TY - JOUR A1 - Oesch, Tyler A1 - Weise, Frank A1 - Bruno, Giovanni T1 - Detection and Quantification of Cracking in Concrete Aggregate through Virtual Data Fusion of X-ray Computed Tomography Images JF - Materials N2 - In this work, which is part of a larger research program, a framework called “virtual data fusion“ was developed to provide an automated and consistent crack detection method that allows for the cross-comparison of results from large quantities of X-ray Computed Tomography (CT) data. A partial implementation of this method in a custom program was developed for use in research focused on crack quantification in Alkali-Silica Reaction (ASR)-sensitive concrete aggregates. During the CT image processing, a series of image analyses tailored for detecting specific, individual crack-like characteristics were completed. The results of these analyses were then “fused” in order to identify crack-like objects within the images with much higher accuracy than that yielded by any individual image analysis procedure. The results of this strategy demonstrated the success of the program in effectively identifying crack-like structures and quantifying characteristics, such as surface area and volume. The results demonstrated that the source of aggregate has a very significant impact on the amount of internal cracking, even when the mineralogical characteristics remain very similar. River gravels, for instance, were found to contain significantly higher levels of internal cracking than quarried stone aggregates of the same mineralogical type. KW - X-ray Computed Tomography (CT) KW - Alkali-Silica Reaction (ASR) KW - Crack Detection KW - Damage Quantification KW - ASR-Sensitive Aggregate PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512170 DO - https://doi.org/10.3390/ma13183921 VL - 13 IS - 18 SP - Paper 3921 PB - MDPI CY - Basel, Switzerland AN - OPUS4-51217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Wolf, M. A1 - Alentiev, D. A1 - Bermeshev, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Low frequency vibrational density of state of highly permeable super glassy polynorbornenes – The Boson peak JF - Physical Chemistry Chemical Physics N2 - Inelastic incoherent neutron time-of flight scattering was employed to measure the low frequency density of states for a series of addition polynorbornenes with bulky side groups. The rigid main chain in combination with the bulky side groups give rise to a microporosity of these polymers in the solid state. The microporosity characterized by the BET surfaces area varies systematically in the considered series. Such materials have some possible application as active separation layer in gas separation membranes. All investigated materials show excess contributions to the Debye type density of states characteristic for glasses known as Boson peak. The maximum position of the Boson peak shifts to lower frequency values with increasing microporosity. Data for PIM-1 and Matrimid included for comparison are in good agreement to this dependency. This result supports the sound wave interpretation of the Boson peak. KW - Polynorbornes KW - Neutron Scattering PY - 2020 DO - https://doi.org/10.1039/d0cp03360j SN - 1463-9076 VL - 22 IS - 33 SP - 18381 EP - 18387 PB - Royal Chemical Society AN - OPUS4-51165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolmangadi, Mohamed Aejaz A1 - Szymoniak, Paulina A1 - Smales, Glen Jacob A1 - Alentiev, D. A1 - Bermeshev, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Molecular Dynamics of Janus Polynorbornenes: Glass Transitions and Nanophase Separation JF - Macromolecules N2 - For the first time, dielectric and calorimetric investigations of an homologous series of Janus polynorbornenes with rigid main backbones and flexible -Si(OR)3 side groups, of differing length alkyl chains (R = Propyl, Butyl, Hexyl, Octyl, Decyl) is reported. Generally, this class of polymers has some potential for applications in the field of gas separation membranes. Two dielectrically active processes are observed at low temperatures, denoted as β- and α- relaxation. The former can be assigned to localized fluctuations, whilst the latter is related to the glassy dynamics of the flexible -Si(OR)3 side groups, creating a nanophase separation in both the alkyl chain rich and backbone rich domains. This is confirmed through temperature modulated DSC measurements and X-ray scattering experiments. The glass transition temperatures of the backbone rich domains, which are beyond or near to their degradation temperatures in terms of conventional DSC, are determined for the first time using Fast Scanning Calorimetry employing both fast heating and cooling rates. This is complimented with scattering experiments that show how the size of the alkyl chain rich domains increases with chain length. Alongside these results, a significant conductivity contribution was observed for all poly(tricyclononenes) with -Si(OR)3 side groups, which is interpreted in terms of a percolation model. KW - Polynorbornenes KW - Broadband Dielectric Spectrscopy KW - Advanced calorimetry PY - 2020 DO - https://doi.org/10.1021/acs.macromol.0c01450 VL - 53 IS - 17 SP - 7410 EP - 7419 PB - ACS AN - OPUS4-51196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bäßler, Ralph T1 - Rezension: Analytik - Daten, Formeln, Übungsaufgaben T2 - Materials and Corrosion N2 - Seit seiner erstmaligen Veröffentlichung im Jahre 1894 als „Logarithmische Rechentafeln für Chemiker“ und ab 1982 als „Rechentafeln für die chemische Analyse“ begleitet der „Küster‐Thiel“ Generationen nicht nur von Laborantinnen und Laboranten sowie Studierende hilfreich bei der analytischen Arbeit. Mit der 108. Auflage änderte sich 2016 der Titel dieses in der „Studium“‐Reihe des De Gruyter Verlages herausgegebenen Standardwerkes ein weiteres Mal. Die 109. Auflage des Klassikers der chemischen Analytik‐Literatur setzt die Tradition fort, mit zahlreichen anschaulichen Erklärungen, Beispiele und Rechnungen Chemikern, Physikern und Ingenieurswissenschaftlern an Universitäten und Fachhochschulen; Auszubildenden und Laboranten ein übersichtliches und aktuelles Arbeitsmittel für den analytischen Alltag zur Verfügung zu stellen. Nutzern früherer Ausgaben wird der Umstieg auf die neue Ausgabe empfohlen, damit auch sie auf dem neuesten Stand arbeiten können. KW - Analyse KW - Labor KW - Formeln KW - Laborarbeit PY - 2020 DO - https://doi.org/10.1002/maco.202070106 SN - 1521-4176 SN - 0947-5117 VL - 71 IS - 10 SP - 2 EP - 3 PB - WILEY‐VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-51415 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bäßler, Ralph T1 - Review: Polymer Coatings ‐ A Guide to Chemistry, Characterization, and Selected Applications T2 - Materials and Corrosion N2 - This book grew out of a course on polymer coatings held by the author at the university. It shall serve as an introduction to the wide field of polymer coatings. It is not intended to cover completely all facts on polymer coatings. All chapters are well structured. Selected figures and formulas illustrate the content and contribute to a good understandability. At the end of each chapter some hints for further reading are provided. Finally, the book fulfills its intention to introduce into the topic by providing basics on science and technology of polymer coatings, suitable for chemists in industry, materials scientists, polymer chemists and physical chemists. KW - Corrosion KW - Coating KW - Polymer PY - 2020 DO - https://doi.org/10.1002/maco.202070024 SN - 1521-4176 SN - 0947-5117 VL - 71 IS - 2 SP - 321 EP - 322 PB - WILEY‐VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-50374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy A1 - Stelzner, Ludwig A1 - Strangfeld, Christoph A1 - Kruschwitz, Sabine T1 - Ermittlung der Porosität von Sandsteinen - Vergleich von Quecksilberporosimetrie, Tauchwägung und NMR N2 - Die Porosität sowie die Porengrößenverteilung (PSD) eines Baustoffs sind wichtige petrophysikalische Eigenschaften, die Transportprozesse im Material beeinflussen und im direkten Zusammenhang mit der Schadensanfälligkeit stehen (Frost-Tau-Schäden, Schäden durch Salzeinträge und sauren Regen). Verfahren zur Ermittlung der Porosität stellen die Quecksilberporosimetrie (MIP), das Prinzip der Tauchwägung nach Archimedes (triple weighing method, TWM) und die Nuklear Magnetische Resonanz (NMR) dar. Das Hauptziel dieser Arbeit ist der Vergleich der drei Methoden für die Porositätsbestimmung. Als Untersuchungsmaterial wurde Sandstein gewählt. Als Baustoff wird Sandstein trotz einer teilweise geringen Festigkeit, aber aufgrund seiner Farbvielfalt häufig für Kulturbauten, Gehwegmaterial und Fassaden eingesetzt. Sandsteine weisen zudem meist eine hohe effektive Porosität (bis zu ca. 30 %) und teilweise breite Porengrößenspektren auf, wodurch Feuchte- und Ioneneinträge begünstigt werden und zu z. B. langfristigen Verfärbungen an Sandsteinfassaden führen können. Im Rahmen dieser Arbeit werden die Porositäten von 10 verschiedenen Sandsteinen aus Deutschland und Tschechien bestimmt. Für die Untersuchungen mittels TWM und NMR wurden für jede Sandsteinart zwei zylinderförmige Proben unter Unterdruck mit Leitungswasser aufgesättigt. Beim Vergleich der Verfahren liegt der Fokus insbesondere auf NMR und der verwendeten Gerätetechnik, die mit einer minimalen Echozeit von 50 µs ein Wasserstoffsignal in Sandsteinen aus bis zu ca. 2 nm kleine Poren erfassen kann. Darüber hinaus wird das Auflösungsvermögen von MIP und NMR bezüglich der Poren- bzw. Poreneingangsgrößen diskutiert. Für den Vergleich von NMR und MIP werden an ausgewählten Sandsteinproben ebenfalls die zusätzlich ermittelten PSD in Korrelation zueinander gebracht. Erste Ergebnisse zeigen eine gute Korrelation von NMR- und TWM-Daten, aber teilweise starke Abweichungen zu den mit MIP bestimmten Porositäten. Ergebnisse zu den PSD zeigen teilweise nahezu identische Kurvenverläufe. Jedoch ist die Abschätzung des Umrechnungsfaktors für die NMR-Daten ohne Hinzuziehen von zusätzlichen Referenzverfahren wie Röntgen-Computer-Tomographie oder Spektral Induzierte Polarisation teilweise sehr schwierig. T2 - Bauwerksdiagnose CY - Berlin, Germany DA - 13.02.2020 KW - NMR KW - Porosität KW - Sandsteine KW - Quecksilberporosimetrie KW - Tauchwägung PY - 2020 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-50405 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bäßler, Ralph T1 - Rezension: Einführung in die Physikalische Chemie T2 - Materials and Corrosion N2 - Unabhängig vom im Chemieunterricht erworbenen Wissensstand der Studienanfänger liefert dieses, in der Reihe „De Gruyter Studium“ erschienene Lehrbuch einen Einstieg in die Physikalische Chemie. Basierend auf den Erfahrungen seiner Lehrtätigkeit für Erstsemester der Fachrichtung Chemie an der Universität des Saarlandes geht der Autor auf beinahe alle Themengebiete der Physikalischen Chemie ein, wobei die Schwerpunkte auf klassischer Thermodynamik und Grundlagen der chemischen Bindung liegen. Dieses Lehrbuch ist nicht nur für Studierende im Bachelorstudium der Chemie sowohl im Haupt‐ als auch im Nebenfach geeignet. Es liefert zudem Interessierten anderer Fachrichtungen einen übersichtlichen und verständlichen Einstieg in die komplexe Welt der Physikalischen Chemie und sorgt für ein Grundverständnis. KW - Elektrochemie PY - 2020 DO - https://doi.org/10.1002/maco.202070126_2 SN - 1521-4176 SN - 0947-5117 VL - 71 IS - 12 SP - 3 EP - 4 PB - WILEY‐VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-51779 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesch, Tyler A1 - Weise, Frank A1 - Marx, Heidi A1 - Kositz, M. A1 - Huenger, K.-J. T1 - Analysis of the porosity of alkali-sensitive aggregates for the assessment of microstructure-dependent solubility in the context of ASR N2 - Intensified Alkali-Silica Reaction (ASR) damage has occurred on German roadways in recent years, leading to requirements for compulsory pre-construction investigation of aggregate alkali sensitivity using concrete tests with external alkali supply. However, since these tests are time-consuming and cost-intensive, there is interest in replacing them with a solubility test on pure aggregate in 0.1 M KOH solution at 80°C with a defined NaCl content (1wt.-%). In this context, the influence of aggregate pore structure on SiO2 and Al2O3 solubility was investigated in this project. This paper compares the results of porosity studies with X-ray Computed Tomography (3D-CT) and the Brunauer-Emmett-Teller (BET) method on individual quarried and river gravel granules of both rhyolite and greywacke. For visualization and quantification of both externally accessible and fully enclosed surfaces of granules using X-ray 3D-CT, special software tools were developed. The results demonstrated that the river gravel granules had significantly larger externally accessible surfaces than the quarried granules. BET measurements on individual stones showed, as expected, that measured surfaces were about three orders of magnitude larger than those from the X-ray 3D-CT analyses due to the higher spatial resolution of BET. There was no apparent correlation between the X-ray 3D-CT and BET surface areas. Mercury porosimetry measurements indicate that this may be due to the presence of significant porosity below the spatial resolution of the X-ray 3D-CT. A comparison of SiO2 and Al2O3 solubility measurements with the X-ray 3D-CT and BET surface area data resulted only in weak, inconclusive correlations, indicating the need for further experimental investigation. T2 - Microdurability Webinar CY - Online meeting DA - 12.10.2020 KW - X-ray Computed Tomography (CT) KW - Brunauer-Emmett-Teller (BET) Method KW - Alkali-Silica Reaction (ASR) KW - Porosity KW - Solubility PY - 2020 AN - OPUS4-51429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Goedecke, Caroline A1 - Dittmann, Daniel A1 - Eisentraut, Paul A1 - Wiesner, Yosri A1 - Schartel, Bernhard A1 - Klack, Patrick A1 - Braun, Ulrike T1 - Evaluation of thermoanalytical methods equipped with evolved gas analysis for the detection of microplastic in environmental samples JF - Journal of Analytical and Applied Pyrolysis N2 - Microplastic particles are currently detected in almost all environmental compartments. The results of detection vary widely, as a multitude of very different methods are used with very different requirements for analytical validity. In this work four thermoanalytical methods are compared and their advantages and limitations are discussed. One of them is thermal extraction-desorption gas chromatography mass spectrometry (TED-GC/MS), an analysis method for microplastic detection that has become established in recent years. In addition, thermogravimetric analysis coupled with Fourier-transform infrared spectroscopy (TGA-FTIR) and mass spectrometry (TGA-MS) were applied, two methods that are less common in this field but are still used in other research areas. Finally, microscale combustion calorimeter (MCC) was applied, a method not yet used for microplastic detection. The presented results are taken from a recently published interlaboratory comparison test by Becker et al. (2020). Here a reference material consisting of suspended matter and specified added polymer masses was examined, and only the results of the recoveries were presented. In the present paper, however, the results for the individual polymers are discussed in detail and individual perspectives for all instruments are shown. It was found that TED-GC/MS is the most suitable method for samples with unknown matrix and unknown, variable kinds and contents of microplastic. TGA-FTIR is a robust method for samples with known matrix and with defined kinds of microplastic. TGA-MS may offer a solution for the detection of PVC particles in the future. MCC can be used as a very fast and simple screening method for the identification of a potential microplastic load of standard polymers in unknown samples. KW - Microplastic KW - TED-GC/MS KW - TGA-MS KW - TGA-FTIR KW - MCC KW - Thermal analysis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-516687 DO - https://doi.org/10.1016/j.jaap.2020.104961 VL - 152 SP - 104961 PB - Elsevier B.V. AN - OPUS4-51668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Raschpichler, C. A1 - Goroncy, C. A1 - Langer, B. A1 - Antonsson, E. A1 - Wassermann, B. A1 - Graf, C. A1 - Klack, Patrick A1 - Lischke, T. A1 - Rühl, E. T1 - Surface Properties and Porosity of Silica Particles Studied by Wide-Angle Soft X-ray Scattering JF - Journal of Physical Chemistry C N2 - Wide-angle soft X-ray scattering on free silica particles of different porosity prepared in a beam is reported. The explored q region is mostly dominated by features due to surface roughness and bulk porosity. A comprehensive experimental and theoretical analysis of silica particles of different porosity is presented for various incident photon energies. A correlation analysis, based on the theory of Porod, is used to test the validity of exact Mie theory in different pore density limits. The ability of the discrete dipole scattering model (DDSCAT) to resolve local effects, caused by various pore distributions, is discussed. Characteristic differences between the soft X-ray scattering patterns of the particle samples of different surface properties and porosity are detected. For all mentioned cases, it was confirmed that the effective radius concept of the Guinier model can be successfully extended to Mie theory and DDSCAT in describing the additive contributions of the primary particles, including a thin inhomogeneous solvent-rich surface shell and empty bulk pores. Close agreement, within ±15%, between the calculated and observed pore sizes and porosity values is reached. The influence of pores is alternatively described either in terms of secondary Mie scattering, which is modulated by the local internal electrical field within the particles, or by an independent Mie scattering process induced by the incident field on isolated pores. It is found that for the typical pore/particle size ratios the latter approach presents the best choice. KW - Wide-Angle Soft X‑ray Scattering KW - Silica KW - Porosity PY - 2020 DO - https://doi.org/10.1021/acs.jpcc.0c04308 SN - 1932-7447 SN - 1932-7455 VL - 124 SP - 16663 EP - 16674 AN - OPUS4-51089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -