TY - CONF A1 - Rosner, M. T1 - Intercomparison of delta26Mg Values in Mg Isotope RMs and Standards N2 - Accurate measurements of stable isotope abundance ratio variations are often reported using artifact based delta-scales, which rely on suitable isotopic reference materials (iRM) for their realization. For example, variations in the 26Mg/24Mg isotope abundance ratio in natural systems are typically reported as delta26Mg values that represents the relative difference between the 26Mg/24Mg ratio measured in a sample relative to its measurement preferably in an iRM. In the past, such delta26Mg measurements were referenced to NIST SRM 980, the initial zero of the delta26Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. It was then replaced by a Mg solution (DSM3), the new zero of the delta26Mg scale. A potential replacement iRM for DSM3 has been developed, ERM-AE143. This iRM has also been measured for its absolute isotope amount ratios1,2 making it traceable to the SI. The results of an delta26Mg intercomparison experiment include the Mg iRMs SRM 980, IRMM-009, ERM-AE143, AE144, AE145 standards DSM3 and Cambridge-1. The intercomparison involved 5 expert laboratories, consisting of 3 national metrological institutes (BAM, NIST, PTB) and 2 scientific research laboratories (GFZ Potsdam, UBremen). The iRMs were measured relative to AE143 and cover a range of ≈5 ‰ in delta26Mg. IRMM-009 has the lowest delta26Mg value while DSM3 has the highest, spanning a range in values that covers natural Mg isotope variations. The 2SD reproducibilities of the individual values from the different laboratories range from 0.02 to 0.26 ‰. The mean delta26Mg values, calculated from the laboratory means however show 2SD reproducibilities varing between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for delta26Mg determinations. 1 JAAS, 2015, 31,179; 2JAAS, 2016, 31, 1440 T2 - Goldschmidt Conference 2017 CY - Paris, France DA - 13.08.2017 KW - Magnesium delta scale KW - Isotope reference material KW - Intercalibration PY - 2017 AN - OPUS4-43995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred T1 - Determination of lost paint layers by scanning electron microskopy N2 - The identification of external paint layers on medieval stained glass windows in Lincoln Cathedral is not only of interest for art historians but is also important for the development of conservation proposals. For the gradual reduction and removal of corrosion layers conservators have to take care to preserve any remaining paint layers which are hidden underneath these corrosion and weathering crusts. T2 - Aspects of Glass - Stained Glass - Art at the Glass Surface CY - Cambridge, Great Britain DA - 02.09.2017 KW - Medieval glass composition KW - SEM/EDX KW - Glass conservation PY - 2017 AN - OPUS4-42131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - In situ monitoring of a mechanochemical Knoevenagel condensation N2 - Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions. T2 - BESSY II User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - Mechanochemistry KW - In situ KW - Knoevenagel condensation KW - C-C coupling PY - 2017 AN - OPUS4-44142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - In situ monitoring of mechanochemical Knoevenagel condensations N2 - Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions. T2 - Adlershofer Forschungsforum CY - Berlin, Germany DA - 10.11.2017 KW - Mechanochemistry KW - Knoevenagel condensation PY - 2017 AN - OPUS4-44140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - In situ investigation of a mechanochemical Knoevenagel condensation N2 - Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions. T2 - PRORA CY - Berlin, Germany DA - 30.11.2017 KW - C-C coupling KW - Knoevenagel condensation KW - In situ PY - 2017 AN - OPUS4-44141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tvrdoňová, M. A1 - Ascher, Lena T1 - A new strategy of reagents labeling (NPs) used in immunoassay with LA-ICP-MS N2 - Laser ablation with inductively coupled plasma is still more used in life science as biology and biomedicine and the utilization of metals and proteins determination simultaneously is also growing up. We have developed a new strategy of labeling of antibody (it can specific binds to proteins) by nanoparticles and quantum dots which is composed of thousands of atoms and thus increases the sensitivity enormously and of course decreases the Limit of detection, compare to lanthanoids labeling. The ability of successfully tagged antibodies bound to Antigen (protein) was proved by dot blot on membrane imaged by LA-ICP-MS. T2 - Euroanalysis 2017 CY - Stockholm, Sweden DA - 28.08.2017 KW - Immunoassay KW - LA-ICP-MS KW - Labeling KW - Nanoparticle PY - 2017 AN - OPUS4-43168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hiller, Th. A1 - Costabel, S. A1 - Müller-Petke, M. A1 - Kruschwitz, Sabine T1 - Evaluation of different laboratory NMR devices in a tripartite round robin test N2 - Nuclear magnetic resonance (NMR) is a well established laboratory / borehole method to characterize the storage and transport properties of rocks due to its direct sensitivity to the corresponding pore fluid saturation (water or oil) and pore sizes. For petrophysical applications there are several different NMR laboratory devices commercially available varying over a wide range of e.g. magnetic field strength / frequency (2 MHz to 30 MHz), applicable measurement protocols (T1, T2, T1-T2, T2-D, etc.) and sample sizes (2.5 cm to 10 cm in diameter). In this work we present NMR measurements, layed out in a round robin like manner, on a set of 20 sandstone samples. We use three different NMR devices containing two standard setups with homogenous magnetic fields (LIAG and RWTH) and one single-sided setup with gradient field (BGR) to measure T1 and T2 relaxation data. In our evaluation we especially focus on the comparison of the individually inverted relaxation time distributions to quantify the differences arising from different laboratory setups. Diverging results can be deduced on the one hand to the inherit differences between homogeneous and gradient fields but on the other hand also due to quality differences between the two homogeneous setups. Additionally, we also examine the influence of the individually chosen inversion parameters (signal processing, distribution sampling points, error weighting, regularization, etc.) to establish a general standardized best practice recommendation for future petrophysical NMR laboratory measurements. T2 - 77. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Potsdam, Germany DA - 27.03.2017 KW - Nuclear Magnetic Resonance KW - Sandstone PY - 2017 AN - OPUS4-43244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Determination of plant essential nutrients in soils using DP-LIBS N2 - LIBS (laser-induced breakdown spectroscopy) is known as a fast and simultaneous multi-element analysis with little or no sample preparation. In the last few years there has been a growing interest in applications of LIBS in the field of agriculture. As part of the National Research Strategy BioEconomy 2030 the German Federal Ministry of Education and Research (BMBF) started an innovation programme called BonaRes. BonaRes consists of ten interdisciplinary research project associations which are dealing with soil as a sustainable resource for the bio-economy. One of these research projects is I4S (intelligence for soil) which has the goal to develop an integrated system for site-specific soil fertility management. This system includes a sensor platform, which contains different sensors, like XRF, VIS-NIR, Gamma and LIBS. The main task of LIBS measurements in this project is the real time determination of the elemental contents of nutrients in soils, like calcium, magnesium, potassium. For this purpose, a special setup has been designed. The sample uptake operates with the help of a rotatable sample plate which circulates with different velocities to simulate the application on the field. To provide a higher intensity and a better reproducibility of the obtained signal, a double-pulse Nd:YAG laser was used. In order to minimize dust formation from the soil during the operation of the laser, a dust removal by suction has been integrated. When using relative methods such as LIBS, a suitable calibration curve is needed for absolute quantification. With the help of 16 certified reference soils, calibration curves for different elements were initially calculated and used for the quantification of seven soil samples from different testing grounds in Germany. The complex matrix of soils, as well as the influence of moisture and grain size in soils makes the absolute quantification by LIBS challenging. To overcome these influences, a calibration curve based on multivariate analysis (partial least square regression) was generated. T2 - Adlershof Forschungsforum CY - Berlin, Germany DA - 10.11.2017 KW - Fertility management KW - Multivariate KW - Soil KW - LIBS PY - 2017 AN - OPUS4-43154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram A1 - Paul, Andrea T1 - Approaches to measurement uncertainty estimates for nominal properties N2 - Qualitative reference materials (RM) cover a wide range of the overall RM market. Proficiency testing providers attract up to a thousand of participants in PT schemes purely oriented on qualitative results. The RM used for these kinds of PT are poorly regulated, nevertheless with a more and more general acceptance of accreditation in the field of RM production and PT provision, there is an ever increasing interest in assessing producers and providers according to rules already well accepted in the field of quantitative analysis. The basic governing document, ISO 17034:2016, is written in a form that, at least for the overwhelming majority of requirements, may be applied to both qualitative and quantitative RM. However, problems remain. In particular, the expression of uncertainty of a purely qualitative result is still unresolved, and under discussion, the latter now lasting already dozens of years. Some handles would be needed. In the poster, existing approaches and some pragmatic, new ways to tackle the problem are displayed and discussed. T2 - Advanced Mathematical and Computational Tools for Metrology; AMCTM (XI) CY - Glasgow, Scotland, UK DA - 29 August 2017 KW - Nominal properties KW - Qualitative RM PY - 2017 AN - OPUS4-42467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Determining the shell thickness of PTFE@PS core@shell nanoparticles using scanning transmission x-ray microscopy (STXM) N2 - A scanning transmission x-ray microscopy (STXM) based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core-shell nanoparticles which exhibit a strong x-ray absorption contrast and a well-defined interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less x-ray beam induced damage of the sample is achieved by recording STXM images only at two predetermined energies of maximum absorption contrast, instead of recording a stack of images across the whole absorption edge. A model core-shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, is used for demonstration. Near edge x-ray absorption fine structure (NEXAFS) spectroscopy confirms the significant difference in x-ray absorption behavior between PTFE and PS. Additionally, due to the insolubility of styrene in PTFE a well-defined interface between particle core and shell is expected. In order to validate the STXM results, both the naked PTFE cores as well as the complete core-shell nanoparticles are examined by scanning electron microscopy (SEM). The introduced STXM based methodology yields particle dimensions in good agreement with the SEM results (deviation equal or less than 10%) and provides additional information such as the position of the particle core which cannot be extracted from a SEM micrograph. T2 - BAM PhD Day 2017 CY - Berlin, Germany DA - 21.09.2017 KW - STXM KW - SEM KW - PTFE KW - PS KW - Core-shell nanoparticles KW - Polymers KW - Metrology PY - 2017 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-42430 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Simple calibration concept of an online NMR module demonstrated in a modularised production plant N2 - Monitoring specific information (such as physico-chemical properties, chemical re-actions, etc.) is the key to chemical process control. Within the CONSENS Project, the challenge to adapt a commercially available benchtop NMR spectrometer to the full requirements of an automated chemical production environment was tack-led. The developed online NMR module was provided in an explosion proof housing and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit, a programmable logic controller for automated triggering, flow con-trol, as well as data communication. First results of an aromatic coupling reaction in lab scale showed a general feasibil-ity according to the signal information in the acquired NMR spectra even though with a considerable overlap. Due to the comparatively low field strength of the NMR spectrometer multivariate methods had to be considered for the prediction of con-centration profiles based on spectral data. Typically, for industrial application of those methods, e.g. Partial Least Squares Regression (PLS-R) as well as Indirect Hard Modeling, large amount of calibration data is demanded, which must be ac-quired in time consuming lab-scale experiments and offline analytics. When it comes to changes in raw materials (e.g., varying functional groups, additional stabi-lizing agents) calibration experiments and data evaluation models are developed again. Here we present an approach of automated data analysis tools for low field NMR spectra with minimal calibration effort. The algorithms are based on Indirect Hard Modeling, whereby each component in each mixture spectra can be rep-resented by several flexible peak functions (pure component models). This means, that only pure component NMR spectra are needed to generate a first evaluation model. The flexibility of peak functions in the spectral model can be adjusted via constraints of peak parameters. The area of any pure component model can either be converted to concentrations based on a one-point calibration on raw material concentration or even neat solvent signals. In several cases it has been shown, the IHM works almost independently of the matrix of the real samples. Such a calibration can be repeated daily in the beginning of each process run with minimal time effort. Moreover, additional pure components can be added to the model or even substitut-ed while keeping the previously adjusted peak function constraints. The proposed method exhibited good agreement of resulting concentration data from low field NMR spectra, when compared to an online high field NMR spectrometer as refer-ence instrument. T2 - 13. Kolloquium des Arbeitskreises Prozessanalytik der DECHEMA und der GDCh-Fachgruppe Analytische Chemie CY - Esslingen, Germany DA - 20.11.2017 KW - Online monitoring KW - Online NMR spectroscopy KW - Modularised production PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-430999 AN - OPUS4-43099 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Size effects in electrodeposited Ni-coatings N2 - Polycrystalline Ni materials with grain sizes less than 100 nm (nano crystalline NC) and with grain sizes in the micrometer range (micro crystalline MC) in form of thin films have become important in many technologies due to their improved physical, chemical and mechanical properties. Usual the mechanical properties of such coatings are described by a Hardness value and a Young´s modulus measured by Instrumented Indentation Testing (IIT).The behavior of such coatings during indentation test is influenced by different size effects having their representative length scale – grain size, coating thickness, length that characterizes the depth dependence of the hardness (Indentation Size Effect ISE). To estimate realistic values for the intrinsic coating Hardness and Young´s modulus all size effects have to be considered. For this work thin nano crystalline Ni – coatings (average grain size 30 nm) with thickness from 1 μm to 5 μm were electrodeposited on brass substrates. Indentation tests in the continuous stiffness measurement (CSM) mode were provided on as prepared Ni – coatings using a G200 Nanoindentation system (Fa. Keysight). For estimation of the intrinsic hardness of the coatings from composite hardness values calculated from the measured force –displacement curve using the Oliver & Pharr method, the model described by Z.S. Ma [1] was used. It was found that the experimental data can be well described by the model. The fitted values for the intrinsic hardness and the fitting parameters will be given. The different values of intrinsic hardness and of length characterizing depth dependence of the hardness for different coating thickness are discussed as results of changes in the coating structure because of changes in deposition parameters. [1] Z.S. Ma, Y.C. Zhou, S.G. Long, C. Lu: On the intrinsic hardness of a metallic film/substrate system: Indentation size and substrate effects. International Journal of Plasticity 34 (2012) 1-11. This work is supported by European Metrology Program for Innovation and Research (EMPIR) (JRP 14IND03 Strength – ABLE) T2 - Conference: Nanomechanical Testing in Materials Research and Development CY - Dubrovnik, Croatia DA - 01.10.2017 KW - Size effect KW - Substrate effect KW - Electrodeposited Ni - coatings KW - Instrumented indentation testing PY - 2017 AN - OPUS4-42664 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hupatz, H. T1 - Deposition of redox-switchable rotaxanes on surfaces N2 - Deposition of Redox-switchable rotaxanes on surfaces Nature has created molecular machines which can perform a variety of different tasks. They exhibit defined operational pathways and order, resulting in directed macroscopic effects. Within the last decades researchers have been developing numerous artificial molecular machines which are so far mostly operating in solution. However, this represents a major obstacle for the generation of a macroscopic output, due to the random orientation of molecules in solution. As a general approach to this problem, interfaces have been used to generate ordered arrays of functional molecules. Recently, we developed a new class of redox-switchable crown ether/ammonium-based [2]- and [3]rotaxanes which incorporate redox-active tetrathiafulvalene and naphthalene diimide units in their wheels resulting in emergent optoelectronic properties. Electrochemical stimuli influence the interactions between the two macrocycles of [3]rotaxanes and induce conformational changes. In a proof-of-principle study [2]pseudorotaxanes were deposited on gold surfaces by “click”-reaction to azide-terminated self-assembled monolayers to generate ordered arrays of redox-active rotaxanes on-surface. X-ray photoelectron spectroscopy (XPS) confirms the successful deposition of a rotaxane monolayer, though angle-resolved near-edge X-ray absorption fine structure spectroscopy (NEXAFS) exhibits poor order of the rotaxanes. Following, new terpyridine-stoppered rotaxanes will be synthesised opening a pathway for the deposition of [2]- and [3]rotaxanes in a layer-by-layer metal-mediated self-assembly procedure. This approach would allow for a programmed sequence of different rotaxanes in multilayers. Electrochemical on-surface switching will be investigated by angle-resolved NEXAFS spectroscopy, XPS, cyclic voltammetry and UV/Vis spectroscopy. A more detailed understanding of the electron-transfer between the surface and the different rotaxane layers as well as of the on-surface switching could give rise to potential applications like optoelectric data-storage devices or potential-driven molecular motors. T2 - Gordon Research Conference - Artificial Molecular Switches & Motors CY - Holderness, NH, USA DA - 11.06.2017 KW - Rotaxane KW - Immobilization KW - XPS KW - NEXAFS PY - 2017 AN - OPUS4-42843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hupatz, H. T1 - Redox-Switchable Rotaxanes on Surfaces N2 - Nature has created molecular machines which can perform a variety of different tasks. They exhibit defined operational pathways and order, resulting in directed macroscopic effects. Within the last decades researchers have been developing numerous artificial molecular machines which are so far mostly operating in solution. However, this represents a major obstacle for the generation of a macroscopic output, due to the random orientation of molecules in solution. As a general approach to this problem, interfaces have been used to generate ordered arrays of functional molecules. Recently, we developed a new class of redox-switchable crown ether/ammonium-based [2]- and [3]rotaxanes which incorporate redox-active tetrathiafulvalene and naphthalene diimide units in their wheels resulting in emergent optoelectronic properties. Electrochemical stimuli influence the interactions between the two macrocycles of [3]rotaxanes and induce conformational changes. In a proof-of-principle study [2]pseudorotaxanes were deposited on gold surfaces by “click”-reaction to azide-terminated self-assembled monolayers to generate ordered arrays of redox-active rotaxanes on-surface. X-ray photoelectron spectroscopy (XPS) confirms the successful deposition of a rotaxane monolayer, though angle-resolved near-edge X-ray absorption fine structure spectroscopy (NEXAFS) exhibits poor order of the rotaxanes. Following, new terpyridine-stoppered rotaxanes will be synthesised opening a pathway for the deposition of [2]- and [3]rotaxanes in a layer-by-layer metal-mediated self-assembly procedure. This approach would allow for a programmed sequence of different rotaxanes in multilayers. Electrochemical on-surface switching will be investigated by angle-resolved NEXAFS spectroscopy, XPS, cyclic voltammetry and UV/Vis spectroscopy. A more detailed understanding of the electron-transfer between the surface and the different rotaxane layers as well as of the on-surface switching could give rise to potential applications like optoelectric data-storage devices or potential-driven molecular motors. T2 - GDCh-Wissenschaftsforum Chemie CY - Berlin, Germany DA - 10.09.2017 KW - NEXAFS KW - Rotaxane KW - XPS KW - Surface characterization PY - 2017 AN - OPUS4-42848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik T1 - Novel thermographic methods for non-destructive testing using structured illumination N2 - Photothermal imaging is commonly used for the characterization of material properties, the determination of layer thicknesses or the detection of inhomogeneities such as voids or cracks. For this purpose, the solid specimen is externally heated, e.g. by using a light source. The resulting transient heat flows interact with the inner structures of the specimen, which in turn is measured as a transient temperature distribution at the surface. Novel array-shaped, high-power laser light sources allow to control the heating of the surface arbitrarily, both temporally and spatially. This enables us to shape the heat flows within the material in a very specific way. In a first application, we demonstrate how to apply destructively interfering thermal wave fields in order to detect subsurface defects with a very high sensitivity. A similar technique, although originating from a very different physical domain, is already in use for medical 3D imaging showing the high potential of this approach. T2 - Adlershofer For­schungs­forum 2017 CY - Berlin, Germany DA - 10.11.2017 KW - Active thermography KW - Photothermal KW - Crack detection KW - Thermal wave KW - Structured heating PY - 2017 AN - OPUS4-42835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pignatelli, Giuseppe T1 - Effects of nanoparticles on laser ablation N2 - Introduction: Laser Induced Breakdown Spectroscopy (LIBS) is an atomic emission analytical technique, wide spreading in laboratories and industries. One way to dramatically increase its analytical results is to deposit metal NPs on the sample surface, resulting in an better version called Nanoparticle Enhanced LIBS (NELIBS). In order to better know and use this technique, the evolution of the plasma has been studied with Tomography. T2 - CHESS 2017 CY - Florence, Italy DA - 27.11.2017 KW - LIBS KW - Nanoparticles PY - 2017 AN - OPUS4-43476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulla, Hannes T1 - In situ PXRD monitoring of a mechanochemical cocrystal formation in milling jars of different material N2 - We present an in situ PXRD investigation of the mechanochemical cocrystal formation of pyrazinamide with pimelic acid in two milling jar materials. In the steel jar a polymorph transformation presenting an exception of Ostwald’s rule of stages is observed. T2 - BESSY User Meeting 2017 CY - Bessy II (HZB), Berlin, Germany DA - 14.12.2017 KW - In situ KW - XRD KW - Polymorph KW - Cocrystal KW - Milling PY - 2017 AN - OPUS4-43502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kormunda, M. T1 - Study of magnetron sputtering deposited ultrathin FeSnOx films for Surface Plasmon Resonance sensors towards gas sensing applications N2 - In this study, series of coatings with the goal of sensitising gold SPR sensors towards CO, NH4, etc. were prepared. To better understand the mechanism behind the sensitizing effect and to enable the targeted production of optimized layers, the wide range of coatings was studied by multiple methods from spectroscopic ellipsometry for their dielectric function, by XPS for chemical composition and SEM, TEM to determine their microscopic structure. The coatings were deposited at inert Ar gas and reactive Ar/O2 gas mixture by RF magnetron sputtering or DC pulsed magnetron sputtering with settable RF bias on the substrates. The plasma processes were monitors by mass spectrometry. The metal oxide coatings in SPR sensors have to be prepared reproducible with thickness about 5 nm therefore lower deposition rate conditions were advantages. T2 - THE 14th INTERNATIONAL SYMPOSIUM ON SPUTTERING & PLASMA PROCESSES,ISSP 2017 CY - Kanazawa, Japan DA - 05.07.2017 KW - Surface Plasmon Resonance KW - Magnetron sputtering KW - FeSnOx PY - 2017 AN - OPUS4-43536 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical reactions - new insights in formation pathways N2 - Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals. The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms. We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases because of the reaction heat. Based on the data, temperature rises as postulated in the magma plasma and hot spot theory can be excluded for soft matter milling syntheses. Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds. T2 - Wissenschaftsforum Chemie CY - Berlin, Germany DA - 10.09.17 KW - Mechanochemistry KW - In situ PY - 2017 AN - OPUS4-43563 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Breitfeld, Steffen T1 - High energy ball milling of a new representative of coordination polymers without organofluorine linkers N2 - Metal organic frameworks and coordination polymers play an important role in different fields of applications. Moreover, particularly fluorinated metal-organic frameworks (FMOFs) are in the focus of interest during the last years. In most cases, fluorine is implemented using perfluorinated organic linkers at the synthesis, usually performed by solvothermal synthesis. However, only few examples are known so far where fluorine is coordinated directly to the metal cation. Recently, we reported about mechanochemical syntheses and characterization of fluorine-containing coordination polymers of alkaline earth metals by milling M(OH) (M: Ca, Sr, Ba) with fluorinated benzene dicarboxylic acids 2 and we reported about mechanochemical syntheses of alkaline earth metal fluorides with ammonium fluoride. Now we are reporting about a combination of both synthesis routes. That is the first mechanochemical synthesis of coordination polymers where fluorine is coordinated directly to the metal cation. T2 - Konferenz CY - Berlin, Germany DA - 30.11.2017 KW - Metal organic frameworks KW - Coordination polymer KW - Mechanochemical syntheses KW - Direct fluorine-metal bond KW - Alkaline earth metal PY - 2017 AN - OPUS4-46898 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosner, Martin T1 - Intercomparison of delta26Mg Values in Mg Isotope RMs and Standards N2 - Accurate measurements of stable isotope abundance ratio variations are often reported using artifact based delta-scales, which rely on suitable isotopic reference materials (iRM) for their realization. For example, variations in the 26Mg/24Mg isotope abundance ratio in natural systems are typically reported as delta26Mg values that represents the relative difference between the 26Mg/24Mg ratio measured in a sample relative to its measurement preferably in an iRM. In the past, such delta26Mg measurements were referenced to NIST SRM 980, the initial zero of the delta26Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. It was then replaced by a Mg solution (DSM3), the new zero of the delta26Mg scale. A potential replacement iRM for DSM3 has been developed, ERM-AE143. This iRM has also been measured for its absolute isotope amount ratios1,2 making it traceable to the SI. The results of an delta26Mg intercomparison experiment include the Mg iRMs SRM 980, IRMM-009, ERM-AE143, AE144, AE145 standards DSM3 and Cambridge-1. The intercomparison involved 5 expert laboratories, consisting of 3 national metrological institutes (BAM, NIST, PTB) and 2 scientific research laboratories (GFZ Potsdam, UBremen). The iRMs were measured relative to AE143 and cover a range of ≈5 ‰ in delta26Mg. IRMM-009 has the lowest delta26Mg value while DSM3 has the highest, spanning a range in values that covers natural Mg isotope variations. The 2SD reproducibilities of the individual values from the different laboratories range from 0.02 to 0.26 ‰. The mean delta26Mg values, calculated from the laboratory means however show 2SD reproducibilities varing between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for delta26Mg determinations. T2 - Goldschmidt 2017 CY - Paris, France DA - 13.08.2017 KW - Magnesium delta value KW - Isotope reference material KW - Intercalibration KW - Magnesium isotope ratio PY - 2017 AN - OPUS4-44639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg T1 - THz-TDS-SAFT for the detection of inherent discontinuities in dielectric materials N2 - X-ray computed tomography (CT) model holds only for THz-TDS reconstruction if minor refraction index differences between the inhomogeneities and the surrounding material matrix exist. A Time Domain SAFT algorithm has been developed to overcome the restrictions. THz time domain measurement on representative sample sets with inherent artefacts were performed to use them for the Image reconstructions. The results will be presented and compared with optical surface images of the used test objects to evaluate the SAFT algorithm in relation to the reconstruction quality. T2 - 42nd International Conference on Infrared, Millimeter and THz waves CY - Cancun, Mexico DA - 27.08.2017 KW - THz-time-domain spectroscopy KW - SAFT KW - Tomography PY - 2017 AN - OPUS4-42034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Donsky, I. S. T1 - 2D nanomaterials with switchable pathogen binding N2 - Graphene derivatives have shown great promise in the field of pathogen binding and sensing. Due to their diverse applications, they show a variety of activities that range from bacterial adhesion to bacterial resistance. Therefore, domination of the graphene-pathogen interactions is highly relevant for producing 2D platforms with the desired applications. In order to gain control over the interactions between graphene and biosystems, mechanisms should be fully understood. The surface functionality of graphene is one of the most important factors that dominates its interactions with biosystems and pathogens. Covalent functionalization is a robust method through which functionality, chemical structure, and subsequently physicochemical properties of graphene are abundantly manipulated. A critical issue for preparing graphene-based 2D materials with a defined surface structure, however, is controlling the functionalization in terms of number, position, and type of functional groups. T2 - 9th Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - Graphene KW - Functionalization KW - XPS KW - C Kedge NEXAFS PY - 2017 AN - OPUS4-43456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Quantitative chemical depth-profiling by synchrotron-radiation-XPS: Investigation of SrF2-CaF2 core-shell nanoparticles N2 - SrF2 nanoparticles can be doped with trivalent earth metal ions such as Eu3+ and Tb3+ to generate materials exhibiting an intensive red or green fluorescence. A CaF2 shell increases intensity, fluorescence lifetie and quantum yield. The chemical composition of the nanoparticle core-shell region is investigated by XPS at different excitation energies corresponding to different information depths. T2 - Ninth Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - Core-shell nanoparticles KW - Synchrotron-XPS KW - Depth-profiling PY - 2017 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-43464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ickert, Stefanie T1 - Collision Specific Fragmentation of Oligonucleotides in Tandem Mass Spectrometry N2 - Tandem MS experiments allow the fast acquisition of spectral datasets with enormous size and unprecedented content of information. The most commonly used method is undoubtedly collision induced dissociation (CID). The relatively young technical adaptation of CID to modern day Orbitrap experiments needs a higher confinement voltage and has accordingly been named higher-energy collisional dissociation HCD. Despite the name the absolute value of transferred energy per collision in HCD is lower than in CID. Since for many proteins CID and HCD result in comparable fragmentation patterns the two techniques are often treated as interchangeable. This approach is, however, not without pitfalls as other classes of biomolecules often exhibit strongly pronounced fragmentation specificity. As an example, MS/MS experiments on several 4-mer oligonucleotides were conducted employing both collision methods and the results were thoroughly compared. It is apparent that not only the total fragment yield but also the identity of the observed fragments differ significantly between the two methods. T2 - Jahrestagung der Deutschen Gesellschaft für Massenspektrometrie DGMS CY - Kiel, Germany DA - 05.03.2017 KW - Tandem MS KW - DNA KW - Mass Spectrometry PY - 2017 AN - OPUS4-42328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosner, M. T1 - Intercomparison of d26Mg Values in Mg Isotope RMs and Standards N2 - Accurate measurements of stable isotope abundance ratio variations are often reported using artifact based delta-scales, which rely on suitable isotopic reference materials (iRM) for their realization. For example, variations in the 26Mg/24Mg isotope abundance ratio in natural systems are typically reported as delta26Mg values that represents the relative difference between the 26Mg/24Mg ratio measured in a sample relative to its measurement preferably in an iRM. In the past, such delta26Mg measurements were referenced to NIST SRM 980, the initial zero of the delta26Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. It was then replaced by a Mg solution (DSM3), the new zero of the delta26Mg scale. A potential replacement iRM for DSM3 has been developed, ERM-AE143. This iRM has also been measured for its absolute isotope amount ratios1,2 making it traceable to the SI. The results of a delta26Mg intercomparison experiment include the Mg iRMs SRM 980, IRMM-009, ERM-AE143, AE144, AE145 standards DSM3 and Cambridge-1. The intercomparison involved 5 expert laboratories, consisting of 3 national metrological institutes (BAM, NIST, PTB) and 2 scientific research laboratories (GFZ Potsdam, UBremen). The iRMs were measured relative to AE143 and cover a range of ≈5 ‰ in delta26Mg. IRMM-009 has the lowest delta26Mg value while DSM3 has the highest, spanning a range in values that covers natural Mg isotope variations. The 2SD reproducibilities of the individual values from the different laboratories range from 0.02 to 0.26 ‰. The mean delta26Mg values, calculated from the laboratory means however show 2SD reproducibilities varing between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for delta26Mg determinations. 1 JAAS, 2015, 31,179; 2JAAS, 2016, 31, 1440 T2 - Goldschmidt Conference 2017 CY - Paris, France DA - 13.08.2017 KW - Iisotope reference materials KW - Delta values KW - Magnesium isotope PY - 2017 AN - OPUS4-42742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - NEXAFS and XPS investigations of a dual switchable rotaxane multilayer N2 - A multilayer consisting of two different rotaxanes was investigated with different analytical methods. The rotaxanes can be switched with two different stimuli - chemical and photochemical. XPS indicates that our layer-by-layer approach worked and a layer growth with every deposition step is present. NEXAFS showed that both stimuli cause an increase of the multilayer's preferential orientation. T2 - BESSY User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - NEXAFS KW - XPS KW - Rotaxanes PY - 2017 AN - OPUS4-43616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Embedded passive RFID-based sensors for moisture monitoring in concrete N2 - Moisture measurements based on passive RFID based sensors. These sensors are embedded into stell reinforced concrete to enable long-term monitoring. T2 - IEEE Sensors 2017 CY - Glasgow, Scotland, UK DA - 30.10.2017 KW - Concrete KW - Embedded sensors KW - RFID based sensors KW - Passive sensors KW - Moisture monitoring PY - 2017 AN - OPUS4-42746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana T1 - Process monitoring of an intensified continuous production unit with compact NMR spectroscopy N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and inexpensive analysers, which feature advantages like low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. Otherwise there is a huge risk of producing large amounts of out-of-spec (OOS) products. This is addressed in the European Union’s Research Project CONSENS by development and integration of smart sensor modules for process monitoring and control within such modular plant setups. The presented NMR module is provided in an explosion proof housing with a module size of 57 x 57 x 85 cm and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction) and evaluation. Indirect Hard Modeling (IHM) was selected for data analysis of the low-field NMR spectra. A set-up for monitoring continuous reactions in a thermostated 1/8” tubular reactor using automated syringe pumps was used to validate the IHM models by using high-field NMR spectroscopy as analytical reference method. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) CY - Kaiserslautern, Germany DA - 19.01.2017 KW - Online NMR spectroscopy PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-390117 AN - OPUS4-39011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Asadujjaman, Asad T1 - Functional polymer based on 2,6-diaminopyridine with tunable UCST behaviour in water/alcohol mixture N2 - Thermoresponsive polymers are of great importance in numerous applications such as bioseparation, drug delivery, diagnostic and microfluidic applications.[1-2] Only a few thermoresponsive polymers have been reported that present an Upper Critical Solution Temperature (UCST), i.e. phase separate from solution upon cooling, in a relevant temperature range and “green” solvents such as water or ethanol.[3] Indeed, polymers with UCST behavior below 60°C in alcohol or water/alcohol mixtures are extremely promising for the preparation of “smart” materials for sensing. In this work, two novel functional polymers of based on a 2,6-diaminopyridine motif were synthesized by free-radical polymerization. Their UCST-type transition temperature is tunable by varying either their concentration in solution or the type of solvent. Insights into this phenomenon are investigated using turbidimetry and temperature dependent dynamic light scattering. T2 - Konferenz CY - Lisbon, Portugal DA - 06.03.2017 KW - Thermoresponsive polymers KW - UCST-type polymers PY - 2017 AN - OPUS4-39579 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illner, M. T1 - Operation and optimal control of multiphase systems – Hydroformylation in microemulsions on the mini-plant scale N2 - develops new process concepts, involving innovative tuneable solvent systems to enable rather difficult or inapplicable synthesis paths. One possible concept is the hydroformylation of long-chained alkenes in microemulsions. For this, a modular mixer-settler concept was proposed, combining high reaction rates and efficient catalyst recycling via the application of technical grade surfactants. The feasibility of such a concept is evaluated in a fully automated, modular mini-plant system within which the characteristics of such a multiphase system pose several obstacles in operating this mini-plant. Maintaining a stable phase separation for efficient product separation and catalyst recycling is complicated by small and highly dynamic operation windows as well as poor measurability of component concentrations in the liquid phases. In this contribution, a model-based strategy is presented to enable concentration tracking and phase state control within dynamic mini-plant experiments. Raman spectroscopy is used as an advanced process analytical tools, which allows for online in-situ tracking of concentrations. Combined with optical and conductivity analysis optimal plant trajectories can be calculated, solving a dynamic optimization problem under uncertainty. Applying these, a stable reaction yield of 40 % was achieved, combined with an oil phase purity of 99,8 % (total amount of oily components in the oil phase) and a catalyst leaching below 0.1 ppm. T2 - 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) CY - Potsdam, Germany DA - 10.05.2017 KW - Process monitoring KW - Hydroformylation KW - Mini-plant KW - Process control KW - Process analytical technology KW - EuroPACT KW - InPROMPT PY - 2017 UR - http://dechema.de/en/europact17.html AN - OPUS4-40233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Bridge Monitoring by Passive Seismic Data, First tests at the BLEIB reference structure N2 - Seismic wave velocities are related to elastic moduli and other properties and can serve as indicators for changes in the material. They are conventionally determined by active measurements. Using ideas from seismic interferometry determination from stacked cross-correlations of registrations of man-made and natural noise (“passive seimics“) is an effective alternative, as these data might be available from vibration monitoring anyway. The validity of this approach is demonstrated by a simple experiment based on recordings of man made noise using accelerometers at the reference structure. The s-wave (or more probable. guided wave) velocity was determined to be 2100 m/s in both active and passive experiments. T2 - Passive Imaging and monitoring in wave physics: from seismology to ultrasound CY - Cargese, France DA - 05.06.2017 KW - Bridge monitoring KW - Passive seismics KW - Ambient noise KW - Interferometry KW - Elastic wave velocity PY - 2017 AN - OPUS4-40577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bennetts, V.H. A1 - Neumann, Patrick P. T1 - Probabilistic air flow modelling using turbulent and laminar characteristics for ground and aerial robots N2 - For mobile robots that operate in complex, uncontrolled environments, estimating air flow models can be of great importance. Aerial robots use air flow models to plan optimal navigation paths and to avoid turbulence-ridden areas. Search and rescue platforms use air flow models to infer the location of gas leaks. Environmental monitoring robots enrich pollution distribution maps by integrating the information conveyed by an air flow model. In this paper, we present an air flow modelling algorithm that uses wind data collected at a sparse number of locations to estimate joint probability distributions over wind speed and direction at given query locations. The algorithm uses a novel extrapolation approach that models the air flow as a linear combination of laminar and turbulent components. We evaluated the prediction capabilities of our algorithm with data collected with an aerial robot during several exploration runs. The results show that our algorithm has a high degree of stability with respect to parameter selection while outperforming conventional extrapolation approaches. In addition, we applied our proposed approach in an industrial application, where the characterization of a ventilation system is supported by a ground mobile robot. We compared multiple air flow maps recorded over several months by estimating stability maps using the Kullback-Leibler divergence between the distributions. The results show that, despite local differences, similar air flow patterns prevail over time. Moreover, we corroborated the validity of our results with knowledge from human experts. T2 - IEEE International Conference on Robotics and Automation (ICRA) CY - Singapore DA - 29.05.2017 KW - Mapping KW - Field robots KW - Environment monitoring and management KW - Aerial systems KW - Perception and autonomy PY - 2017 AN - OPUS4-40549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Esteban-Fernandez, Diego A1 - Traub, Heike A1 - Hutchinson, R. T1 - High resolution laser ablation NWRimage system for single cell imaging N2 - The traceability and availability of nanoparticles enables their use to enhance a variety of nano-biological and nano-medicinal applications. The particular size and shape of nanoparticles determine the uptake rate and pathway into the cell, and therefore impact specific cell components and processes. Selecting specific particle types allows researchers to target the process or structure of interest, with minimal additional impact. This can be used for drug or DNA delivery, and is being explored for use in oncology. Understanding the different uptake mechanisms and impacted processes requires sub-cellular Imaging resolution to determine, for example, whether or not the nanoparticles are reaching the nucleus. Sub-cellular imaging has traditionally been challenging to achieve with laser ablation ICP-MS due to a lack of sensitivity at small spots. Bioimaging using LA-ICP-MS is a well-established technique, but usually applied on the tissue scale, which depends on larger spot areas where sensitivity is less problematic. The improved sensitivity and washout from the NWRimage has allowed faster imaging of smaller spots. The NWRimage also provides the possibility of true sub-micron spot sizes. This work compares the capabilities of standard laser Ablation (NWR213 system) with results from the NWRimage platform, which has been optimized for imaging applications. T2 - European Winter Conference on Plasma Spectrochemistry CY - St. Anton, Austria DA - 19.02.2017 KW - Laser ablation KW - Imaging KW - Nanoparticle PY - 2017 AN - OPUS4-39281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Quantitative NMR spectroscopy for gas metrology – applications in liquefied petroleum gases N2 - The field of gas metrology is dealing with the development and improvement of gas analytical methods, as well as production of highly accurate primary reference standards. These are prepared at national metrological institutes (NMI) and represent the highest national level of traceability. Used for certification of secondary standards provided by specialty gas distributors these are very important for a high number of industrial sectors, which have to proof traceability due to legal or regulatory affairs, e.g., natural gas suppliers. Thus, improvements in the production and certification of these mixtures will have a direct influence on gas industry. Due to its direct correlation to the number of spins within active sample volume quantitative NMR spectroscopy (qNMR) is a highly promising method with absolute comparison abilities in complex systems. Especially for liquefied petroleum gases (LPG) it has the ability of studying the unmodified sample at same conditions like in the cylinder. In contrast to gas chromatography no preparation steps and no changes like evaporation of the sample are necessary. In this work we show the most recent results of our investigations on highly accurate LPG mixtures provided in constant-pressure piston cylinders. A dynamic pressure-resistant setup allows for sampling and circulation of the samples to ensure a homogeneous withdrawal from the cylinder. This is presented on examples of a commercial multicomponent LPG mixture obtained from specialty gas distributor, as well as two cylinders from the key comparison CCQM-K119 at highest level of international metrology. T2 - 5th Panic - Practical Applications of NMR in Industry Conferece CY - Hilton Head Island, SC 29928, USA DA - 20.02.2017 KW - Quantitative NMR spectroscopy KW - Gas metrology KW - Liquefied petroleum gas PY - 2017 AN - OPUS4-39234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krause, B. T1 - Detection of aluminum nanoparticles in biological media and in vitro N2 - Aluminum is the third most abundant element in the earth crust and therefore ubiquitously detectable in the environment. Mostly found in the form of derivatives such as silicates or oxides, it also occurs as metallic aluminum for example as colorant in sweets or in aluminum foil. With regard to potential toxicological effects, the different solubility of metallic aluminum nanoparticles compared to Al2O3 is of high relevance. Formation of ions may facilitate the crossing of blood-tissue barriers. Distribution towards other organs and subsequent re-formation of particulate aluminum due to milieu changes might occur. Therefore, the determination of solubility is required for proper risk assessment. Inductively coupled plasma mass spectrometry (ICP-MS) allows determination of aluminum with a detection limit of about 6 ppb. It could be proven that dissolution and solubility of metallic aluminum is significantly different when compared to Al2O3. Using ICP-MS in the single particle mode, a significant change in the behavior of both aluminum species was detected after undergoing the artificial digestion. Nearly unchanged in the saliva, particles show dissolution and high agglomeration during the gastric state before deagglomerating again in the intestine. Further analysis by time-of-flight secondary ion mass spectrometry (ToF-SIMS) revealed the uptake of both aluminum forms by proliferating and differentiated Caco-2 cells. For both particle forms different ions could be detected. Several aluminum-amino acid complex-derived ions from serine and valine were identified. In the case of Al2O3, Al2O2+, AlOH+, AlH2O+ and Al[(H2O)6]3+ were the main ions found co-localizing within treated cells. T2 - European Winter Conference for Plasma Spectrochemistry 2017 CY - Sankt Anton, Austria DA - 19.02.2017 KW - Aluminum KW - SP-ICP-MS KW - SAXS KW - Artificial digestion KW - Cellular uptake PY - 2017 AN - OPUS4-39201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bierstedt, Andreas T1 - Improving the performance of the laser-spark ion source for the detection of volatile organic compounds under ambient conditions N2 - Recently, a novel ionization scheme for ambient MS has been introduced. It is based on a quasi-continuous laser induced plasma (LIP), ignited in front of the MS inlet. This setup comprises the advantages of an ambient probe, electro neutrality, a sufficient duty cycle, a ubiquitous plasma medium, low power consumption, the absence of solvents and high sensitivity. To assess its future applicability for the detection of volatile organic compounds, plasma properties and operating conditions are investigated to understand the processes, that lead to the unexpected formation of intact molecular ions. Comprehensive studies include optical Emission spectroscopy, shadowgraphic shockwave visualization and time-of-flight mass spectrometry. T2 - 50. Jahrestagung der Deutschen Gesellschaft für Massenspektrometrie CY - Kiel, Germany DA - 05.03.2017 KW - Laser-spark KW - Laser induced plasma KW - Mass spectrometry KW - Ambient ionization PY - 2017 AN - OPUS4-39309 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Online spectroscopy in micellar systems – A process analytical approach for a hydroformylation mini-plant N2 - Within the Collaborative Research Center InPROMPT a novel process concept for the hydroformylation of long-chained olefins is studied in a mini-plant, using a rhodium complex as catalyst in the presence of syngas. Recently, the hydroformylation in micro¬emulsions, which allows for the efficient recycling of the expensive rhodium catalyst, was found to be feasible. However, the high sensitivity of this multi-phase system with regard to changes in temperature and composition demands a continuous observation of the reaction to achieve a reliable and economic plant operation. For that purpose, we tested the potential of both online NMR and Raman spectroscopy for process control. The lab-scale experiments were supported by off-line GC-analysis as a reference method. A fiber optic coupled probe of a process Raman spectrometer was directly integrated into the reactor. 25 mixtures with varying concentrations of olefin (1-dodecene), product (n-tridecanal), water, n-dodecane, and technical surfactant (Marlipal 24/70) were prepared according to a D-optimal design. Online NMR spectroscopy was implemented by using a flow probe equipped with 1/16” PFA tubing serving as a flow cell. This was hyphenated to the reactor within a thermostated bypass to maintain process conditions in the transfer lines. Partial least squares regression (PLSR) models were established based on the initial spectra after activation of the reaction with syngas for the prediction of unknown concentrations of 1-dodecene and n-tridecanal over the course of the reaction in the lab-scale system. The obtained Raman spectra do not only contain information on the chemical composition but are further affected by the emulsion properties of the mixtures, which depend on the phase state and the type of micelles. Based on the spectral signature of both Raman and NMR spectra, it could be deduced that especially in reaction mixtures with high 1-dodecene content the formation of isomers as a competitive reaction was dominating. Similar trends were also observed during some of the process runs in the mini-plant. The multivariate calibration allowed for the estimation of reactants and products of the hydroformylation reaction in both laboratory setup and mini-plant. T2 - 11. Doktorandenseminar 2017 des Arbeitskreis Prozessanalytik der GDCh und DECHEMA CY - Berlin, Germany DA - 12.03.2017 KW - Online reaction monitoring PY - 2017 AN - OPUS4-39398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertin, Annabelle T1 - Temperature Sensitive Aggregation Behavior of Poly(Acrylamide-co-Acrylonitrile) in Water N2 - Thermoresponsive polymers have shown great potential in applications such as bioseparation, drug delivery and diagnostic. Only few thermoresponsive polymers that present an upper critical solution temperature (UCST), i.e. phase separate from solution upon cooling, in a relevant temperature range have been reported so far. Herein, a robust UCST-type copolymer of acrylamide (AAm) and acrylonitrile (AN) (poly(AAm-co-AN)) was prepared by reversible addition fragmentation chain transfer (RAFT) polymerization and its thermo-induced aggregation behavior in aqueous media was studied. We propose a model for the temperature-induced aggregation behaviour of UCST-type poly(AAm-co-AN) copolymer in aqueous solution on the basis of turbidity measurements, SLS, DLS, SANS and cryo-TEM. T2 - German Physical Society - Spring Meeting 2017 CY - Dresden, Germany DA - 19.03.2017 KW - Thermoresponsive polymers KW - UCST-type copolymer PY - 2017 AN - OPUS4-39465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertin, Annabelle T1 - Functional polymer based on 2,6-diaminopyridine with tunable UCST behaviour in water/alcohol mixture N2 - Thermoresponsive polymers are of great importance in numerous applications such as bioseparation, drug delivery, diagnostic and microfluidic applications. Only few thermoresponsive polymers that present an upper critical solution temperature (UCST), i.e. phase separate from solution upon cooling, in a relevant temperature range and green solvents such as water or ethanol have been reported. Indeed, polymers with UCST behavior below 60°C in alcohol or water/alcohol mixtures are extremely promising for the preparation of smart materials for sensing. In this work two novel functional polymers of based on a 2,6-diaminopyridine motif were synthesized by free radical polymerization. Their UCST-type transition temperature is tunable by varying either their concentration in solution or the type of solvent. Insights into this phenomenon will be given based on turbidimetry and temperature dependent dynamic light scattering T2 - German Physical Society - Spring Meeting 2017 CY - Dresden, Germany DA - 19.03.2017 KW - Thermoresponsive polymers KW - USCT-type polymers KW - Polymers based on 2,6-diaminopyridine PY - 2017 AN - OPUS4-39466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Design of an online-analysis technique for the determination of major and minor nutrients in soils using DP-LIBS N2 - LIBS (laser-induced breakdown spectroscopy) is known as a fast and simultaneous multi-element analysis with little or no sample preparation. Because of that, over the last few years there has been a growing interest in applications of LIBS in the field of agriculture. As part of the National Research Strategy BioEconomy 2030 the German Federal Ministry of Education and Research (BMBF) started an innovation programme called BonaRes. BonaRes consists of ten interdisciplinary research project as-sociations which are dealing with soil as a sustainable resource for the bio-economy. One of these research projects is I4S (intelligence for soil) which has the goal to develop an integrated system for site-specific soil fertility management. This system includes a sensor platform, which contains different sensors, like XRF, VIS-NIR, Gamma and LIBS. The main task of LIBS measurements in this project is the real time determination of the elemental contents of major and minor nutrients in soils, like calcium, magnesium, potassium. For this purpose, a special setup has been designed. The sample uptake operates with the help of a rotatable sample plate, on which the loose soil sample can be placed in form of a track. The sample plate circulates with different velocities to simulate the application on the field. To provide a higher intensity and a better re-producibility of the obtained signal, a double-pulse Nd:YAG laser (1064 nm) was used. In order to minimize dust formation from the soil during the operation of the laser, a dust removal by suction has been integrated When using relative methods such as LIBS, a suitable calibration curve is needed for absolute quantification. Within the I4S project a large number of soil samples from different testing grounds with known data of chemical composition, texture etc. is available. For the first calibration curves seven soil samples from different grounds in Germany were prepared as reference materials and four certified reference materials from China and Canada were purchased. With the help of these reference materials, calibration curves for different elements were initially calculated based on internal standard addi-tion. Copper was used as internal standard because of its low concentration in soils. The complex matrix of soils, as well as the influence of moisture and grain size in soils makes the absolute quantification by LIBS challenging. To overcome these influences, a calibration curve based on multivariate analysis was generated. Therefore, baseline correction on the second derivative with a Savitzky-Golay filter was followed by a partial least squares regression (PLSR). Multivariate analysis leads to noise reduction and neglection of interfering signals. Therefore, a better correlation between signal intensity and nutrient concentration is observed and a robust calibration curve is obtained. T2 - 9. Euro-Mediterranes Symposium LIBS CY - Pisa, Italy DA - 11.06.2017 KW - LIBS KW - Soil KW - Matrix KW - Multi-element PY - 2017 AN - OPUS4-40807 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gebbers, R. T1 - Laser-induced breakdown spectroscopy (LIBS) for efficient quantitative determination of elemental plant nutrients in soils: A contribution to precision agriculture N2 - One important aim of precision agriculture (PA) is the optimization of crop growth by means of site-specific measures, e.g. fertilizer application. Thus, PA should contribute to a resource efficient and ecofriendly soil management. Due to the expenses associated with traditional methods of soil analysis, requiring sample collection and laboratory analysis, PA technologies are still not in widespread use. Therefore, the aim of the project “I4S – Integrated System for Site-Specific Soil Fertility Management” is the development of a field-deployed, sensor-based analysis system offering rapid, cost-effective and spatially-resolved fertilizer recommendations. In this system, laser-induced breakdown spectroscopy (LIBS) could be ideally suited to assessing elemental nutrient contents of soils. In addition to low cost, durability and small size, a reliable quantification procedure is a crucial requirement for such a system. However, the texture as well as the composition of the soil can affect the spectra. This matrix dependence is the key challenge to be addressed in the application of LIBS for soil evaluation. The focus of this work was the establishment of a LIBS method for soil analysis in a laboratory environment for future field application. Natural soil samples of various origins, textures and compositions were used to characterize the matrix dependence of the LIBS spectra. Reference samples were prepared by adding defined amounts of the target elements to the soils (standard addition). Signals not superimposed by peaks of other elements were identified for each element. The reference samples also provided calibration curves for the respective soil type when the initial concentrations in the soils were taken into account. Additionally, the common laboratory method ICP-OES following aqua regia extraction was used to obtain reference values. Various approaches of calibration free evaluation of the data were also evaluated. In addition to traditional single-pulse experiments, the advantages of dual-pulse LIBS in relation to signal intensity, reproducibility as well as overcoming the matrix dependence of soil spectra were investigated. These methods were subsequently applied to validation samples collected on a dense grid within a field. T2 - Pedometrics 2017 CY - Wageningen, The Netherlands DA - 26.06.2017 KW - LIBS KW - Precision KW - Agriculture KW - Soil KW - Site-specific PY - 2017 AN - OPUS4-40808 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riaz, Muhammad T1 - Effect of modification on acidity and porosity of natural zeolite clinoptilolite N2 - 1. Introduction Catalytic processing of heavy feedstock can meet the increased demand of energy up to a great extent. It requires the application of acidic catalysts like zeolites. However, the used synthetic catalysts are difficult to recover and reuse and are mostly spent. The use of natural zeolite as spent catalysts may open new perspectives in the chemical use of heavy feed feedstock by chemical conversion. Natural zeolites are not expensive, widely available and environment friendly. Clinoptilolite is a natural, most abundant medium pore size zeolite, consisting of 2-deminsional pore system containing of oxygen-8- membered and oxygen-10-membered rings.Although clinoptilolite is porous and can be acidified by ion exchange or acid treatment. Samples were characterized by XRD regarding crystallinity and phase composition. The acidity was studied by ammonia-TPD measurements and 1H solid state MAS NMR as well as REDOR experiments. Structure and structural changes caused by applied modifications were studied by 27Al- and 29Si MAS NMR measurements and thermal analysis. 2. Experimental Part The ion exchange behaviour of natural zeolite tuff contained ca. 90 ma. % of clinoptilite was studied in 0.1 and 0.5 M ammonium nitrate solution and for comparison with HCl solution of similar concentration. The activation temperature was varied between 300-600°C.The catalytic test was performed using ca. 0.2 g of the catalyst and ca.10g of the aldehyde and alcohol using toluene as solvent and under reflux. Reaction water was removed via a by-pass. 3. Results and discussion The experiments show that a part of the cations of clinoptilolite readily exchange with ammonium ions and protons supplied by acid treatment. Substitution of the compensating cations by NH4+ followed by calcination and HCl treatment does not produce structural changes in the original material, but it opens the channels and increases acidity and thermal stability. Calcination at higher temperature and exchange with concentrated acid has a more severe impact on the clinoptilolite structure dealumination as indicated by the appearance of 5- and 6-fold coordinated aluminum. Catalytic activity of sample is related to the surface acidity. The presence of acidic protons of medium to strong strength is confirmed by ammonia-TPD and proton NMR measurements. 4. Conclusions Acidic natural clinoptilolite catalysts prepared via ammonium exchange followed by calcination and acid treatment shows a positive influence on acidity and porosity. Modification creates hierarchical micro-nano porosity. The specific surface area varies between ca. 45 m2/g and 245 m2/g. T2 - Catalysis summer school-UK CY - Liverpool, UK DA - 17.07.2017 KW - Natural Zeolite Clinoptilolite PY - 2017 AN - OPUS4-40689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Muhammad, Riaz T1 - Effect of the ammonium ion exchange and HCl treatment on the acidity of natural zeolite clinoptilolite N2 - Clinoptilolite is a natural, medium pore size, zeolite. It contains a 2-deminsional pore system containing of oxygen-8- membered and oxygen-10-membered rings. It is one of the most abundant natural zeolites. Clinoptilolite has a crystalline structure showing unique ion exchange and sorption properties. It is mainly used as ion exchanger and adsorbent for removal of toxic elements and compounds from the environment. The use of natural zeolite as spent catalysts may open new perspectives in the chemical use of heavy feed feedstock by chemical conversion. Natural zeolites are not expensive, widely available and environment friendly. Clinoptilolite is the most abundant natural zeolite. Although clinoptilolite is a potential acid catalyst, reports on its application in catalysis are limited so far. This contribution deals with the modification of the acidity of the natural zeolite clinoptilolite, the characterization of the acid sites and the catalytic activity in the Brønsted acid catalyzed acetalization of benzaldehyde with butandiol-1,3. The samples were acidified by via ammonium-ion exchange followed by calcination and acid treatment. The obtained catalysts were characterized by XRD regarding crystallinity and phase composition. The morphology was studied by TEM images The acidity was studied by ammonia-TPD measurements and 1H solid state MAS NMR as well as REDOR experiments. Structure and structural changes caused by applied modifications were studied by 27Al- and 29Si MAS NMR measurements and thermal analysis. The ion experiments show that a part of the cations of clinoptilolite readily exchange with ammonium ions and protons from HCl treatment. The NMR results give first hints for a relation of the catalytic conversion with the presence of 5-fold coordinated aluminum. The results will be discussed in terms of a collaborative action of Brønsted acid sites and 5-fold coordinated aluminum. T2 - Deutsche Zeolith Tagung-2017 CY - Frankfurt Germany DA - 01.03.2017 KW - Natural zeolite clinoptilolite PY - 2017 AN - OPUS4-40684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riaz, Muhammad T1 - Influence of the acidic, thermal, and water vapour treatment on the catalytic performance of acidic hierarchical structured clinoptilolite N2 - Clinoptilolite is a natural, medium pore size zeolite. It contains a 2-deminsional pore system consisting of oxygen-8- membered and oxygen-10-membered rings. It is one of the most abundant natural zeolites. It is mainly used as ion exchanger and adsorbent for removal of toxic elements and compounds from the environment. Although clinoptilolite is microporous and can be acidified by ion exchange or acid treatment and a potential catalyst, reports on its application in catalysis are limited so far. This contribution deals with modification of a natural zeolite clinoptilolite, and the study of the influence of the textural and acidic properties on the catalytic performance in the acid catalyzed acetalization of bezaldehyde with butandiol-1,3 and the more demanding etherification of glycerol with t-butanol or isomerization of n-hexane. The samples were acidified by via ammonium-ion exchange followed by calcination and acid treatment. Samples were characterized by XRD regarding crystallinity and phase composition, FTIR, and N2-adsorption for porosity. The morphology was studied by TEM images. The acidity was studied by ammonia-TPD measurements and 1H solid state MAS NMR. Structure and structural changes caused by applied modifications were studied by 27Al- and 29Si MAS NMR measurements and TRAPDOR experiments as well as thermal analysis. The studied natural zeolite tuff contained ca. 90 ma.-% of clinoptilolite. The ion exchange behavior was studied with ammonium nitrate solution and for comparison with HCl solution of similar concentration. The cation exchange was followed by AES. The activation temperature was varied between 400-600°C. The catalytic test was performed e.g. using ca. 0.2 g of the catalyst and ca.10g of the aldehyde or alcohol using toluene as solvent and under reflux. Reaction water was removed via a by-pass. The isomerization of n-hexane was performed in a fall stream reactor at elevated temperature at gas phase. Water vapour saturated air was passed over clinoptilolite samples at elevated temperature for different time. The ion exchange experiments shows that ca 45% of the cations of clinoptilolite readily exchange with ammonium ions and protons supplied by acid treatment. However, exchange with the acid has a more severe impact on the clinoptilolite structure. More severe treatment times leads to a loss of activity in terms of acetal formation. Sample show all high conversions after 4 h of reaction, but show markedly differences after short reaction times. The presence of acidic protons of medium to strong strength is confirmed by ammonia-TPD and proton NMR measurements. The sample activation causes a partial dealumination as indicated by the appearance of 5- and 6-fold coordinated aluminum. Interestingly, the NMR results give first hints for a relation of the catalytic conversion with the amount of 5-fold coordinated aluminum. The results will be discussed in terms of a collaborative action of Brønsted acid sites and 5-fold coordinated aluminum. Modified clinoptilpolite is highly active in acid catalyst acetalization of aldehydes, isomerization of n-hexane and etherification of glycerol with t-butanol. Acidic natural clinoptilolite catalysts prepared via ammonium exchange followed by calcination and acid treatment shows a positive influence on acidity and porosity. Modification creates hierarchical micro-nano porosity. The specific surface area varies between ca. 45 m2/g and 257 m2/g. T2 - EUROPA CAT 2017 CY - Florence Italy DA - 27.08.2017 KW - Natural Zeolite Clinoptilolite PY - 2017 AN - OPUS4-40687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Material properties and their impact on laserinduced plasmas for concrete analysis N2 - For concrete production aggregates, cement and water are mixed together and after 28 days of hydration a porous and multiphase material is formed. To consider the heterogeneity of concrete a 2D scanning system is used. The coarse aggregates (limit > 2 X d ) can be excluded. laser spot The remaining content is a mixture of flour grains and cement particles (micro heterogeneity). Harmful species like chlorides may penetrate together with water through the capillary pore space. A quantification of Cl regarding to the cement content only (European standard EN 206) is necessary for the damage assessment. A LIBS system operating with a NdCr:YAG laser (pulse energy of 3 mJ, a wavelength of 1064 nm, a pulse width of 1.5 ns, a repetition rate of 100 Hz) and two Czerny-Turner spectrometer (UV and NIR range) have been used. T2 - EMSLIBS Konferenz 2017 CY - Pisa, Italy DA - 12.06.2017 KW - Concrete KW - LIBS KW - Micro-heterogeneity PY - 2017 AN - OPUS4-40938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tütken, T. A1 - Tatzel, Michael A1 - Vogl, Jochen A1 - Rosner, M. T1 - Assessing δ26Mg in bioapatite as proxy for faunivory N2 - Knowledge about feeding behavior is essential to determine trophic interactions and reconstruct predator-prey relationships in modern and past foodwebs. Traditionally, nitrogen isotopes (δ15N) of collagen are used to quantify the ingestion of animal protein, however collagen usually does not preserve over geological time scales. To infer the diet of extinct vertebrates from fossil material more resistant dietary proxies such as Ca and Mg isotopes are needed, which are major elements in the bioapatite of bones and teeth. Magnesium is a bio-essential element that replaces calcium in the bioapatite lattice and bone and enamel δ26Mg values of extant mammals increase systematically along the foodchain [1, 2]. The existing δ26Mg data, however, is scarce, in particular with respect to carnivores, thus still limiting the capability of this dietary proxy to reliably determine trophic differences between plant- and animal-feeders. To better constrain trophic-level effects recorded in Mg isotopes, we analyzed δ26Mg of bioapatite from modern mammals with a focus on faunivores, both carnivores and as yet unexplored insectivores. The trophic level effect of δ26Mg is influenced by the geological substrate which causes isotope variability in δ26Mg of faunal remains between different ecosystems [1, 2]. Therefore, as first-order proxy for sample provenance and to assess potential influences of the bedrock substrate of the animals´ habitats on δ26Mg of bones and teeth, we measured the 87Sr/86Sr on the same specimens. This information will enable us to refine trophic level effects and determine whether δ26Mg can be used to distinguish different faunivores isotopically. This will be of paramount importance for dietary reconstructions of trophic niches in fossil foodwebs. [1] Martin et al. (2014) Geochmica Cosmochimica Acta 130, 12-20. [2] Martin et al. (2015) Proceedings of the National Academy of Sciences 112, 430-435. T2 - Goldschmidt CY - Paris, France DA - 13.08.2017 KW - Magnesium stable isotopes KW - Isotope fractionation KW - Trophic level KW - 87Sr/86Sr KW - Provenance PY - 2017 AN - OPUS4-41535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram T1 - Mathematical and statistical tools for online NMR spectroscopy in chemical processes N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied, which are calibration intensive. NMR spectroscopy has a high potential for direct loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and harsh environments for advanced process monitoring and control. Within the European Union’s Research Project CONSENS (Integrated CONtrol and SENsing by development and integration of a smart NMR module for process monitoring was designed and delivers online spectra of various reactions. The presented NMR module is provided in an explosion proof housing of 57 x 57 x 85 cm module size and involves a compact spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction), and evaluation. For reaction monitoring and process control using NMR instruments after acquisition of the FID the data needs to be corrected in real-time for common effects using fast interfaces and automated methods. When it comes to NMR data evaluation under industrial process conditions, the shape of signals can change drastically due to nonlinear effects. Additionally, the multiplet structure becomes more dominant because of the comparably low-field strengths which results in overlapping of multiple signals. However, the structural and quantitative information is still present but needs to be extracted by applying predictive models. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). By using the benefits of traditional qNMR experiments data analysis models can meet the demands of the PAT community (Process Analytical Technology) regarding low calibration effort/calibration free methods, fast adaptions for new reactants, or derivatives and robust automation schemes. T2 - Advanced Mathematical and Computational Tools in Metrology and Testing XI (AMCTM) CY - Glasgow, UK DA - 29.08.2017 KW - Process Monitoring KW - CONSENS KW - Online NMR Spectroscopy KW - Indirect Hard Modeling KW - Data Analysis PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-416560 AN - OPUS4-41656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - In situ investigations of mechanochemical Knoevenagel condensations N2 - Mechanaochemistry is an effecthive method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions. T2 - INCOME2017 CY - Kosice, Slovakia DA - 03.09.2017 KW - C-C coupling KW - Mechanochemistry KW - Knoevenagel condensation KW - Synchrotron KW - In situ PY - 2017 AN - OPUS4-41845 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sahre, Mario T1 - Electroplated magnetostrictive actuator layer enabling the external diagnosis of strain sensors N2 - Embedded fibre-opticaloptical strain sensors are suitable for structural health monitoring. In order to validate long-term performance (e.g.sensors integrated in airplane wings or wind power turbine blades) an external diagnostics is required. A strain-detecting region of the optical fibre, the fibre Bragg grating (FBG, is encased by a magnetostrictive layer system serving as actuator. For the validation of the correct sensor function, an external magnetic field introduces mechanical strain resulting in a defined shift of the Bragg wavelength. The layer system is realized by acombined PVD /ECD process optimized regarding magnetostrictive and mechanical properties. The long -term stability of layer adhesion and actuator function has been verified. T2 - 12. Thementage Grenz- und Oberflächentechnik (ThGOT) und das 5. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Germany DA - 14.03.2017 KW - Magnetostrictive actuator layer KW - PVD /ECD process KW - Magnetostrictive layer KW - Strain sensors PY - 2017 AN - OPUS4-41800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -