution through the partially resolved isotope shift in its electronic transition around 670.80 nm using a commercially available high-resolution continuum source graphite furnace atomic absorption spectrometer. With this technique, serum samples only require acidic digestion before analysis. The procedure requires three measurements—an enriched 6Li spike, a mixture of a certified standard solution and spike, and a mixture of the sample and spike with a nominal 7Li/6Li ratio of 0.82. Lanthanum has been used as an internal spectral standard for wavelength correction. The spectra are described as the linear superposition of the contributions of the respective isotopes, each consisting of a spin-orbit doublet, which can be expressed as Gaussian components with constant spectral position and width and different relative intensity, reflecting the isotope ratio in the sample. Both the spectral constants and the correlation between isotope ratio and relative band intensity have been experimentally obtained using commercially available materials enriched with Li isotopes. The Li characteristic mass (mc) obtained corresponds to 0.6 pg. The procedure has been validated using five human serum certified reference materials. The results are metrologically comparable and compatible to the certified values. The measurement uncertainties are comparable to those obtained by the more complex and expensive technique, isotope dilution mass spectrometry. KW - Lithium KW - Human serum KW - Isotope dilution KW - Atomic absorption spectrometry KW - High-resolution continuum source graphite furnace atomic absorption spectrometry PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532446 DO - https://doi.org/10.1007/s00216-021-03636-6 VL - 414 IS - 1 SP - 251 EP - 256 PB - Springer CY - Berlin AN - OPUS4-53244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Applications of atomic absorption spectrometry for lithium isotope analysis N2 - An alternative method for lithium isotope analysis by using high-resolution atomic absorption spectrometry (HR-CS-AAS) is proposed herein. This method is based on monitoring the isotope shift of approximately 15 pm for the electronic transition 22P←22S at around the wavelength of 670.8 nm, which can be measured by state-of-the-art HR-CS-AAS. Isotope analysis can be used for (i) the traceable determination of Li concentration and (ii) isotope amount ratio analysis based on a combination of HR-CS-AAS and spectral data analysis by machine learning (ML). In the first case, the Li spectra are described as the linear superposition of the contributions of the respective isotopes, each consisting of a spin-orbit doublet, which can be expressed as Gaussian components with constant spectral position and width and different relative intensity, reflecting the isotope ratio in the sample. Precision was further improved by using lanthanum as internal spectral standard. The procedure has been validated using human serum-certified reference materials. The results are metrologically comparable and compatible with the certified values. In the second case, for isotope amount ratio analysis, a scalable tree boosting ML algorithm (XGBoost) was employed and calibrated using a set of samples with 6Li isotope amount fractions ranging from 0.06 to 0.99 mol mol−1. The training ML model was validated with certified reference materials. The procedure was applied to the isotope amount ratio determination of a set of stock chemicals and a BAM candidate reference material NMC111 (LiNi1/3Mn1/3Co1/3O2), a Li-battery cathode material. These determinations were compared with those obtained by MC-ICP-MS and found to be metrologically comparable and compatible. The residual bias was −1.8‰, and the precision obtained ranged from 1.9‰ to 6.2‰. This precision was sufficient to resolve naturally occurring variations. The NMC111 cathode candidate reference material was analyzed using high-resolution continuum source atomic absorption spectrometry with and without matrix purification to assess its suitability for technical applications. The results obtained were metrologically compatible with each other. T2 - Colloquium Spectroscopicum Internationale XLII (CSI XLII) CY - Gijón, Spain DA - 30.05.2022 KW - Lithium KW - HR-CS-AAS KW - Chemometrics KW - Atomic spectrometry PY - 2022 AN - OPUS4-56498 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -