TY - CONF A1 - Zientek, Nicolai A1 - Meyer, Klas A1 - Panne, Ulrich A1 - Kraume, M. A1 - Maiwald, Michael T1 - Untersuchung der Auflösungskinetik von pharmazeutischen Cokristallen mittels Onlilne-NMR-Spektroskopie N2 - Bei der Entwicklung pharmazeutischer Wirkstoffe werfen Substanzen mit einer geringen Löslichkeit, Auflösungsrate und damit einhergehend schlechten Bioverfügbarkeit immer größere Probleme auf. Diese Eigenschaften und nicht etwa toxikologische Eigenschaften oder schlechte Wirksamkeit sorgen dafür, dass es weniger als 1 % aller Wirkstoffe bis in die Markteinführung schaffen. Eine Reihe von Ansätzen zur Verbesserung der schlechten Wasserlöslichkeit konnten bereits etabliert werden. Hierunter zählen die gezielte Salzbildung bzw. Salzscreening, Solubilisierung mit Cosolventien oder die Nutzung von Polymeren als mögliche Transportwege. Eine weitere Möglichkeit bietet die Bildung verschiedener polymorpher Formen, sowohl der Einzelkomponente als auch von den verschiedenen Mehrkomponentenverbindungen. T2 - 7. Interdisziplinäres Doktorandenseminar CY - Berlin, Germany DA - 24.02.2013 KW - Quantitative Online-NMR-Spektroskopie KW - Pharmazeutische Cokristalle PY - 2013 SN - 978-3-9815360-9-6 SP - 9 EP - 11 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) AN - OPUS4-28266 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhu, Shengchao A1 - Panne, Ulrich A1 - Rurack, Knut T1 - A rapid method for the assessment of the surface group density of carboxylic acid-functionalized polystyrene microparticles N2 - Particle-based assays are becoming versatile analytical tools due to their cost-effectiveness, speed, straightforward and diverse functionalization chemistries, especially when polystyrene particles are used. The introduction of functional groups (–COOH, –NH2, etc.) to the surface of such polystyrene particles promotes their application in bioanalytics. However, the traditional method to determine the amount of surface carboxylate groups is conductivity titration, which is usually time- and resources-consuming and discontinuous. Here, we synthesized polystyrene microparticles with different contents of carboxylate groups, and then investigated a simpler and potentially continuous approach to determine the amount of surface carboxylate groups by Zeta potential measurements. The results were compared to the traditional titration method and to actual coupling efficiencies of the functionalized particles with a model oligonucleotide probe as determined by flow cytometry. All quantification methods revealed good agreement. KW - Konduktometrische Titration KW - Mikropartikel KW - Oberflächenfunktionalisierung KW - Polystyrol KW - Zeta-Potential PY - 2013 DO - https://doi.org/10.1039/c3an36578f SN - 0003-2654 SN - 1364-5528 VL - 138 IS - 10 SP - 2924 EP - 2930 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-28660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Zengchao A1 - Nirmalananthan-Budau, Nithiya A1 - Resch-Genger, Ute A1 - Panne, Ulrich A1 - Weidner, Steffen T1 - Separation of polystyrene nanoparticles bearing different carboxyl group densities and functional groups quantification with capillary electrophoresis and asymmetrical flow field flow fractionation N2 - Two sets of polystyrene nanoparticles (PSNPs) with comparable core sizes but different carboxyl group densities were made and separated using asymmetric flow field flow fractionation (AF4), capillary electrophoresis (CE), and the off-line hyphenation of both methods. Our results revealed the significant potential of two-dimensional off-line AF4-CE hyphenation to improve the separation and demonstrated for the first time, the applicability of CE to determine the functional group density of nanoparticles (NPs). Compared to the result acquired with conductometric titration, the result obtained with synthesized 100 nm sized PSNPs revealed only a slight deviation of 1.7%. Commercial 100 nm sized PSNPs yielded a deviation of 4.6 %. For 60 nm sized PSNPs, a larger deviation of 10.6 % between both methods was observed, which is attributed to the lower separation resolution. KW - Nanoparticle KW - A4F KW - Capillary electrophoresis KW - Carboxyl group PY - 2020 DO - https://doi.org/10.1016/j.chroma.2020.461392 VL - 1626 SP - 461392 PB - Elsevier B.V. AN - OPUS4-51080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Zengchao A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Weidner, Steffen T1 - Separation of polystyrene nanoparticles with different coatings using two-dimensional off-line coupling of asymmetrical flow field flow fractionation and capillary electrophoresis N2 - The successful off-line coupling of asymmetrical flow field flow fractionation (AF4) and capillary electrophoresis (CE) for separation of nanoparticles (NPs) with different surface coatings was shown. We could successfully demonstrate that, in a certain NP size range, hyphenation of both techniques significantly improved the separation of differently coated NPs. Three mixtures of polystyrene nanoparticles (PS-NPs) with comparable core sizes but different coatings (no coating/carboxyl-coated) were studied. Separation in either method resulted in non-baseline resolved or non-separated peaks. In contrast, two-dimensional off-line coupling of AF4 and CE resulted in clearly separated regions in their 2 D plots in case of 20 and 50 nm particle mixtures, whereas the 100 nm NP mixture could not be separated at all. Various factors affecting the separation like hydrodynamic diameter or SDS concentration were discussed. KW - Capillary electrophoresis (CE) KW - Nanoparticles with same nominal diameter KW - Surface coating KW - Two-dimensional off-line coupling KW - Asymmetrical flow field flow fractionation (AF4) PY - 2019 DO - https://doi.org/10.1016/j.chroma.2019.01.056 VL - 1593 SP - 119 EP - 126 PB - Elsevier AN - OPUS4-47363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - González, M.G. A1 - Niessner, R. A1 - Panne, Ulrich A1 - Haisch, C. A1 - Resch-Genger, Ute T1 - Determination of the absolute fluorescence quantum yield of rhodamine 6G with optical and photoacoustic methods - providing the basis for fluorescence quantum yield standards N2 - To establish the methodical basis for the development and certification of fluorescence quantum yield standards, we determined the fluorescence quantum yield Φf of rhodamine 6G (R6G) with two absolute methods with complementary measurement principles, here optical spectroscopy using an integrating sphere setup and pulsed laser photoacoustic spectroscopy (PAS). For the assessment of aggregation- and reabsorption-induced distortions of measured fluorescence quantum yields and procedures for the reliable consideration of such effects, this systematic comparison was performed in ethanol and in water employing different concentrations of R6G. In addition, the relative and absolute fluorescence quantum yields of these solutions were obtained with a calibrated spectrofluorometer and a commercialized integrating sphere setup. Based upon this systematic comparison, experimental advantages and systematic sources of variation were identified for both methods. KW - Fluorescence KW - Photoluminescence KW - Quantum yield KW - Photoacoustic spectroscopy KW - Absolute quantum yield KW - Integrating sphere KW - Rhodamine 6G KW - Aggregation KW - Reabsorption PY - 2012 DO - https://doi.org/10.1016/j.talanta.2011.12.051 SN - 0039-9140 VL - 90 SP - 30 EP - 37 PB - Elsevier CY - Amsterdam AN - OPUS4-25710 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wooley, A. T. A1 - Cárdenas, S. A1 - Cavazzini, A. A1 - Panne, Ulrich T1 - Meet the three newest ABC Editors N2 - Editorial - Introduction of the new editors. KW - ABC PY - 2023 DO - https://doi.org/10.1007/s00216-023-04615-9 SP - 1 EP - 3 PB - Springer Verlag GmbH CY - Germany AN - OPUS4-57188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolf, S. E. A1 - Müller, L. A1 - Barrea, R. A1 - Kampf, C.J. A1 - Leiterer, Jork A1 - Panne, Ulrich A1 - Hoffmann, T. A1 - Emmerling, Franziska A1 - Tremel, W. T1 - Carbonate-coordinated metal complexes precede the formation of liquid amorphous mineral emulsions of divalent metal carbonates N2 - During the mineralisation of metal carbonates MCO3 (M = Ca, Sr, Ba, Mn, Cd, Pb) liquid-like amorphous intermediates emerge. These intermediates that form via a liquid/liquid phase separation behave like a classical emulsion and are stabilized electrostatically. The occurrence of these intermediates is attributed to the formation of highly hydrated networks whose stability is mainly based on weak interactions and the variability of the metal-containing pre-critical clusters. Their existence and compositional freedom are evidenced by electrospray ionization mass spectrometry (ESI-MS). Liquid intermediates in non-classical crystallisation pathways seem to be more common than assumed. PY - 2011 DO - https://doi.org/10.1039/c0nr00761g SN - 2040-3364 SN - 2040-3372 IS - 3 SP - 1158 EP - 1165 PB - RSC Publ. CY - Cambridge AN - OPUS4-23355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winckelmann, Alexander A1 - Nowak, S. A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Riedel, Jens A1 - Vogl, Jochen A1 - Panne, Ulrich A1 - Abad Andrade, Carlos Enrique T1 - High-Resolution Atomic Absorption Spectrometry Combined With Machine Learning Data Processing for Isotope Amount Ratio Analysis of Lithium N2 - An alternative method for lithium isotope amount ratio analysis based on a combination of high-resolution atomic absorption spectrometry and spectral data analysis by machine learning (ML) is proposed herein. It is based on the well-known 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 the state-of-the-art high-resolution continuum source graphite furnace atomic absorption spectrometry. 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, previously determined by a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS). The calibration ML model was validated with two certified reference materials (LSVEC and IRMM-016). The procedure was applied toward the isotope amount ratio determination of a set of stock chemicals (Li2CO3, LiNO3, LiCl, and LiOH) and a BAM candidate reference material NMC111 (LiNi1/3Mn1/3Co1/3O2), a Li-battery cathode material. The results of 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, as demonstrated for samples ranging from approximately −3 to +15‰. To assess its suitability to technical applications, the NMC111 cathode candidate reference material was analyzed using high-resolution continuum source atomic absorption spectrometry with and without matrix purification. The results obtained were metrologically compatible with each other. KW - Lithium KW - Isotope KW - Machine learning KW - Algorithms KW - Reference material KW - AAS KW - Atomic Absorption Spectrometry PY - 2021 DO - https://doi.org/10.1021/acs.analchem.1c00206 SN - 1520-6882 VL - 93 IS - 29 SP - 10022 EP - 10030 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-53028 LA - eng 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 - JOUR A1 - Wienold, Julia A1 - Traub, Heike A1 - Lange, Britta A1 - Giray, Thorsten A1 - Recknagel, Sebastian A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Elemental analysis of copper and magnesium alloy samples using IR-laser ablation in comparison with spark and glow discharge methods N2 - Three methods for direct solid sampling of bulk material namely IR laser ablation, glow discharge and spark OES, were compared with respect to analytical figures of merit obtained for elemental analysis with atomic spectrometry. Matrices investigated were copper, pressed doped copper powder, and magnesium alloys. For the vast majority of analytes, statistical equivalence regarding precision (usually ≤ 5%) and the performance of the calibrations between the compared methods was demonstrated. KW - LA-ICP-MS KW - GD-MS KW - Spark-OES KW - LA-ICP-OES KW - Copper KW - Magnesium PY - 2009 DO - https://doi.org/10.1039/b903251g SN - 0267-9477 SN - 1364-5544 VL - 24 SP - 1570 EP - 1574 PB - Royal Society of Chemistry CY - London AN - OPUS4-20257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Knappe, Patrick A1 - Panne, Ulrich T1 - MALDI-TOF imaging mass spectrometry of artifacts in 'dried droplet' polymer samples N2 - Matrix-assisted laser desorption/ionization-timeof-flight (MALDI-TOF) imaging of polystyrenes with various molecular masses was applied to study spatial molecular mass distribution of polymers in sample spots prepared by the 'dried droplet' method. When different solvents and target surfaces were examined, a segregation of single homologous polymers was observed depending upon the evaporation rate of the solvent. For the observed Patterns left by the evaporating droplet, a hypothesis is offered taking into account different hydrodynamic interactions and diffusion. The results illustrate that spot preparation using the conventionally 'dried droplet' method is prone to artifacts and should be avoided for reliable and reproducible MALDI mass spectrometry experiments with regards to the Determination of molecular masses and mass distributions. KW - MALDI KW - Mass spectrometry imaging KW - Polymer KW - Droplet PY - 2011 DO - https://doi.org/10.1007/s00216-011-4773-1 SN - 1618-2642 SN - 1618-2650 VL - 401 IS - 1 SP - 127 EP - 134 PB - Springer CY - Berlin AN - OPUS4-24538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Warschat, Carsten A1 - Stindt, Arne A1 - Panne, Ulrich A1 - Riedel, Jens T1 - Mass spectrometry of levitated droplets by thermally unconfined infrared-laser desorption N2 - An ionization scheme for fast online mass spectrometric interrogation of levitated droplets is presented. That renewed method comprises the output of an a Er:YAG laser at λ = 2.94 µm which is in resonance with the OH stretch vibration band of solvents like water and alcohols. A temporal pulse width larger than the time needed for pressure redistribution and also above the temperature redistribution time constant was found to lead to soft evaporation/ionization. Despite these mild desorption conditions, no additional postionization is found to be needed. Accordingly, the ionization is found to be very soft resulting in entirely intact analyte ions and concentration dependent cluster ions. Resulting mass spectra of small amino acids and large antibiotics are presented showing the versatility of the introduced technique. Above a critical mass of m ≈ 1 kDa, the formed ions carry multiple charges as it is typical for thermospray or electrospray ionization. The detection technique enables fast contactless analysis of the chemical composition of levitated microreactors and, thus, paves the way for future contactless reaction monitoring. KW - Laser desorption ionization KW - Levitated droplets KW - Ambient mass spectrometry PY - 2015 DO - https://doi.org/10.1021/acs.analchem.5b01495 SN - 0003-2700 SN - 1520-6882 VL - 87 IS - 16 SP - 8323 EP - 8327 PB - American Chemical Society CY - Washington, DC AN - OPUS4-35134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Walter, Astrid A1 - Pfeifer, Dietmar A1 - Kraus, Werner A1 - Emmerling, Franziska A1 - Schneider, Rudolf A1 - Panne, Ulrich A1 - Weller, Michael G. T1 - Triacetone Triperoxide (TATP): Hapten design and development of antibodies N2 - Triacetone triperoxide (TATP), an improvised explosive, is a potential security threat because of its cost-efficient synthesis and the difficulty in detecting it. A highly selective antibody could provide the necessary specificity to the detection process. To obtain antibodies, a hapten made from acetone, hydrogen peroxide, and 7-oxooctanoic acid has been designed, synthesized, and confirmed by NMR that displays the utmost similarity to the analyte. The single-crystal X-ray structures of the solvated species TATP·methanol (1:1) and the TATP derivate were determined. In both compounds, the molecules exhibit D3 symmetry and adopt a twisted boat-chair conformation. The hapten was coupled to bovine serum albumin, and mice were immunized. An immune response against TATP was elicited, and selective antibodies were detected in the mouse serum, which should be very useful for the development of a TATP biosensor system. An ELISA with a limit of detection for TATP of 65 µg L-1 is shown. KW - TATP KW - Triacetone triperoxide KW - Explosive KW - Antibody KW - Hapten immunoassay KW - Structure PY - 2010 DO - https://doi.org/10.1021/la1018339 SN - 0743-7463 SN - 1520-5827 VL - 26 IS - 19 SP - 15418 EP - 15423 PB - American Chemical Society CY - Washington, DC AN - OPUS4-22469 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Walter, Astrid A1 - Panne, Ulrich A1 - Weller, Michael G. T1 - A novel immunoreagent for the specific and sensitive detection of the explosive triacetone triperoxide (TATP) N2 - Triacetone triperoxide (TATP) is a primary explosive, which was used in various terrorist attacks in the past. For the development of biosensors, immunochemical µ-TAS, electronic noses, immunological test kits, or test strips, the availability of antibodies of high quality is crucial. Recently, we presented the successful immunization of mice, based on the design, synthesis, and conjugation of a novel TATP derivative. Here, the long-term immunization of rabbits is shown, which resulted in antibodies of extreme selectivity and more than 1,000 times better affinity in relation to the antibodies from mice. Detection limits below 10 ng L-1 (water) were achieved. The working range covers more than four decades, calculated from a precision profile. The cross-reactivity tests revealed an extraordinary selectivity of the antibodies—not a single compound could be identified as a relevant cross-reactant. The presented immunoreagent might be a major step for the development of highly sensitive and selective TATP detectors particularly for security applications. KW - Organic peroxides KW - Terrorism KW - Biosensor development PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-240291 UR - http://www.mdpi.com/2079-6374/1/3/93 DO - https://doi.org/10.3390/bios1030093 SN - 2079-6374 VL - 1 IS - 3 SP - 93 EP - 106 PB - MDPI CY - Basel AN - OPUS4-24029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traub, Heike A1 - Wälle, M. A1 - Koch, J. A1 - Panne, Ulrich A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Günther, D. T1 - Evaluation of different calibration strategies for the analysis of pure copper and zinc samples using femtosecond laser ablation ICP-MS N2 - Solution-doped metal powder pellets as well as aspirated liquids were used as calibration samples to analyze pure copper and zinc certified reference materials (CRMs) by femtosecond laser ablation ICP-MS. It was demonstrated that calibration by copper pellets resulted in relative deviations up to 20%, whereas fs-LA-ICP-MS among copper-based CRMs led to inaccuracies in the same range unless nominal mass fractions were chosen to be <3 mg/kg. Calibration by zinc pellets generally provided better accuracy. Depending on the analyte considered, deviations below 10% were obtained even for mass fractions close to the limit of quantification. Our data, therefore, indicate solution-doped metal powder pellets to be suitable as calibration samples for fs-LA-ICP-MS of metals. Furthermore, the utilization of liquid standards for calibration was found to result in stronger deviations of up to 50% for both copper and zinc samples which, in addition, turned out to be dependent on the plasma conditions. KW - Laser ablation KW - ICP-MS KW - Calibration KW - Copper KW - Zinc KW - Metal PY - 2009 DO - https://doi.org/10.1007/s00216-009-3061-9 SN - 1618-2642 SN - 1618-2650 VL - 395 IS - 5 SP - 1471 EP - 1480 PB - Springer CY - Berlin AN - OPUS4-20402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traub, Heike A1 - Czerwensky, Michael A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Panne, Ulrich T1 - Homogenitätsprüfung und Analyse von reinem Kupfer mit Laserablation-ICP-Massenspektrometrie KW - Laserablation KW - Kupfer KW - Homogenität KW - ZRM PY - 2007 SN - 0026-0746 VL - 61 IS - 11 SP - 744 EP - 745 PB - Giesel Verlag GmbH CY - Isernhagen AN - OPUS4-16153 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traub, Heike A1 - Czerwensky, Michael A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Panne, Ulrich T1 - Different calibration strategies for the analysis of pure copper metal by nanosecond laser ablation inductively coupled plasma mass spectrometry N2 - In this work, different calibration strategies for the determination of trace elements in pure copper metal by nanosecond laser ablation ICP-MS were investigated. In addition to certified reference materials (CRMs), pellets of doped copper powder were used for calibration. The micro homogeneity of the CRMs as well as the solution-doped pellets was sufficient to use them as calibration samples in combination with a laser spot size of 200 µm. In contrast, pellets doped with analytes in solid form showed a significant heterogeneity. For most of the investigated analytes and copper CRMs the measured mass fractions were within ± 20% of their certified values when other copper CRMs were used as calibration samples. When solution-doped powder pellets were used as calibration samples a systematic trend towards mass fractions below the certified values was observed for nearly all elements determined in the analysed CRMs. Thermal fractionation effects during the ablation of the solution-doped pellets were suspected as the extent of the fractionation depends on the irradiance, whereas fractionation is reduced at higher irradiance. PY - 2010 DO - https://doi.org/10.1039/b915564c SN - 0267-9477 SN - 1364-5544 VL - 25 IS - 5 SP - 690 EP - 696 PB - Royal Society of Chemistry CY - London AN - OPUS4-21195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tognoni, E. A1 - Cristoforetti, G. A1 - Legnaioli, S. A1 - Palleschi, V. A1 - Salvetti, A. A1 - Müller, Maike A1 - Panne, Ulrich A1 - Gomushkin, I. T1 - A numerical study of expected accuracy and precision in Calibration-Free Laser-Induced Breakdown Spectroscopy in the assumption of ideal analytical plasma N2 - Calibration-Free Laser-Induced Breakdown Spectroscopy (CF-LIBS) has been proposed several years ago as an approach for quantitative analysis of Laser-Induced Breakdown Spectroscopy spectra. Recently developed refinement of the spectral processing method is described in the present work. Accurate quantitative results have been demonstrated for several metallic alloys. However, the degree of accuracy that can be achieved with Calibration-Free Laser-Induced Breakdown Spectroscopy analysis of generic samples still needs to be thoroughly investigated. The authors have undertaken a systematic study of errors and biasing factors affecting the calculation in the Calibration-Free Laser-Induced Breakdown Spectroscopy spectra processing. These factors may be classified in three main groups: 1) experimental aberrations (intensity fluctuations and inaccuracy in the correction for spectral efficiency of a detection system), 2) inaccuracy in theoretical parameters used for calculations (Stark broadening coefficients and partition functions) and 3) plasma non-ideality (departure from thermal equilibrium, spatial and temporal inhomogeneities, optical thickness, etc.). In this study, the effects of experimental aberrations and accuracy of spectral data were investigated, assuming that the analytical plasma is ideal. Departure of the plasma conditions from ideality will be the object of future work. The current study was based on numerical simulation. Two kinds of metallic alloys, iron-based and aluminum-based, were studied. The relative weight of the error contributions was found to depend on the sample composition. For the here-investigated samples, the experimental aberrations contribute to the overall uncertainty on the quantitative results more than theoretical parameters. The described simulation method can be applied to the Calibration-Free Laser-Induced Breakdown Spectroscopy analysis of any other kind of sample. KW - LIBS KW - Quantitative analysis KW - Standard-less analysis KW - Accuracy KW - Precision PY - 2007 DO - https://doi.org/10.1016/j.sab.2007.10.005 SN - 0584-8547 SN - 0038-6987 VL - 62 IS - 12 SP - 1287 EP - 1302 PB - Elsevier CY - Amsterdam AN - OPUS4-16566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sötebier, Carina A1 - Weidner, Steffen A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Bettmer, J. T1 - Separation and quantification of silver nanoparticles and silver ions using reversed phase high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry in combination with isotope dilution analysis N2 - A reversed phase high performance liquid chromatography coupled to an inductively coupled plasma mass spectrometer (HPLC-ICP-MS) approach in combination with isotope dilution analysis (IDA) for the separation and parallel quantification of nanostructured and ionic silver (Ag) is presented. The main focus of this work was the determination of the ionic Ag concentration. For a sufficient stabilization of the ions without dissolving the nanoparticles (NPs), the eluent had to be initially optimized. The determined Ag ion concentration was in a good agreement with results obtained using ultrafiltration. Further, the mechanism of the NP separation in the HPLC column was investigated. Typical size exclusion effects were found by comparing results from columns with different pore sizes. Since the recovery rates decreased with increasing Ag NP size and large Ag NPs did not elute from the column, additional interactions of the particles with the stationary phase were assumed. Our results reveal that the presented method is not only applicable to Ag NPs, but also to gold and polystyrene NPs. Finally, IDA-HPLC-ICP-MS experiments in single particle mode were performed to determine the particle cut-off size. The comparison with conventional spICP-MS experiments resulted in a similar diameter and particle size distribution. KW - ICP-MS KW - Silver nanoparticles KW - HPLC KW - Isotope dilution analysis KW - Field flow fractionation KW - Toxicology PY - 2016 DO - https://doi.org/10.1016/j.chroma.2016.09.028 SN - 0021-9673 VL - 1468 SP - 102 EP - 108 PB - Elsevier B.V. AN - OPUS4-38642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sötebier, Carina A1 - Bierkandt, Frank A1 - Rades, Steffi A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Weidner, Steffen T1 - Sample loss in asymmetric flow field-flow fractionation coupled to inductively coupled plasma-mass spectrometry of silver nanoparticles N2 - In this work, sample losses of silver nanoparticles (Ag NPs) in asymmetrical flow field-flow fractionation (AF4) have been systematically investigated with the main focus on instrumental conditions like focusing and cross-flow parameters as well as sample concentration and buffer composition. Special attention was drawn to the AF4 membrane. For monitoring possible silver depositions on the membrane, imaging laser ablation coupled to inductively coupled plasma mass spectrometry (LA-ICP-MS) was used. Our results show that the sample residue on the membrane was below 0.6% of the total injected amount and therefore could be almost completely avoided at low sample concentrations and optimized conditions. By investigation of the AF4 flows using inductively coupled plasma mass spectrometry (ICP-MS), we found the recovery rate in the detector flow under optimized conditions to be nearly 90%, while the cross-flow, slot-outlet flow and purge flow showed negligible amounts of under 0.5%. The analysis of an aqueous ionic Ag standard solution resulted in recovery rates of over 6% and the ionic Ag content in the sample was found to be nearly 8%. Therefore, we were able to indicate the ionic Ag content as the most important source of sample loss in this study. KW - Asymmetric flow filed-flow fractionation KW - ICP-MS KW - Nanoparticles KW - Sample loss KW - Quantification PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-336171 DO - https://doi.org/10.1039/c5ja00297d SN - 0267-9477 SN - 1364-5544 VL - 30 IS - 10 SP - 2214 EP - 2222 PB - Royal Society of Chemistry CY - London AN - OPUS4-33617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sötebier, Carina A. A1 - Weidner, Steffen A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Bettmer, J. T1 - Separation and quantification of silver nanoparticles and silver ions using reversed phase high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry in combination with isotope dilution analysis N2 - A reversed phase high performance liquid chromatography coupled to an inductively coupled Plasma mass spectrometer (HPLC–ICP-MS) approach in combination with isotope dilution analysis (IDA) for the separation and parallel quantification of nanostructured and ionic silver (Ag) is presented. The main Focus of this work was the determination of the ionic Ag concentration. For a sufficient stabilization of the Ions without dissolving the nanoparticles (NPs), the eluent had to be initially optimized. The determined Ag ion concentration was in a good agreement with results obtained using ultrafiltration. Further, the mechanism of the NP separation in the HPLC column was investigated. Typical size exclusion effects were found by comparing results from columns with different pore sizes. Since the recovery rates decreased with increasing Ag NP size and large Ag NPs did not elute from the column, additional interactions of the particles with the stationary phase were assumed. Our results reveal that the presented method is not only applicable to Ag NPs, but also to gold and polystyrene NPs. Finally, IDA-HPLC-ICP-MS experiments in single particle mode were performed to determine the particle cut-off size. The comparison with conventional spICP-MS experiments resulted in a similar diameter and particle size distribution. KW - ICP-MS KW - Silver nanoparticles KW - Speciation KW - High performance liquid chromatography KW - Isotope dilution analysis PY - 2016 DO - https://doi.org/10.1016/j.chroma.2016.09.028 SN - 0021-9673 VL - 1468 SP - 102 EP - 108 AN - OPUS4-37652 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sötebier, Carina A. A1 - Kutscher, D. J. A1 - Rottmann, L. A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Bettmer, J. T1 - Combination of single particle ICP-QMS and isotope dilution analysis for the determination of size, particle number and number size distribution of silver nanoparticles N2 - Single particle ICP-MS (spICP-MS) has gained great influence in the analysis of engineered nanoparticles (NPs) due to its simplicity, speed and ability to obtain a particle number size distribution. Despite its many advantages, the method is hampered by matrix effects affecting the sensitivity of the instruments. Consequently, over- or underestimated particle sizes might be obtained. To overcome these challenges, we present in this work the detection of both Ag isotopes with a quadrupole mass spectrometer for the application of isotopic dilution analysis (IDA) in combination with spICP-MS. Here, the isotopes are measured sequentially using the conventional spICP-MS integration time of 10 ms. Citrate stabilized Ag NPs of a spherical shape with the nominal diameters of 30, 40, 50 and 80 nm have been investigated. The experimental concept of adding ¹⁰⁹Ag+ solutions to the NP suspensions resulted in the NP Spikes being only visible in the ¹⁰⁷Ag trace. Therefore, a maximum of 45% of the particles was detected compared to that by conventional spICP-MS. A modified mass flow equation was applied to determine the particle sizes, particle size distributions and particle number concentrations of various Ag NPs. The addition of different spike concentrations between 0.5 and 4 mg L⁻¹ ¹⁰⁹Ag resulted in similar particle diameters, suggesting that the calculated diameter might be independent of the spike concentration. This would have the advantage that no size information would be needed before the analysis. By analyzing Ag NP suspensions in a simulated seawater matrix, we demonstrate its significant influence on the particle size determination using conventional spICP-MS. A lower transport efficiency of 6.1% was found in the matrix compared to 7.3% without the matrix. In our approach, the addition of the Matrix influenced the NP intensity stronger than the spike signal, resulting in slightly smaller diameters using IDA–spICP-MS with the matrix compared to the results without the matrix. On the other hand, the IDA–spICP-MS approach with the matrix can result in equivalent results for the particle sizes compared with conventional spICP-MS using suspensions without the matrix. Due to the lower instrument sensitivity in the matrix, a diameter of 30 nm was found to be close to the detection limit of the instrument. KW - Ag nanoparticles KW - Single particle ICP-MS KW - Matrix influence KW - Isotope dilution analysis PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-376490 DO - https://doi.org/10.1039/c6ja00137h SN - 0267-9477 VL - 31 IS - 10 SP - 2045 EP - 2052 AN - OPUS4-37649 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stindt, Arne A1 - Warschat, Carsten A1 - Bierstedt, Andreas A1 - Panne, Ulrich A1 - Riedel, Jens T1 - Characterisation of an inexpensive sonic spray ionisation source using laser induced fluorescence imaging and mass spectrometry N2 - A commercially available airbrush gun as a new source for spray ionization is presented. It is best operated employing moderate stagnation pressures, resulting in a sonic gas flow. A mass spectrometric investigation on the amino acid lysine and several peptides reveals that this inexpensive approach results in reproducible mass spectra. The ion patterns strongly resemble the results from other studies obtained with custom made sonic spray vaporizers. The patterns as well resemble the mass spectra recorded with electrospray devices. For a better understanding of the vaporization process, the mass spectrometry experiments are accompanied by laser induced fluorescence experiments. Inverse Abel transform of the obtained fluorescence maps allows the determination of the full 3D distribution of the spray cone. Furthermore, via exploitation of the solvatochromism of the used dye the solvation state distribution can be visualized. In addition, expansion parameters like droplet size and velocity are obtained by laser stroboscopy. The experiments demonstrate that the analyte is hardly desolvated throughout the expansion. This indicates a subsequent vaporization of the residual solvent in the intermediate pressure region of the mass spectrometer. KW - Sonic spray ionization KW - Mass spectrometry KW - Solvatochromism KW - Inverse Abel Transform KW - Sonic spray KW - Airbrush KW - Laser induced fluorescence PY - 2014 DO - https://doi.org/10.1255/ejms.1242 SN - 1469-0667 SN - 1356-1049 SN - 1365-0718 VL - 20 IS - 1 SP - 21 EP - 29 PB - IM Publications CY - Chichester AN - OPUS4-30403 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stindt, Arne A1 - Buurman, Merwe A1 - Panne, Ulrich A1 - Riedel, Jens T1 - CO2 laser ionization of acoustically levitated droplets N2 - For many analytical purposes, direct laser ionization of liquids is desirable. Several studies on supported droplets, free liquid jets, and ballistically dispensed microdroplets have been conducted, yet detailed knowledge of the underlying mechanistics in ion formation is still missing. This contribution introduces a simple combination of IR-MALDI mass spectrometry and an acoustical levitation device for contactless confinement of the liquid sample. The homebuilt ultrasonic levitator supports droplets of several millimeters in diameter. These droplets are vaporized by a carbon dioxide laser in the vicinity of the atmospheric pressure interface of a time of flight mass spectrometer. The evaporation process is studied by high repetition rate shadowgraphy experiments elucidating the ballistic evaporation of the sample and revealing strong confinement of the vapor by the ultrasonic field of the trap. Finally, typical mass spectra for pure glycerol/water matrix and lysine as an analyte are presented with and without the addition of trifluoracetic acid, and the ionization mechanism is briefly discussed. The technique is a promising candidate for a reproducible mass spectrometric detection scheme for the field of microfluidics. KW - Ambient mass spectrometry KW - Levitated droplets KW - IR-MALDI PY - 2012 UR - http://link.springer.com/content/pdf/10.1007%2Fs00216-012-6500-y DO - https://doi.org/10.1007/s00216-012-6500-y SN - 1618-2642 SN - 1618-2650 N1 - Geburtsname von Buurman, Merwe: Albrecht, M. - Birth name of Buurman, Merwe: Albrecht, M. SP - 1 EP - 6(?) PB - Springer CY - Berlin AN - OPUS4-27429 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stindt, Arne A1 - Andrade, M. A. B. A1 - Buurman, Merwe A1 - Adamowski, J. C. A1 - Panne, Ulrich A1 - Riedel, Jens T1 - Experimental and numerical characterization of the sound pressure in standing wave acoustic levitators N2 - A novel method for predictions of the sound pressure distribution in acoustic levitators is based on a matrix representation of the Rayleigh integral. This method allows for a fast calculation of the acoustic field within the resonator. To make sure that the underlying assumptions and simplifications are justified, this approach was tested by a direct comparison to experimental data. The experimental sound pressure distributions were recorded by high spatially resolved frequency selective microphone scanning. To emphasize the general applicability of the two approaches, the comparative studies were conducted for four different resonator geometries. In all cases, the results show an excellent agreement, demonstrating the accuracy of the matrix method. KW - Acoustic levitation KW - Matrix calculation KW - Microphony KW - Noncontact ultrasonic transportation KW - Small objects KW - Matrix-method KW - Droplets KW - Air KW - Manipulation KW - Simulation KW - Fields KW - Water PY - 2014 DO - https://doi.org/10.1063/1.4861197 SN - 0034-6748 SN - 1089-7623 N1 - Geburtsname von Buurman, Merwe: Albrecht, M. - Birth name of Buurman, Merwe: Albrecht, M. VL - 85 IS - 015110 SP - 1 EP - 6 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-30405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shigeta, K. A1 - Traub, Heike A1 - Panne, Ulrich A1 - Okino, A. A1 - Rottmann, L. A1 - Jakubowski, Norbert T1 - Application of a micro-droplet generator for an ICP-sector field mass spectrometer - optimization and analytical characterization N2 - A micro-droplet generator (µDG) sample introduction system was coupled to a sector field ICP-MS instrument to investigate the analytical figures of merit with respect to single cell analysis. The sector field instrument was operated for the first time in a fast scanning mode (E-scan) with the shortest time resolution of 100 µs to measure the single droplet time resolved and using the original detector in a pulse counting mode without modification of the existing electronics. For reduction of the droplet diameter a triple pulse mode of the droplet generator was applied and a droplet diameter down to 23 µm has been achieved for this investigation with a 100% transport efficiency of droplets. Signal duration times of single droplets of less than 500 µs have been measured. Overall detection efficiencies in the range of 10-3 counts per atom have been achieved and absolute limits of detection range between 120 ag for Fe and 1.1 ag for Mg as a mean value from 1000 droplet events. PY - 2013 DO - https://doi.org/10.1039/c2ja30207a SN - 0267-9477 SN - 1364-5544 VL - 28 IS - 5 SP - 646 EP - 656 PB - Royal Society of Chemistry CY - London AN - OPUS4-29447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shigeta, K. A1 - Koellensperger, G. A1 - Rampler, E. A1 - Traub, Heike A1 - Rottmann, L. A1 - Panne, Ulrich A1 - Okino, A. A1 - Jakubowski, Norbert T1 - Sample introduction of single selenized yeast cells (Saccharomyces cerevisiae) by micro droplet generation into an ICP-sector field mass spectrometer for label-free detection of trace elements N2 - We have applied a micro droplet generator (µDG) for sample introduction of single selenized yeast cells into a sector field ICP-MS, which was operated in a fast scanning mode with sampling rates of up to 10 kHz, to measure single cells time resolved with 100 µs integration time. Selenized yeast cells have been used as a model system for preliminary investigation. The single cells to be measured have been embedded into droplets and it will be shown that the time duration of a single cell event always is about 400 to 500 µs, and thus comparable to the time duration of a droplet without a cell. A fixed droplet generation rate of 50 Hz produced equidistant signals in time of each droplet event and was advantageous to separate contribution from background and blank from the analytical signal. Open vessel digestion and a multielement analysis were performed with washed yeast cells and absolute amounts per single cell were determined for Na (0.91 fg), Mg (9.4 fg), Fe (5.9 fg), Cu (0.54 fg), Zn (1.2 fg) and Se (72 fg). Signal intensities from single cells have been measured for the elements Cu, Zn and Se, and histograms were calculated for about 1000 cell events. The mean elemental sensitivities measured here range from 0.7 counts per ag (Se) to 10 counts per ag (Zn) with RSD's from 49% (Zn) to 69% (Se) for about 1000 cell events. PY - 2013 DO - https://doi.org/10.1039/c3ja30370e SN - 0267-9477 SN - 1364-5544 VL - 28 IS - 5 SP - 637 EP - 645 PB - Royal Society of Chemistry CY - London AN - OPUS4-29448 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shelby, D. A1 - Merk, Sven A1 - Smith, B.W. A1 - Gornushkin, Igor B. A1 - Panne, Ulrich A1 - Omenetto, N. T1 - Temperature evaluation by simultaneous emission and saturated fluorescence measurements: A critical theoretical and experimental appraisal of the approach N2 - Temperature is one of the most important physical parameters of plasmas induced by a focused laser beam on solid targets, and its experimental evaluation has received considerable attention. An intriguing approach, first proposed by Kunze (H.-J. Kunze, Experimental check of local thermodynamic equilibrium in discharges, Appl. Opt., 25 (1986) 13–13.) as a check of the existence of local thermodynamic equilibrium, is based upon the simultaneous measurement of the thermal emission and the optically saturated fluorescence of the same selected atomic transition. The approach, whose appealing feature is that neither the calibration of the set-up nor the spontaneous radiative probability of the transitions is needed, has not yet been applied, to our knowledge, to analytical flames and plasmas. A critical discussion of the basic requirements for the application of the method, its advantages, and its experimental limitations, is therefore presented here. For our study, Ba+ transitions in a plasma formed by focusing a pulsed Nd:YAG laser (1064 nm) on a glass sample containing BaO are selected. At various delay times from the plasma initiation, a pulsed, excimer-pumped dye laser tuned at the center of two Ba transitions (6s ²S1/2 → 6p ²P°3/2; 455.403 nm and 6p ²P°1/2 → 6d ²S1/2; 452.493 nm) is used to enhance the populations of the excited levels (6p ²P°3/2 and 6d ²S1/2) above their thermal values. The measured ratio of the emission and direct line fluorescence signals observed at 614.171 nm (6p ²P°3/2 → 5d ²D5/2) and 489.997 nm (6d ²S1/2 → 6p ²P°3/2) is then related to the excitation temperature of the plasma. Our conclusion is that the approach, despite being indeed attractive and clever, does not seem to be easily applicable to flames and plasmas, in particular to transient and inhomogeneous plasmas such as those induced by lasers on solids. KW - Plasma temperature KW - Optically saturated fluorescence KW - Laser induced plasma KW - Barium ion emission KW - Emission/fluorescence ratio PY - 2013 DO - https://doi.org/10.1016/j.sab.2013.09.002 SN - 0584-8547 SN - 0038-6987 VL - 89 SP - 50 EP - 59 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-30436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Seifert, Stephan A1 - Weidner, Steffen A1 - Panne, Ulrich A1 - Kneipp, Janina T1 - Taxonomic relationship of pollen from MALDI TOF MS data using multivariate statistics N2 - Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) has been suggested as a promising tool for the investigation of pollen, but the usefulness of this approach for classification and identification of pollen species has to be proven by an application to samples of varying taxonomic relations. KW - MALDI mass spectrometry KW - Pollen KW - Multivariate statistics PY - 2015 DO - https://doi.org/10.1002/rcm.7207 SN - 0951-4198 SN - 1097-0231 VL - 29 SP - 1145 EP - 1154 PB - Wiley CY - Chichester AN - OPUS4-35296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulte, Franziska A1 - Panne, Ulrich A1 - Kneipp, Janina T1 - Molecular changes during pollen germination can be monitored by Raman microspectroscopy N2 - The processes associated with pollen germination were studied in vitro for two tree species, Salix caprea and Fraxinus excelsior under different nutrient conditions. The results provide evidence of changes in chemical composition of the pollen grains during germination. From the comparison of spectra of the pollen grain body and the growing pollen tube, it can be concluded that there are major chemical differences between these two morphological units. Comparison of germinated and ungerminated pollen grains reveals alterations in the metabolism. Composition of the germinating pollen grain and its morphological units depends on the plant species, but also on the nutrient conditions. The results suggest species-specific utilization of metabolite storage, and potential alterations of the pollen outer coat. Furthermore, discharge of molecules into the nutrient medium may depend on the nutrient conditions in the germination experiments. This has implications for further experiments on dynamic processes in pollen and related plant materials. KW - Pollen germination KW - Raman microspectroscopy KW - Imaging KW - Coumaric acid KW - Pollen tube KW - Sporopollenin PY - 2010 DO - https://doi.org/10.1002/jbio.201000031 SN - 1864-063X VL - 3 IS - 8-9 SP - 542 EP - 547 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-23211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulte, Franziska A1 - Mäder, J. A1 - Kroh, L.W. A1 - Panne, Ulrich A1 - Kneipp, Janina T1 - Characterization of pollen carotenoids with in situ and high-performance thin-layer chromatography supported resonant Raman spectroscopy N2 - Raman signatures of the carotenoid component are studied in individual pollen grains from different species of trees. The information is obtained as differences in the strong pre-resonant Raman spectra measured before and after photodepletion of the carotenoid molecules. The results provide the first in situ evidence of interspecies differences in pollen carotenoid content, structure, and/or assembly between plant species without prior purification. The analysis of carotenoids in situ is confirmed by high-performance thin-layer chromatography (HPTLC)-supported resonance Raman data measured directly on the HPTLC plates after separation of carotenoids in pollen extracts. Utilization of the in situ, extraction-free procedure in carotenoid analysis will improve sensitivity and structural selectivity and provides insight into carotenoid structure and composition in single pollen grains. PY - 2009 DO - https://doi.org/10.1021/ac901389p SN - 0003-2700 SN - 1520-6882 VL - 81 IS - 20 SP - 8426 EP - 8433 PB - American Chemical Society CY - Washington, DC AN - OPUS4-20260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulte, Franziska A1 - Lingott, J. A1 - Panne, Ulrich A1 - Kneipp, Janina T1 - Chemical characterization and classification of Pollen N2 - We report on the in situ characterization of tree pollen molecular composition based on Raman spectroscopy. Different from purification-based analysis, the nondestructive approach allows (i) to analyze various classes of molecules simultaneously at microscopic resolution and (ii) to acquire fingerprint-like chemical information that was used for the classification of pollen from different species. Hierarchical cluster analysis of spectra from fresh pollen samples of 15 species partly related at the genus level and family level indicates separation of species based on the complete Raman spectral signature and yields classification in accord with biological systematics. The results have implications for the further elucidation of pollen biochemistry and also for the development of chemistry-based online pollen identification methods. PY - 2008 DO - https://doi.org/10.1021/ac801791a SN - 0003-2700 SN - 1520-6882 SP - 1 EP - 12 PB - American Chemical Society CY - Washington, DC AN - OPUS4-18234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulte, Franziska A1 - Brzezinka, K.-W. A1 - Lutzenberger, K. A1 - Stege, H. A1 - Panne, Ulrich T1 - Raman spectroscopy of synthetic organic pigments used in 20th century works of art N2 - Raman microscopy allows a non-destructive characterisation of inorganic and organic painting materials such as pigments and organic dyestuffs. The objectives of this study are the more recent organic pigments typically present in paintings and other art works from the 20th century. More than 20 organic synthetic pigments from different chemical classes could be identified by Raman spectroscopy using different excitation wavelengths (457.9, 476.5, 487.9, 514.5, 632.8, and 1064 nm). To evaluate the performance for real paint samples, varying paint mixtures of the Hansa Yellow pigment PY 3 and the binding medium Mowilith, a polyvinyl acetate (PVAC) compound, were characterised; PY 3 was determined at a 1 wt% level in the binder. In addition, commercial tube paints containing the quinacridone violet PV 19 were studied. The pigment was clearly identified in all of these more complex oil and acrylic paints. Finally, alizarin (PR 83) and a green copper phthalocyanine pigment (PG 7) could unambiguously be identified by Raman microscopy in the painting Woman with mandolin in yellow and red of Max Beckmann dating 1950. The discovery of a red naphthol AS pigment by Raman spectroscopy in a sample from the Three field workers by Georg Baselitz (1964/1965) demonstrated that in some cases complementary chromatographic methods are needed for a comprehensive identification of the organic pigments. KW - Raman microscopy KW - FT-Raman spectroscopy KW - Synthetic organic pigments KW - Modern art PY - 2008 DO - https://doi.org/10.1002/jrs.2021 SN - 0377-0486 SN - 1097-4555 VL - 39 IS - 10 SP - 1455 EP - 1463 PB - Wiley CY - Chichester AN - OPUS4-18401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholz, Philipp A1 - Wachtendorf, Volker A1 - Panne, Ulrich A1 - Weidner, Steffen ED - Scholz, Philipp T1 - Degradation of MDI-based polyether and polyester-polyurethanes in various environments - Effects on molecular mass and crosslinking N2 - Size-exclusion chromatography (SEC) was used to monitor changes of the molecular masses of thermoplastic polyether – and polyester urethane (TPU) exposed to thermal, hydrolytic, and photo-oxidative (UV) Degradation conditions for several days. The thermal treatment was performed at elevated temperatures (100–200 °C) under oxidative (air) as well as non-oxidative (nitrogen) conditions to evaluate the specific influence of oxygen on the degradation. At higher temperatures (≥175 °C) a fast decrease of the molecular masses of both PU accompanied by a high degree of crosslinking was found. At lower temperatures (≤150 °C) the polymers remained widely unaffected by thermal degradation within the investigated degradation interval of up to two weeks. Surprisingly, the influence of oxygen (air) was found to be less distinct. In contrast to that, UV treatment at 25 °C at less than 10% rel. humidity (RH) resulted in a fast crosslinking, whereas the molecular masses of both PU decreased slower than for thermal treatments. The depth of penetration of the UV radiation was estimated using 3D printed PU samples with different thicknesses. Hydrolysis based degradation effects were less significant. Only slight molecular mass changes were detected at temperatures ≤80 °C within a time span of 14 days, while no crosslinking could be measured. Considering the degradation results at the investigated exposure parameters, it could be shown that esterbased PU in general exhibits a significant higher stability compared to ether-based materials. KW - Polyurethane KW - Thermal degradation KW - UV degradation KW - Molecular masses KW - Crosslinking PY - 2019 UR - https://www.sciencedirect.com/science/article/pii/S0142941819302363 DO - https://doi.org/10.1016/j.polymertesting.2019.04.028 SN - 0142-9418 VL - 77 SP - 105881, 1 EP - 12 PB - Elsevier CY - Amsterdam AN - OPUS4-48619 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Wenzel, Klaus-Jürgen A1 - Sarfraz, Adnan A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - A wall-free climate unit for acoustic levitators N2 - Acoustic levitation represents the physical background of trapping a sample in a standing acoustic wave with no contact to the wave generating device. For the last three decades, sample holders based on this effect have been commonly used for contact free handling of samples coupled with a number of analytical techniques. In this study, a wall-free climate unit is presented, which allows the control of the environmental conditions of suspended samples. The insulation is based on a continuous cold/hot gas flow around the sample and thus does not require any additional isolation material. This provides a direct access to the levitated sample and circumvents any influence of the climate unit material to the running analyses. KW - Acoustic levition PY - 2012 DO - https://doi.org/10.1063/1.4705968 SN - 0034-6748 SN - 1089-7623 VL - 83 IS - 5 SP - 055101-1 - 055101-3 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-25881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Sarfraz, Adnan A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - First seconds in a building's life - In situ synchrotron X-ray diffraction study of cement hydration on the millisecond timescale N2 - Setting cement: Highly dynamic hydration processes that occur during the first seconds of cement hydration were studied by time-resolved synchrotron X-ray diffraction. Polycarboxylate ether additives were found to influence the formation of the initial crystalline hydration products on a molecular level. KW - Cement hydration KW - Colloidal suspensions KW - In situ analysis KW - X-ray diffraction KW - SyXRD KW - High resolution KW - In-situ PY - 2012 DO - https://doi.org/10.1002/anie.201200993 SN - 1433-7851 SN - 1521-3773 SN - 0570-0833 VL - 51 IS - 20 SP - 4993 EP - 4996 PB - Wiley-VCH CY - Weinheim AN - OPUS4-26287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Sarfraz, Adnan A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Erste Sekunden im Leben eines Bauwerks - In-situ-Synchrotron-Röntgenbeugungsuntersuchungen der Zementhydratation mit Millisekunden-Auflösung N2 - Höchst dynamische Hydratationsprozesse in den ersten Sekunden bei der Entstehung eines Bauwerkes lassen sich mithilfe von Synchrotron-Röntgenbeugung mit einer sehr hohen Zeitauflösung nachverfolgen. Der Schwerpunkt lag dabei auf der Beeinflussung der Bildung erster kristalliner Hydratationsprodukte während des Frühstadiums der Zementhydratation. KW - SyXRD KW - High resolution KW - In-situ KW - Colloidal suspension KW - Cement hydration KW - In-situ-Analyse KW - Kolloidale Suspensionen KW - Röntgenbeugung KW - Zementhydratation PY - 2012 DO - https://doi.org/10.1002/ange.201200993 SN - 0044-8249 SN - 0932-2140 SN - 1521-3757 VL - 124 IS - 20 SP - 5078 EP - 5081 PB - Wiley-VCH CY - Weinheim AN - OPUS4-26284 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schlegel, Moritz-Caspar A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska A1 - Meng, Birgit ED - Rogge, A. ED - Meng, B. T1 - Neue Wege in der Zementanalytik - Hochaufgelöste in-situ Sy-XRD T2 - 52. DAfStb-Forschungskolloquium CY - Berlin, Deutschland DA - 2011-11-07 PY - 2011 SN - 978-3-9814281-0-0 SP - 18 EP - 24 PB - BAM Bundesanstalt für Materialforschung und -prüfung CY - Berlin AN - OPUS4-25197 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Deciphering the sulfate attack of cementitious materials by high-resolution micro-x-ray diffraction N2 - The durability of cementitious materials depends, among others, on their resistance against chemical attack during the service life of a building. Here, we present an approach to analyze changes in the phase composition due to chemical attack in the form of sulfate ingress within the microstructure. Micro-X-ray (µX-ray) diffraction using synchrotron radiation in Debye–Scherrer (transmission) geometry allowed a spatial resolution of 10 µm. Phase transformations in the wake of damaging processes were observed in a detailed high-resolution imaging study. In comparison, samples containing supplementary cementitious materials were investigated and used to reconstruct the influence of different degeneration processes in detail. Additionally, reaction fronts within the bulk were localized by micro-X-ray fluorescence analysis. The experimental setup provided the possibility for analyzing the phase assemblage of a given sample without destroying the microstructure. The specimens for phase analysis are thick sections of the primary material and can be used for further microscopic analysis of the microstructure and microchemistry, e.g., scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM–EDX) or Raman spectroscopy. PY - 2011 DO - https://doi.org/10.1021/ac200181g SN - 0003-2700 SN - 1520-6882 VL - 83 IS - 10 SP - 3744 EP - 3749 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Müller, Urs A1 - Malaga, Katarina A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Spatially resolved investigation of complex multi-phase systems using muXRF, SEM-EDX and high resolution SyXRD N2 - Spatially resolved analysis of complex multi-phase systems can be validated through different analytical methods. This study compares investigations by scanning electron microscopy coupled with energy dispersive X-ray fluorescence analysis and high resolution X-ray diffraction. The studied sulfate attacked cement paste containing fly ashes consists of different interacting crystalline and amorphous phases. The complementary methods revealed in detail changes in phase composition due to the chemical attack. The advantages and disadvantages of both methods are discussed and suggestions are given for combining them with additional methods to maximize the information content. KW - EDX-SEM KW - SyXRD KW - Spatial investigations KW - Comparison KW - High resolution KW - Cement paste KW - Sulfate attack KW - Damaging mechanism PY - 2013 DO - https://doi.org/10.1016/j.cemconcomp.2012.08.018 SN - 0958-9465 SN - 1873-393X VL - 37 SP - 241 EP - 245 PB - Elsevier Ltd. CY - Barking, Essex AN - OPUS4-29111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, M.C. A1 - Stroh, Julia A1 - Malaga, K. A1 - Meng, Birgit A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Pathway of a damaging mechanism - Analyzing chloride attack by synchrotron based X-ray diffraction N2 - Typically, the changes of the phase compositions due to the chemical attack are studied in-situ only by chemical analysis or microscopy. In this study, the chloride transport and binding in the cement matrix in different cementitious materials was analyzed by synchrotron based X-ray diffraction (SyXRD) and energy dispersive X-ray spectroscopy (EDX). Sample materials consisting of cement paste were embedded in high concentrated sodium chloride solution over different time spans. Afterwards, the phase and chemical compositions were determined. The high spatial resolution and the information about the chloride distribution offer a detailed view of chloride binding in the cement matrix and allow the conclusions about the degradation mechanisms. The results are discussed related to the influence of different supplementary cementitious materials on the damaging mechanism. KW - Portland cement KW - In-situ KW - X-Ray diffraction KW - EDX KW - Durability KW - Chloride attack PY - 2015 DO - https://doi.org/10.1016/j.solidstatesciences.2015.03.021 SN - 1293-2558 SN - 1873-3085 VL - 44 SP - 45 EP - 54 PB - Elsevier Masson SAS CY - Amsterdam AN - OPUS4-33171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schenk, Jonas A1 - Panne, Ulrich A1 - Buurman, Merwe T1 - Interaction of levitated ionic liquid droplets with water N2 - The influence of a humid or dry atmosphere on acoustically levitated ionic liquid droplets was studied by volumetric analysis and vibrational spectroscopy. Imidazolium-based ionic liquids with two types of anions, fluorinated (BF4 and PF6) and alkylsulfate anions, were investigated. The amount of absorbed water was correlated with structural differences of the ionic liquids and analyzed in terms of equilibrium mole fraction as well as absorption rate. The type of anion had the most significant influence on the amount of adsorbed water from the atmosphere. Furthermore, spectral changes in the in situ Raman spectra due to absorbed water were studied for all investigated ionic liquids. For 1-ethyl-3-methylimidazolium ethylsulfate, an exemplary detailed analysis of the intermolecular interactions between cations, anions and water was carried out based on the spectroscopic data. The observed band shifts were explained with a hydrogen bond between the anion and water. KW - Ionic liquids KW - Levitated droplets KW - Raman spectroscopy PY - 2012 DO - https://doi.org/10.1021/jp309661p SN - 1520-6106 SN - 1520-5207 SN - 1089-5647 N1 - Geburtsname von Buurman, Merwe: Albrecht, M. - Birth name of Buurman, Merwe: Albrecht, M. VL - 116 IS - 48 SP - 14171 EP - 14177 PB - Soc. CY - Washington, DC AN - OPUS4-27427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schenk, Jonas A1 - Batzdorf, Lisa A1 - Emmerling, Franziska A1 - Kneipp, Janina A1 - Panne, Ulrich A1 - Buurman, Merwe T1 - Simultaneous UV/Vis spectroscopy and surface enhanced raman scattering of nanoparticle formation and aggregation in levitated droplets N2 - The formation and growth of hydroxylamine reduced silver nanoparticles were investigated by simultaneous Raman and UV/Vis spectroscopy coupled to an acoustic levitator as a sample holder. Based on the UV/Vis spectra, a two step particle formation mechanism with fast initial formation and adjacent coalescence can be proposed for the reduction of silver nitrate with hydroxylamine. The presence of the analyte adenine during particle formation resulted in differences in the adenine SERS signature compared to experiments, where adenine was added after particle synthesis. It was possible to monitor the adenine and sodium chloride induced aggregation of the nanoparticles and its dynamics based on both the extinction spectra and the SERS data. Correlating the information from the extinction spectra with the SERS intensity, the maximum SERS signals were observed at maximum extinction of the aggregated nanoparticle solution at the Raman excitation wavelength. PY - 2012 DO - https://doi.org/10.1039/c2ay05744a SN - 1759-9660 SN - 1759-9679 N1 - Geburtsname von Batzdorf, Lisa: Tröbs, L. - Birth name of Batzdorf, Lisa: Tröbs, L. N1 - Geburtsname von Buurman, Merwe: Albrecht, M. - Birth name of Buurman, Merwe: Albrecht, M. VL - 4 IS - 5 SP - 1252 EP - 1258 PB - RSC Publ. CY - Cambridge AN - OPUS4-25742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sarfraz, Adnan A1 - Simo, A. A1 - Fenger, R. A1 - Christen, W. A1 - Rademann, K. A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Morphological diversity of caffeine on surfaces: needles and hexagons N2 - A systematic crystal morphology study on the pharmaceutical model compound caffeine has been conducted on different surfaces: silicon, silver, soda lime glass, and silver subsurface ion-exchanged soda-lime silicate (SIMO) glasses. The morphology of the solid caffeine deposits has been investigated using environmental scanning electron microscopy (ESEM), atomic force microscopy (AFM), and X-ray diffraction (XRD). Needle-shaped caffeine crystals have been observed by drop-casting and also by applying the rapid expansion of supercritical solutions (RESS) technique using supercritical carbon dioxide. The aspect ratio of the crystalline needles typically vary between 10 and 100, but have been observed as large as 500. The XRD data of the RESS products indicate unambiguously the presence of the thermodynamically most stable polymorph of caffeine known as the β-form. Under defined conditions we observe a unique, surface-mediated morphology for caffeine crystals with nearly perfect hexagonal shape. The relative fraction of the hexagons was seen to strongly increase especially when SIMO glasses were used. These hexagons have a distinct upper size limit depending on the solvent and substrate being used. The size distribution analysis of the hexagons yielded an average perimeter of typically 10 µm. The mechanism of the formation process of this new hexagonal motif is explained in terms of the spinodal dewetting of the thin film of caffeine solution on the surface. KW - Caffeine KW - Silicon KW - Silver KW - Ion exchanged soda lime silicate glass KW - ESEM KW - AFM KW - X-ray diffraction KW - RESS KW - Carbon dioxide KW - Supercritical fluids PY - 2012 DO - https://doi.org/10.1021/cg101358q SN - 1528-7483 VL - 12 IS - 2 SP - 583 EP - 588 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-25457 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudtsch, S. A1 - Gusarova, Tamara A1 - Aulich, A. A1 - Fahr, M. A1 - Fischer, J. A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Procedure for the impurity-related correction at the indium fixed-point N2 - Determining the influence of impurities on the fixed-point emperatures of the ITS-90 requires the completion of several tasks. In this paper, the Progress made at Physikalisch-Technische Bundesanstalt (PTB) and BAMFederal Institute for Materials Research and Testing is presented and remaining questions are discussed. The projected characterization procedure at PTB, which is based on the established SIE method (sum of the individual estimates), using a new indium fixed-point cell is described as an example. This procedure includes an SI-traceable chemical Analysis of the material in the fixed-point cell with sufficiently low uncertainties, the individual experimental determination of the influence of the quantified impurities on the fixed-point temperature, and the establishment of direct links to the phase-transition temperatures of the national standard and of an assumed material of ideal purity. A characteristic difference to the common practice is the chemical analysis of the fixed-point metal being done after determining the cell’s freezing temperature. This allows for the detection and consideration of contamination and purification effects due to the filling process, or due to the contact with the carbon crucible and other parts of the fixed-point cell. A chemical analysis of an indium fixed-point was carried out by BAM with relative measurement uncertainties below 30 % which have not been previously achieved. The results provide evidence for the precipitation of some impurities, which is apparently inconsistent with the corresponding binary phase diagrams, but was explained in a recent publication. Implications for the use of the SIE method shall be described briefly at the end. KW - Chemical analysis KW - Fixed-points KW - Impurities KW - ITS-90 PY - 2011 DO - https://doi.org/10.1007/s10765-011-0915-0 SN - 0195-928X SN - 1572-9567 VL - 32 IS - 1-2 SP - 293 EP - 302 PB - Springer CY - Dordrecht AN - OPUS4-23373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosenkranz, Daniel A1 - Kriegel, F. L. A1 - Mavrakis, E. A1 - Pergantis, S. A. A1 - Reichardt, Ph. A1 - Tentschert, J. A1 - Jakubowski, Norbert A1 - Laux, P. A1 - Panne, Ulrich T1 - Improved validation for single particle ICP-MS analysis using a pneumatic nebulizer / microdroplet generator sample introduction system for multi-mode nanoparticle determination N2 - This study reports on the development of a single-particle (sp) inductively coupled plasma mass spectrometry (ICP-MS) technique suitable for the multi-mode determination of nanoparticle (NP) metal mass fraction and number concentration. The described technique, which is based on a dual inlet System consisting of a pneumatic nebulizer (PN) and a microdroplet generator (MDG), allows for the sequential introduction of ionic metal calibrant solutions and nanoparticle suspensions via all combinations of the two inlets; thus allowing for a combination of three independent modes of analysis. A novel interface, assembled using standard analytical components (a demountable quartz ICP-MS torch, flexible nonconducting silicon tubing and various connectors), was used to interface the dual inlet system to an ICP-MS. The interface provided improved functionality, compared to a previous design. It is now possible to conveniently exchange and introduce standard solutions and samples via all inlet combinations, analyze them, and also wash the sample inlet systems while the whole setup is still connected to an operating ICP-MS. This setup provided seamless and robust operation in a total of three analysis modes, i.e. three ways to independently determine the metal mass fraction and NP number concentration. All three analyses modes could be carried out within a single analytical run lasting approximately 20 min. The unique feature of the described approach is that each analysis mode is based on a different. KW - Nanomaterials KW - Nanoparticles KW - Single particle ICP-MS KW - Microdroplet generator PY - 2020 DO - https://doi.org/10.1016/j.aca.2019.11.043 VL - 1099 SP - 16 EP - 25 PB - Elsevier B.V. AN - OPUS4-50361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosenkranz, D. A1 - Kriegel, F. L. A1 - Mavrakis, E. A1 - Pergantis, S. A. A1 - Reichardt, P. A1 - Tentschert, J. A1 - Jakubowski, N. A1 - Laux, P. A1 - Panne, Ulrich A1 - Luch, A. T1 - Versatile dual-inlet sample introduction system for multi-mode single particle inductively coupled plasma mass spectrometry N2 - Metal-containing nanoparticles (NP) can be characterized with inductively coupled plasma mass spectrometers (ICP-MS) in terms of their size and number concentration by using the single-particle mode of the instrument (spICP-MS). The accuracy of measurement depends on the setup, operational conditions of the instrument and specific parameters that are set by the user. The transport efficiency of the ICP-MS is crucial for the quantification of the NP and usually requires a reference material with homogenous size distribution and a known particle number concentration. Currently, NP reference materials are available for only a few metals and in limited sizes. If particles are characterized without a reference standard, the results of both size and particle number may be biased. Therefore, a dual-inlet Setup for characterizing nanoparticles with spICP-MS was developed to overcome this problem. This setup is based on a conventional introduction system consisting of a pneumatic nebulizer (PN) for nanoparticle solutions and a microdroplet Generator (μDG) for ionic calibration solutions. A new and flexible interface was developed to facilitate the coupling of μDG, PN and the ICP-MS system. The interface consists of available laboratory components and allows for the calibration, nanoparticle (NP) characterization and cleaning of the arrangement, while the ICP-MS instrument is still running. Three independent analysis modes are available for determining particle size and number concentration. Each mode is based on a different calibration principle. While mode I (counting) and mode III (μDG) are known from the literature, mode II (sensitivity), is used to determine the transport efficiency by inorganic ionic Standard solutions only. It is independent of NP reference materials. The μDG based inlet system described here guarantees superior analyte sensitivities and, therefore, lower detection limits (LOD). The size dependent LODs achieved are less than 15 nm for all NP (Au, Ag, CeO2) investigated. KW - Spectrometer KW - Reference KW - Calibration PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536121 DO - https://doi.org/10.3791/61653 SN - 1940-087X IS - 163 SP - 1 EP - 19 PB - MyJoVE Corporation CY - Cambridge, MA, USA AN - OPUS4-53612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Silke A1 - Meckelburg, Angela A1 - Recknagel, Sebastian A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Determination of trace elements in iron ore, cast iron and steel using the 7500cs KW - Steel KW - Iron ore KW - Cast iron KW - ICP-MS PY - 2009 IS - 38 SP - 4 EP - 5 PB - Agilent Technologies CY - Santa Clara, CA, USA AN - OPUS4-19476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Janine A1 - Fettig, I. A1 - Philipp, Rosemarie A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Fisicaro, P. A1 - Alasonati, E. T1 - Determination of tributyltin in whole water matrices under the European water framework directive N2 - Monitoring of water quality is important to control water pollution. Contamination of the aquatic systemhas a large effect on human health and the environment. Under the European Water Framework Directive(WFD) 2000/60/EC and the related directive on environmental quality standards (EQS) in the field of waterpolicy 2008/105/EC, the need for sensitive reference methods was highlighted. Since tributyltin (TBT) isone of the WFD listed priority substances a method was developed which is capable to qualify and quantifythe pollutant at the required low WFD EQS of 0.2 ng L⁻¹ in whole water bodies, i.e. in non-filtered watersamples with dissolved organic carbon and suspended particulate matter. Therefore special attention waspaid on the interaction of TBT with the suspended particulate matter and humic substances to obtain acomplete representation of the pollution in surface waters. Different water samples were investigatedvarying the content of organic dissolved and suspended matter. Quantification was performed usingspecies-specific isotope dilution (SSID) and gas chromatography with inductively coupled plasma massspectrometry (GC-ICP-MS). Different sample treatment strategies were evaluated and compared. Theprocess of internal standard addition was investigated and optimized, hence the equilibrium betweeninternal standards and matrix is of primary importance to perform accurate SSID. Samples spiked at EQSlevel were analyzed with a recovery between 95 and 105 %. Additionally real surface water samples wereinvestigated and the TBT concentration for the whole water body was determined and compared withconventional routine analysis method. KW - Tributyltin (TBT) KW - Environmental quality standard (EQS) KW - Isotope dilution KW - Humic acid KW - Surface water KW - Suspended particulate matter PY - 2016 DO - https://doi.org/10.1016/j.chroma.2016.06.068 SN - 0021-9673 VL - 1459 SP - 112 EP - 119 AN - OPUS4-36930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Koch, Matthias A1 - Wise, S. A. A1 - Panne, Ulrich T1 - Fifteenth international symposium on biological and environmental reference materials (BERM-15) N2 - The 15th International Symposium on Biological and Environmental Reference Materials (BERM-15), organized by BAM, took place at in Berlin in September 2018. An overview on main topics of the conference is given. KW - BERM KW - Reference materials PY - 2019 DO - https://doi.org/10.1007/s00769-019-01377-9 SN - 1432-0517 SN - 0949-1775 VL - 24 IS - 3 SP - 249 EP - 250 PB - Springer Verlag AN - OPUS4-48203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Recknagel, Sebastian A1 - Kipphardt, Heinrich A1 - Panne, Ulrich T1 - Certified reference materials: CRM - ERM - EURONORM T2 - Reference Materials and Interlaboratory Comparisons II CY - Medlov, Czech Republic DA - 2005-11-07 KW - CRM KW - ERM KW - ECRM PY - 2005 SN - 80-86380-30-0 SP - 7 EP - 12 PB - Cesky metrologicky institut CY - Medlov AN - OPUS4-11253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, Vanessa A1 - Warrikhoff, A. A1 - Panne, Ulrich A1 - Hodoroaba, Vasile-Dan T1 - Determination of the efficiency of an energy dispersive X-ray spectrometer up to 50 keV with a SEM N2 - Both electron and polychromatic photon excitations (micro-focus X-ray source) at a scanning electron microscope (SEM) are used to determine the efficiency of an energy dispersive X-ray spectrometer up to 50 keV by means of a calibrated X-ray spectrometer and reference materials (RM) specially selected for this purpose. KW - Detector efficiency KW - Calibration KW - XRF KW - EDS KW - SEM KW - EDS-TM001 KW - Scattering PY - 2009 DO - https://doi.org/10.1039/b907815k SN - 0267-9477 SN - 1364-5544 VL - 24 SP - 1034 EP - 1036 PB - Royal Society of Chemistry CY - London AN - OPUS4-19714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, Vanessa A1 - Warrikhoff, A. A1 - Panne, Ulrich A1 - Hodoroaba, Vasile-Dan T1 - Determination of emitted X-ray tube spectra by means of a calibrated instrumental setup KW - X-ray tube spectrum KW - XRF KW - SEM KW - EDS KW - Spectrometer efficiency PY - 2010 DO - https://doi.org/10.1017/S1431927610054292 SN - 1431-9276 SN - 1435-8115 VL - 16 IS - Supplement S2 SP - 930 EP - 931 PB - Cambridge University Press CY - New York, NY AN - OPUS4-22471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, Vanessa A1 - Procop, M. A1 - Bjeoumikhova, S. A1 - Panne, Ulrich A1 - Hodoroaba, Vasile-Dan T1 - A routine procedure for the characterisation of polycapillary X-ray semi-lenses in prallelising mode with SEM/EDS N2 - The accurate knowledge of the properties of polycapillary X-ray semi-lenses has a significant influence on the quantitative results in a widespread field of applications involving microfocus X-ray beams. A routine procedure for the characterisation of a polycapillary X-ray semi-lens with a scanning electron microscope (SEM) having attached an energy dispersive spectrometer (EDS) is presented in this paper. A key issue of the procedure consists of fitting the semi-lens in front of the EDS for spectra acquisition. Relevant semi-lens parameters such as focal distance, full width at half maximum (FWHM) of the acceptance area, and transmission are determined in parallelising mode of the semi-lens. Special attention has been paid to the calculation of the transmission. KW - Polycapillary X-ray optics KW - Semi-lens KW - Parallelising mode KW - SEM KW - EDS KW - Acceptance area KW - FWHM KW - Transmission KW - Focal distance KW - XRF PY - 2011 DO - https://doi.org/10.1039/c0ja00135j SN - 0267-9477 SN - 1364-5544 VL - 26 IS - 3 SP - 499 EP - 504 PB - Royal Society of Chemistry CY - London AN - OPUS4-23555 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, Vanessa A1 - Panne, Ulrich A1 - Hodoroaba, Vasile-Dan T1 - Calculation of X-ray tube spectra by means of photon generation yields and a modified Kramers background for side-window X-ray tubes N2 - Popular X-ray tube models available in the literature, i.e. 'Pella', 'Ebel', and 'Finkelshtein and Pavlova', are systematically evaluated with the focus on the estimation of the associated uncertainties. Also taken in consideration and compared is our recent semi-empirical own approach already employed in our lab. This has been working for the common target elements rhodium, molybdenum and tungsten and was further extended in the present work for the target elements copper, chromium and vanadium. By using a modern scanning electron microscope/energy dispersive spectroscopy (SEM/EDS) system this time, higher performances such as stability of the beam current and especially the better energy resolution of the EDS have enabled the reliable extension of our own X-ray tube spectrum approach into the low-energy range, due to increasing interest. Hence, also the more challenging X-ray lines of copper, chromium and vanadium L-series lying in the energy range below 1–2?keV are included into the model. Such low-energy L-lines or, e.g. M-lines of tungsten, are not treated explicitly by the other existing popular algorithms for the nowadays widely used geometries of side-window tubes, offering a unique virtue to our present, modern approach. With our own model, a measurement uncertainty of the X-ray tube spectra (considering the uncertainties associated with the SEM beam current, the detector acceptance solid angle and efficiency of the spectrometer) within 15% has been estimated. The validation of the approach is demonstrated with metrological measurements with a calibrated SEM/EDS system geometrically configured as a side-window X-ray tube. KW - X-ray tube spectra KW - Side-window X-ray tube KW - Reference-free XRF KW - Photon generation yield KW - Kramers background KW - Calibrated SEM/EDS PY - 2012 DO - https://doi.org/10.1002/xrs.2391 SN - 0049-8246 VL - 41 IS - 4 SP - 264 EP - 272 PB - Wiley CY - Chichester AN - OPUS4-26239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, Vanessa A1 - Ostermann, Markus A1 - Panne, Ulrich A1 - Hodoroaba, Vasile-Dan T1 - Performance of mu-XRF with SEM/EDS for trace analysis on the example of RoHS relevant elements - measurement, optimisation and predivtion of the detection limits N2 - For ten years µ-XRF (micro-focus X-ray fluorescence) analysis has been performed with SEM/EDS (scanning electron microscope with an energy dispersive X-ray detector) so that non-destructive analysis of elements at trace level concentrations below 100 µg g-1 becomes possible. This can be considered as a valuable completion of the classical electron probe microanalysis by EDS, an analytical method 'suffering' from rather poor limits of detection in the range of one to two orders of magnitude higher than those of µ-XRF. Based on a representative actual application, namely analysis of RoHS relevant elements at trace concentration levels, the performance of the rather new analytical method with respect to its limits of detection is systematically evaluated. CRMs (certified reference materials) specially prepared to support the quantitative XRF analysis of RoHS relevant elements were employed. On the other side, based on calculations of µ-XRF spectra according to a recently developed physical model the optimization of the analytical performance is also successfully undertaken. KW - RoHS KW - XRF KW - muXRF KW - SEM/EDS KW - Detection limits KW - Trace elements KW - Modelling PY - 2013 DO - https://doi.org/10.1039/c3ja50064k SN - 0267-9477 SN - 1364-5544 VL - 28 IS - 9 SP - 1466 EP - 1474 PB - Royal Society of Chemistry CY - London AN - OPUS4-29045 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prestel, H. A1 - Schott, L. A1 - Niessner, R. A1 - Panne, Ulrich T1 - Characterization of sewage plant hydrocolloids using asymmetrical flow field-flow fractionation and ICP-mass spectrometry N2 - Asymmetrical flow field-flow fractionation (AF4) was applied to characterize aquatic colloids from biological sewage plants and to infer information of colloidal loads, sources, and sinks within the plants, resp. the colloidal interaction with the aqueous phase and the sewage sludge. To characterize the colloids further, especially the distributions of colloid associated heavy metals, the AF4 system was coupled to an inductively coupled plasma mass spectrometer (ICP-MS). The size distribution is determined by AF4 with UV absorbance and fluorescence detection after a calibration by monodisperse polystyrene sulfonate standards (PSS). Samples from different sewage plants and from different depths and locations within a plant were compared. The fulvic/humic acid fraction with a particle diameter dp < 10 nm appeared to be comparable in all samples and decreases only slightly along the plants, whereas larger colloids with dp > 10 nm almost completely passed into the sewage sludge. The concentrations of the initial colloidal heavy metals decreased along the plants. KW - Humic colloids KW - Biological sewage plants KW - Asymmetrical flow field-flow fractionation (AF4) KW - Inductively coupled plasma mass spectrometry (ICP-MS) PY - 2005 SN - 0043-1354 VL - 39 IS - 15 SP - 3541 EP - 3552 PB - Elsevier CY - Amsterdam AN - OPUS4-10887 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Porizka, Pavel A1 - Klessen, Benjamin A1 - Kaiser, J. A1 - Gornushkin, Igor B. A1 - Panne, Ulrich A1 - Riedel, Jens T1 - High repetition rate laser-induced breakdown spectroscopy using acousto-optically gated detection N2 - This contribution introduces a new type of setup for fast sample analysis using laser-induced breakdown spectroscopy (LIBS). The novel design combines a high repetition rate laser (up to 50 kHz) as excitation source and an acousto-optical modulator (AOM) as a fast switch for temporally gating the detection of the emitted light. The plasma radiation is led through the active medium of the AOM where it is diffracted on the transient ultrasonic Bragg grid. The diffracted radiation is detected by a compact Czerny-Turner spectrometer equipped with a CCD line detector. Utilizing the new combination of high repetition rate lasers and AOM gated detection, rapid measurements with total integration times of only 10 ms resulted in a limit of detection (LOD) of 0.13 wt.% for magnesium in aluminum alloys. This short integration time corresponds to 100 analyses/s. Temporal gating of LIP radiation results in improved LODs and consecutively higher sensitivity of the LIBS setup. Therefore, an AOM could be beneficially utilized to temporally detect plasmas induced by high repetition rate lasers. The AOM in combination with miniaturized Czerny-Turner spectrometers equipped with CCD line detectors and small footprint diode pumped solid state lasers results in temporally gateable compact LIBS setups. KW - Laser Induced Breakdown Spectroscopy KW - LIBS KW - Aluminium KW - Charge coupled devices KW - Magnesium KW - Light diffraction PY - 2014 DO - https://doi.org/10.1063/1.4890337 SN - 0034-6748 SN - 1089-7623 VL - 85 IS - 7 SP - 073104-1 - 073104-8 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-31358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Porizka, Pavel A1 - Demidov, Alexandr A1 - Kaiser, J. A1 - Keivanian, J. A1 - Gornushkin, Igor B. A1 - Panne, Ulrich A1 - Riedel, Jens T1 - Laser-induced breakdown spectroscopy for in situ qualitative and quantitative analysis of mineral ores N2 - In this work, the potential of laser-induced breakdown spectroscopy (LIBS) for discrimination and analysis of geological materials was examined. The research was focused on classification of mineral ores using their LIBS spectra prior to quantitative determination of copper. Quantitative analysis is not a trivial task in LIBS measurement because intensities of emission lines in laser-induced plasmas (LIP) are strongly affected by the sample matrix (matrix effect). To circumvent this effect, typically matrix-matched standards are used to obtain matrix-dependent calibration curves. If the sample set consists of a mixture of different matrices, even in this approach, the corresponding matrix has to be known prior to the downstream data analysis. For this categorization, the multielemental character of LIBS spectra can be of help. In this contribution, a principal component analysis (PCA) was employed on the measured data set to discriminate individual rocks as individual matrices against each other according to their overall elemental composition. Twenty-seven igneous rock samples were analyzed in the form of fine dust, classified and subsequently quantitatively analyzed. Two different LIBS setups in two laboratories were used to prove the reproducibility of classification and quantification. A superposition of partial calibration plots constructed from the individual clustered data displayed a large improvement in precision and accuracy compared to the calibration plot constructed from all ore samples. The classification of mineral samples with complex matrices can thus be recommended prior to LIBS system calibration and quantitative analysis. KW - Laser-induced breakdown spectroscopy KW - LIBS KW - Chemometrics KW - Principal component analysis KW - Geochemical analysis PY - 2014 DO - https://doi.org/10.1016/j.sab.2014.08.027 SN - 0584-8547 SN - 0038-6987 VL - 101 SP - 155 EP - 163 PB - Elsevier CY - Amsterdam AN - OPUS4-32588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Phukphatthanachai, Pranee A1 - Vogl, Jochen A1 - Traub, Heike A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - A new approach of using polyethylene frits for the quantification of sulphur in copper metals by isotope dilution LA-ICP-MS and comparison with conventional IDMS techniques N2 - Polyethylene (PE) frits were used to quantify sulphur in copper and its alloys by isotope dilution combined with LA-ICP-MS as an alternative approach to conventional sample preparation: the copper samples were spiked, the spiked samples were dissolved, the resulting solutions were absorbed in the PE frits and finally the PE frits were analysed by LA-ICP-MS. A prerequisite for such a support material is a low sulphur blank and thus PE was selected for this purpose. The absorption efficiency of the PE frits was studied for varying sulphur amounts ranging from 2 mg S to 80 mg S showing that more than 99.5% of the loaded sulphur was absorbed by the frit. The so prepared PE frits were measured by LA-ICP-MS and yielded a good linearity (R2 ¼ 0.999) for the sulphur ion intensities corresponding to sulphur amounts up to 40 mg S; the associated sensitivity is approximately 3.4 x 10⁴ cps μg⁻¹ for ³²S. For the validation of the developed procedure the reference materials BAM-M376a, BAM-228 and BAM-227 were applied such that 2 μg S, 5 μg S and 11 μg S were absorbed in the PE frits, respectively. These samples were pre-quantified for the adsorbed sulphur amount by external calibration LA-ICP-MS yielding sulphur amounts of 0.9 μg, 5.1 μg and 8.5 μg (quantified for ³²S only), respectively. Relative Standard deviations of the isotope ratios were below 5% in average (n ¼ 3 lines) in all cases (except for the pure spike solution). These samples were then analysed by LA-ICP-IDMS and the measurement results were validated by comparing them with the results obtained by conventional ICP-IDMS. The obtained relative expanded measurement uncertainties ranged between 10% and 26%. Pearson's coefficient was used to express the correlation between both techniques; the obtained value was 0.999 demonstrating a strong correlation. Contrary to most published LA-ICP-IDMS procedures, the developed procedure enables SI-traceability for the measurement results. The metrological traceability to the SI for the sulphur mass fractions in copper was established by an unbroken chain of comparisons, each accompanied by an uncertainty budget. Thus, the measurement results are considered reliable, acceptable and comparable within the stated measurement uncertainty. The metrological traceability chain from the kg down to mass fraction in the samples obtained by LA-ICP-IDMS is presented as well. KW - Laser ablation KW - IDMS KW - Traceability KW - Uncertainty KW - Purity PY - 2018 DO - https://doi.org/10.1039/c8ja00116b SN - 0267-9477 SN - 1364-5544 VL - 33 IS - 9 SP - 1506 EP - 1517 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-45899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Phukphatthanachai, Pranee A1 - Panne, Ulrich A1 - Jakubowski, Norbert A1 - Vogl, Jochen T1 - SI-traceable quantification of sulphur in copper metal and its alloys by ICP-IDMS N2 - Previously applied methods for the quantification of sulphur in copper and other pure metals revealed a lack of SI-traceability and additionally showed inconsistent results, when different methods were compared. Therefore, a reference procedure is required which allows SI-traceable values accompanied by a Sound uncertainty budget. In this study a procedure was developed for the quantification of total sulphur in copper at low concentration levels using inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS). The major part of the copper matrix was separated by adding ammonia which forms a complex with the copper while releasing the sulphur followed by chromatographic separation using a weak cation resin. After that the sulphur fraction was further purified by chromatographic means using first an anion exchange method and second a chelating resin. The developed procedure shows high performance, especially concerning high efficiency in matrix removal (>99.999%) while keeping the recovery of sulphur above 80%. Procedure blanks are in the order of 3–53 ng resulting in LOD and LOQ values of 0.2 mg g1 and 0.54 mg g1, respectively. The procedure is sufficient to facilitate value assignment of the total sulphur mass fraction in reference materials. Additionally, relative measurement uncertainties were calculated to be below 1% and the measurement results were traceable to the SI. The procedure reported in this study is a new reference procedure for sulphur measurement in copper, being fit for two major purposes, certification of reference materials and assignment of reference values for inter-laboratory comparison. KW - Traceability KW - Measuremment uncertainty KW - Isotope dilution mass spectrometry KW - Reference measurements PY - 2018 DO - https://doi.org/10.1039/c7ja00338b SN - 0267-9477 SN - 1364-5544 VL - 33 IS - 1 SP - 90 EP - 101 PB - Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-43614 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Phukphatthanachai, P. A1 - Panne, Ulrich A1 - Traub, Heike A1 - Pfeifer, Jens A1 - Vogl, Jochen T1 - Quantification of sulphur in copper and copper alloys by GDMS and LA-ICP-MS, demonstrating metrological traceability to the international system of units N2 - The quantification of the sulphur mass fraction in pure copper and copper alloys by GDMS and LA-ICP-MS revealed a lack of traceability mainly due to a lack of suitable certified reference materials for calibrating the instruments. Within this study GDMS and LA-ICP-MS were applied as routine analytical tools to quantify sulphur in copper samples by applying reference materials as calibrators, which were characterized for their sulphur mass fraction by IDMS beforehand. Different external calibration strategies were applied including a matrix cross type calibration. Both techniques with all calibration strategies were validated by using certified reference materials (others than those used for calibration) and good agreement with the reference values was achieved except for the matrix cross type calibration, for which the agreement was slightly worse. All measurement results were accompanied by an uncertainty statement. For GDMS, the relative expanded (k = 2) measurement uncertainty ranged from 3% to 7%, while for LA-ICP-MS it ranged from 11% to 33% when applying matrix-matched calibration in the sulphur mass fraction range between 25 mg kg-1 and 1300 mg kg-1. For cross-type calibration the relative expanded (k = 2) measurement uncertainty need to be increased to at least 12% for GDMS and to at least 54% for LA-ICP-MS to yield metrological compatibility with the reference values. The so obtained measurement results are traceable to the international system of units (SI) via IDMS reference values, which is clearly illustrated by the unbroken chain of calibrations in the metrological traceability scheme. KW - Sulfur KW - Copper KW - GDMS KW - LA-ICP-MS KW - Uncertainty KW - Traceability KW - SI PY - 2021 DO - https://doi.org/10.1039/d1ja00137j SN - 0267-9477 VL - 36 IS - 11 SP - 2404 EP - 2414 PB - Royal Society of Chemistry AN - OPUS4-53412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Panne, Ulrich A1 - Bremser, Wolfram T1 - Considerations with regard to the calculation of key comparison reference values and uncertainties N2 - Much has been published over the last years on finding the best (consensus) reference value for a given set of key comparison data, and a suite of approaches proposed. In this paper, several aspects are highlighted which should be taken into account when deciding on key comparison strategies, protocols, and the best approach to reliable key comparison reference value and uncertainty. Some of these aspects are briefly discussed. The paper is intended to intensify discussions, and any comments and opinions are welcome. KW - Key comparison KW - Reference value KW - Reference value uncertainty KW - Equivalence PY - 2009 DO - https://doi.org/10.1007/s00769-009-0515-x SN - 0949-1775 SN - 1432-0517 VL - 14 IS - 5 SP - 281 EP - 287 PB - Springer CY - Berlin AN - OPUS4-19460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich A1 - Kneipp, Janina A1 - Schulte, Franziska T1 - Raman and FT-IR Spectroscopy for bioanalytical applications T2 - EUROANALYSIS 14 CY - Antwerp, Belgium DA - 2007-09-11 PY - 2007 AN - OPUS4-16462 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich A1 - Kneipp, Janina T1 - Chemical analysis of bioaerosols T2 - LIBS 2006 CY - Montreal, Canada DA - 2006-09-04 PY - 2006 AN - OPUS4-16464 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich A1 - Gornushkin, Igor B. T1 - LIBS as an analytical method-facts, figures and high hopes T2 - Winter Plasma Conference 2014 CY - Amelia Island, FL, USA DA - 2014-01-06 PY - 2014 AN - OPUS4-35187 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich A1 - Riedel, Jens A1 - Höhse, Marek A1 - Kadenkin, Alexander A1 - Demidov, Alexandr T1 - Towards Quantitative LIBS: Modeling and Chemometrics T2 - EMSLIBS 2011 CY - Izmir, Turkey DA - 2011-09-11 PY - 2011 AN - OPUS4-24122 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Spectrochemical Analysis: Tools and Toys!? T2 - GDCH-Vortrag, Wintersemester, Universtät Essen-Duisburg CY - Essen, Germany DA - 2011-02-02 PY - 2011 AN - OPUS4-22140 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Against All Odds - Analytical Sciences for Real- World Applications T2 - GDCh-Vortrag/Fresenius-Lecture CY - Tübingen, Germany DA - 2012-05-24 PY - 2012 AN - OPUS4-25750 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Nie wieder Dienstmagd- Analytical Sciences in Action T2 - GDCh-Vortrag/Fresenius-Lecture CY - Münster, Germany DA - 2012-06-18 PY - 2012 AN - OPUS4-25751 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Analytical science of fire T2 - Fire Science Workshop CY - Berlin, Germany DA - 2013-11-29 PY - 2013 AN - OPUS4-30984 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich A1 - Niessner, R. A1 - Prestel, H. T1 - Improvement of Asymmetrical FlowField-flow Fractionation - Using Slot-outlet Technique T2 - First Munich Conference on Field Flow Fractionation in Pharmaceutical Biotechnology CY - Munich, Germany DA - 2005-10-06 PY - 2005 AN - OPUS4-10917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Adlershof - die Stadt für Wissenschaft, Wirtschaft und Medien T2 - Tagung des Verbandes der Chemischen Industrie, AK "Forschung und Innovation", WISTA Adlershof CY - Berlin, Germany DA - 2005-09-20 PY - 2005 AN - OPUS4-10858 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Chemical Analysis of Bioaerosols - Possibilities and Limitations T2 - Workshop CY - Aachen, Germany DA - 2005-09-06 PY - 2005 AN - OPUS4-10337 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Analytische Chemie - Wissenschaft oder Dienstmagd T2 - 6. ASAC Junganalytikertreffen CY - Vienna, Austria DA - 2010-06-11 PY - 2010 AN - OPUS4-21538 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Aktivitäten der BAM im Stahlbereich T2 - Vorstandssitzung Stahlinstitut VDEh und Wirtschaftsvereinigung Stahl CY - Berlin DA - 2014-03-19 PY - 2014 AN - OPUS4-35188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich A1 - Radivojevic, I. A1 - Niessner, R. A1 - Haisch, C. A1 - Becker-Ross, H. A1 - Florek, S. T1 - Laser-induced Plasma Spectroscopy (LIPS) in the VUV - Possibilities and Limitations T2 - 3rd International Conference on Laser Induced Plasma Spectroscopy and Applications (LIBS 2004) CY - Torremolinos, Spain DA - 2004-09-28 PY - 2004 AN - OPUS4-3882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - CRM development at BAM - status and future trends T2 - BERM 10, Tenth International Symposium on Biological and Environmental Reference Materials CY - Charleston, SC, USA DA - 2006-04-30 PY - 2006 AN - OPUS4-12299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Spektrochemische Methoden für die Prozessanalytik T2 - Kolloquium, BASF CY - Ludwigshafen am Rhein, Germany DA - 2005-04-20 PY - 2005 AN - OPUS4-7173 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Standardization in LIBS Measurement T2 - EMSLIBS CY - Rome, Italy DA - 2009-09-28 PY - 2009 AN - OPUS4-19839 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Forschen - Prüfen - Beraten - Ziele und Aufgaben der Ressortforschung N2 - Der Vortrag gibt einen Überblick die deutsche Ressortforschung. Neben einer Einordnung in das deutsche Wissenschaftssystem werden in einem historischen Überblick die Besonderheiten der Ressortforschung diskutiert. Besonderes Augenmerk wird der Frage gewidmet „Was ist gute Ressortforschung“. Kritisch erscheint besonders die Vereinbarkeit von exzellenter Wissenschaft und seriöser und unabhängiger Politikberatung. T2 - Auftaktveranstaltung des BMVI-Expertennetzwerks Wissen - Können - Handeln CY - BMVI, Berlin, Germany DA - 19.04.2016 KW - Ressortforschung KW - Ressortforschungseinrichtung KW - Wissenschaftliche Politikberatung PY - 2016 AN - OPUS4-37530 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Forschungsgemeinsamkeiten BAM - BASt T2 - Forschungskolloquium Betronstraßenbau CY - Dresden DA - 2014-12-11 PY - 2014 AN - OPUS4-35189 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Mit Sicherheit vorn - Analytische Chemie im Dienste der technischen Sicherheit und Materialforschung T2 - Institutskolloquium des GKSS Teltow CY - Teltow, Germany DA - 2010-05-27 PY - 2010 AN - OPUS4-21537 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Analytische Chemie an der BAM - Werkzeug oder Wissenschaft? T2 - Institutskolloqium der Universität Münster, WWU Münster CY - Münster, Germany DA - 2009-11-04 PY - 2009 AN - OPUS4-19885 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Analytical Sciences: From Ostwald's maid to enabling science N2 - The talk will address the paradigm shift in Analytical Sciences in regard to chemistry as a discipline. To illustrate this metamorphose examples from spectroschemical analysis, ufluidics, bioanalysis, and the didgital transformation of analytical sciences are discussed. T2 - GDCh-Wissenschaftsforum 2019 CY - Aachen, Germany DA - 15.09.2019 KW - Spectrochemical analysis KW - Analytical Sciences PY - 2019 AN - OPUS4-51471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich A1 - Braun, Ulrike A1 - Schartel, Bernhard A1 - Weidner, Steffen A1 - Rurack, Knut A1 - Thünemann, Andreas A1 - Sturm, Heinz T1 - Polymerwissenschaften@BAM - Sicherheit macht Märkte N2 - Die Bundesanstalt für Materialforschung und -prüfung (BAM) ist eine Ressortforschungseinrichtung, die zum Schutz von Mensch, Umwelt und Sachgüter, forscht, prüft und berät. Im Fokus aller Tätigkeiten in der Materialwissenschaft, der Werkstofftechnik und der Chemie steht dabei die technische Sicherheit von Produkten und Prozessen. Dazu werden Substanzen, Werkstoffe, Bauteile, Komponenten und Anlagen sowie natürliche und technische Systeme erforscht und auf sicheren Umgang oder Betrieb geprüft und bewertet. Schwerpunkt des Vortrages sind multimodale Polymeranalytik, nanoskalige Sensormaterialien und die Charakterisierung von technischen Eigenschaften von Polymeren sowie ihre Alterung und Umweltrelevanz. T2 - Institutsvortrag CY - Fraunhofer IAP, Potsdam, Germany DA - 18.05.2018 KW - Polymerwissenschaften PY - 2018 AN - OPUS4-45243 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Hyphenated Techniques for New Insights in Polymer Analysis: 2dim LC and MALDI T2 - 4. Workshop Möglichkeiten und Grenzen der HPLC in den Lebenswissenschaften CY - Dresden, Germany DA - 2011-03-30 PY - 2011 AN - OPUS4-23460 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Some Remarks on Reference Materials for Microanalysis T2 - PRORA 2005 (Fachtagung Prozessnahe Röntgenanalytik), WISTA Adlershof CY - Berlin, Germany DA - 2005-11-24 PY - 2005 AN - OPUS4-11367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Mit Sicherheit vorn - Analytische Chemie an der BAM T2 - DGCh-Vortrag, Universität Hannover CY - Hanover, Germany DA - 2008-05-08 PY - 2008 AN - OPUS4-17762 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Analytische Chemie - nur eine Querschnittswissenschaft? T2 - Abteilungsseminar CY - Berlin, Germany DA - 2005-08-17 PY - 2005 AN - OPUS4-10336 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Analytical Sciences in Action: The Graduate School SALSA T2 - IRIS 2015 CY - Berlin DA - 2015-07-10 PY - 2015 AN - OPUS4-35192 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich A1 - Weller, Michael G. A1 - Rurack, Knut T1 - Process Sensing and Chemical Sensor Development at BAM T2 - Sitzung des fms/ProcessNet-Gemeinschafts-Ausschusses „Sensoren und Sensorsysteme“ CY - Frankfurt am Main, Germany DA - 2012-01-26 PY - 2012 AN - OPUS4-24645 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Physikalische Analysemessmethoden, Methodenkopplung, prozessnahe Analytik - Kompetenzzentrum Analytik Adlershof T2 - Roadmap-Meeting, Max-Born-Institut Berlin CY - Berlin, Germany DA - 2005-06-28 PY - 2005 AN - OPUS4-7630 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Analytical chemistry at BAM - Safety in chemistry and technology T2 - Seminarvortrag Warschau CY - Warsaw, Poland DA - 2007-05-20 PY - 2007 AN - OPUS4-16459 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Bioanalytics at BAM: Challenge and Chance T2 - ISAS-Tagung CY - Dortmund, Germany DA - 2006-12-12 PY - 2006 AN - OPUS4-16463 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Spectrochemical Analysis: Tools and Toys!? T2 - eingel. Vortrag CY - Graz, Austria DA - 2010-03-15 PY - 2010 AN - OPUS4-21536 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Against all odds - Analytical Sciences for real-world applications T2 - Fresenius-Lecture CY - Giessen, Germany DA - 2012-07-03 PY - 2012 AN - OPUS4-25624 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Analytical Sciences in Action T2 - Institutskolloquium Max-Planck-Institut für Dynamik komplexer technischer Systeme CY - Magdeburg DA - 2015-03-05 PY - 2015 AN - OPUS4-35191 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Big Data in Analytical and Material Sciences T2 - Adlershofer Forschungsforum CY - Berlin DA - 2014-11-11 PY - 2014 AN - OPUS4-35190 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Analytical chemistry in materials research T2 - CCQM-Meeting CY - Paris, France DA - 2007-04-17 PY - 2007 AN - OPUS4-16461 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -