TY - JOUR A1 - Merkel, Stefan A1 - Köppen, Robert A1 - Koch, Matthias A1 - Emmerling, Franziska A1 - Nehls, Irene T1 - Ergotaminine N2 - The title compound {systematic name: (6aR,9S)-N-[(2R,5S,10aS,10bS)-5-benzyl-10b-hydroxy-2-methyl-3,6-dioxooctahydro-8H-oxazolo[3,2-a]pyrrolo[2,1-c]pyrazin-2-yl]-7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide}, C33H35N5O5, was formed by an epimerization reaction of ergotamine. The non-aromatic ring (ring C of the ergoline skeleton) directly fused to the aromatic rings is nearly planar [maximum deviation = 0.317 (4) Å] and shows an envelope conformation, whereas ring D, involved in an intramolecular N–H···N hydrogen bond exhibits a slightly distorted chair conformation. The structure displays chains running approximately parallel to the diagonal of bc plane that are formed through N–H···O hydrogen bonds. PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-254528 DO - https://doi.org/10.1107/S1600536812003674 SN - 1600-5368 VL - 68 IS - 3 SP - o610-o611, sup1-sup11 PB - Munksgaard CY - Copenhagen AN - OPUS4-25452 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Merkel, Stefan A1 - Köppen, Robert A1 - Koch, Matthias A1 - Emmerling, Franziska A1 - Nehls, Irene T1 - Lysergol monohydrate N2 - In the title compound [systematic name: (7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3,2-fg]quinoline-9-yl)methanol monohydrate], C16H18N2O·H2O, the non-aromatic ring (ring C of the ergoline skeleton) directly fused to the aromatic rings is nearly planar, with a maximum deviation of 0.659 (3) Å, and shows an envelope conformation. In the crystal, hydrogen bonds between the lysergol and water molecules contribute to the formation of layers parallel to (10-2). PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-254015 DO - https://doi.org/10.1107/S1600536812002632 SN - 1600-5368 VL - 68 IS - 2 SP - o523, sup1 EP - sup8 PB - Munksgaard CY - Copenhagen AN - OPUS4-25401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weller, Michael G. T1 - A unifying review of bioassay-guided fractionation, effect-directed analysis and related techniques N2 - The success of modern methods in analytical chemistry sometimes obscures the problem that the ever increasing amount of analytical data does not necessarily give more insight of practical relevance. As alternative approaches, toxicity- and bioactivity-based assays can deliver valuable information about biological effects of complex materials in humans, other species or even ecosystems. However, the observed effects often cannot be clearly assigned to specific chemical compounds. In these cases, the establishment of an unambiguous cause-effect relationship is not possible. Effect-directed analysis tries to interconnect instrumental analytical techniques with a biological/biochemical entity, which identifies or isolates substances of biological relevance. Successful application has been demonstrated in many fields, either as proof-of-principle studies or even for complex samples. This review discusses the different approaches, advantages and limitations and finally shows some practical examples. The broad emergence of effect-directed analytical concepts might lead to a true paradigm shift in analytical chemistry, away from ever growing lists of chemical compounds. The connection of biological effects with the identification and quantification of molecular entities leads to relevant answers to many real life questions. KW - Toxicity KW - Drug discovery KW - Natural products KW - Environmental analysis KW - Lead identification PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-262960 DO - https://doi.org/10.3390/s120709181 SN - 1424-8220 VL - 12 IS - 7 SP - 9181 EP - 9209 PB - MDPI CY - Basel AN - OPUS4-26296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jeromenok, J. A1 - Böhlmann, W. A1 - Jäger, Christian A1 - Weber, J. T1 - Carbon dioxide adsorption in Betulin-based micro- and macroporous polyurethanes N2 - Separation of CO2. Microporous polyurethane networks were prepared based on a renewable resource. Betulin, extracted from birch bark, is used as a structure-directing diol monomer in A3-B2 monomers. The resulting microporous networks show very promising CO2/N2 selectivities. The state of adsorbed CO2 is analyzed by in situ NMR spectroscopy, and pure physisorption is proven. The preparation of monolithic materials is demonstrated as well. KW - Carbon dioxide KW - Gas adsorption KW - Microporous polymers KW - Renewable resources KW - Solid state NMR spectroscopy PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-304431 DO - https://doi.org/10.1002/open.201200045 SN - 2191-1363 VL - 2 IS - 1 SP - 17 EP - 20 PB - Wiley-VCH-Verl. CY - Weinheim AN - OPUS4-30443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Asadi, S. A1 - Hernandez Bennetts, V. A1 - Lilienthal, A.J. A1 - Bartholmai, Matthias T1 - Monitoring of CCS areas using micro unmanned aerial vehicles (MUAVs) N2 - Carbon capture & storage (CCS) is one of the most promising technologies for greenhouse gas (GHG) management. However, an unsolved issue of CCS is the development of appropriate long-term monitoring systems for leak detection of the stored CO2. To complement already existing monitoring infrastructure for CO2 storage areas, and to increase the granularity of gas concentration measurements, a quickly deployable, mobile measurement device is needed. In this paper, we present an autonomous gas-sensitive micro-drone, which can be used to monitor GHG emissions, more specifically, CO2. Two different measurement strategies are proposed to address this task. First, the use of predefined sensing trajectories is evaluated for the task of gas distribution mapping using the micro-drone. Alternatively, we present an adaptive strategy, which suggests sampling points based on an artificial potential field (APF). The results of real-world experiments demonstrate the feasibility of using gas-sensitive micro-drones for GHG monitoring missions. Thus, we suggest a multi-layered surveillance system for CO2 storage areas. T2 - GHGT 11 - Greenhouse gas control technologies conference CY - Kyoto, Japan DA - 18.11.2012 KW - Gas-sensitive micro-drone KW - Gas distribution mapping KW - Sensor planning KW - Artificial potential field KW - CCS PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-289119 DO - https://doi.org/10.1016/j.egypro.2013.06.320 SN - 1876-6102 VL - 37 SP - 4182 EP - 4190 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-28911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schütz, Roman A1 - Bertinetti, L. A1 - Rabin, Ira A1 - Fratzl, P. A1 - Masic, A. T1 - Quantifying degradation of collagen in ancient manuscripts: the case of the Dead Sea Temple Scroll N2 - Since their discovery in the late 1940s, the Dead Sea Scrolls, some 900 ancient Jewish texts, have never stopped attracting the attention of scholars and the broad public alike, because they were created towards the end of the Second Temple period and the 'time of Christ'. Most of the work on them has been dedicated to the information contained in the scrolls' text, leaving physical aspects of the writing materials unexamined. They are, however, crucial for both historical insight and preservation of the scrolls. Although scientific analysis requires handling, it is essential to establish the state of degradation of these valued documents. Polarized Raman Spectroscopy (PRS) is a powerful tool for obtaining information on both the composition and the level of disorder of molecular units. In this study, we developed a non-invasive and non-destructive methodology that allows a quantification of the disorder (that can be related to the degradation) of protein molecular units in collagen fibers. Not restricted to collagen, this method can be applied also to other protein-based fibrous materials such as ancient silk, wool or hair. We used PRS to quantify the degradation of the collagen fibers in a number of fragments of the Temple Scroll (11Q19a). We found that collagen fibers degrade heterogeneously, with the ones on the surface more degraded than those in the core. KW - Dead Sea Scrolls KW - Collagen KW - Raman spectroscopy PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-331769 DO - https://doi.org/10.1039/c3an00609c SN - 0003-2654 SN - 1364-5528 VL - 138 IS - 19 SP - 5594 EP - 5599 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-33176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brosig, Laura A1 - Horn, Wolfgang A1 - Pyza, Lars A1 - Jann, Oliver A1 - Plehn, W. T1 - Round robin test for the implementation of odour measurements according to DIN ISO 16000-28 into the assessment of emissions from building products N2 - Odour measurements become increasingly important in view of the assessment of indoor air quality and the emissions of building products. Hence they need to be implemented into evaluation schemes such as the AgBB scheme. While there are already standards like DIN ISO 16000-28 and VDI 4302 Part 1 specifying the procedure of odour measurements using a comparison scale, no final validation of the method has been carried out so far. Therefore, a round robin test was conducted in 2012 with 12 participating laboratories that mainly consisted of the following two parts: 1) testing of the available comparison scales with respect to their operational performance and 2) execution of an odour assessment of an acrylic sealant using emission test chambers. Part one included the measurement of the air flow rates and the provided concentrations of the reference substance (acetone). Part two was conducted to test the performance of the laboratories and the applicability of DIN ISO 16000-28 and supplementary VDI 4302 Part 1 by assessing the perceived intensity and the hedonic tone of the air samples. Moreover, samples for VOC analysis were taken from the air in the emission test chamber on the 7th day of testing to allow for quality control. Resulting from this round robin test main deficits were detected and suggestions for the improvement of the odour measurement procedure were made. N2 - Im Rahmen der Bewertung von Innenraumluftqualität und von Emissionen aus Bauprodukten gewinnt auch die Beurteilung entstehender Gerüche zunehmend an Bedeutung. Um der daraus resultierenden Forderung nach Geruchsbewertungen gerecht zu werden, müssen entsprechende Methoden in bestehende Bewertungssysteme, wie z. B. das AgBB-Schema, aufgenommen werden. Als Grundlage hierfür bieten sich die bereits bestehenden Regelwerke DIN ISO 16000-28 und VDI 4302 Blatt 1 an, die das Vorgehen bei Geruchsmessungen unter Verwendung eines Vergleichsmaßstabes vorgeben. Da für die beschriebene Methode bisher keine Validierung vorliegt, wurde 2012 ein Ringversuch mit zwölf Instituten durchgeführt, der sich hauptsächlich aus zwei Teilen zusammensetzte: 1) Überprüfung der technischen Funktionsfähigkeit der verwendeten Vergleichsmaßstäbe und 2) Durchführung einer Geruchsbewertung für eine Acryldichtmasse mithilfe von Emissionsprüfkammern. Im ersten Teil wurden sowohl die Volumenströme als auch die bereitgestellten Konzentrationen der Referenzsubstanz Aceton bestimmt. Der zweite Teil diente neben der Ermittlung der Leistungsfähigkeit der Laboratorien vor allem der Feststellung, inwieweit eine Bestimmung der empfundenen Intensität und der Hedonik nach DIN ISO 16000-28, ergänzt durch VDI 4302 Blatt 1, einheitlich möglich ist. Aus Gründen der Vergleichbarkeit und der Qualitätskontrolle wurden am siebten Tag der Messungen zusätzlich Proben der Prüfkammerluft zur VOC-Bestimmung genommen. Mithilfe des Ringversuchs konnten Defizite sowohl technischer als auch methodischer Art festgestellt und Vorschläge für die Verbesserung des Vorgehens bei Geruchsbewertungen erarbeitet werden. PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-293110 UR - http://www.gefahrstoffe.de/gest/article.php?data[article_id]=75118 SN - 0949-8036 SN - 0039-0771 SN - 1436-4891 VL - 73 IS - 10 SP - 441 EP - 445 PB - Springer-VDI-Verlag CY - Düsseldorf AN - OPUS4-29311 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Grabolle, Markus A1 - Pauli, Jutta A1 - Spieles, Monika A1 - Resch-Genger, Ute T1 - Relative and absolute determination of fluorescence quantum yields of transparent samples N2 - Luminescence techniques are among the most widely used detection methods in the life and material sciences. At the core of these methods is an ever-increasing variety of fluorescent reporters (i.e., simple dyes, fluorescent labels, probes, sensors and switches) from different fluorophore classes ranging from small organic dyes and metal ion complexes, quantum dots and upconversion nanocrystals to differently sized fluorophore-doped or fluorophore-labeled polymeric particles. A key parameter for fluorophore comparison is the fluorescence quantum yield (Φf), which is the direct measure for the efficiency of the conversion of absorbed light into emitted light. In this protocol, we describe procedures for relative and absolute determinations of Φf values of fluorophores in transparent solution using optical methods, and we address typical sources of uncertainty and fluorophore class-specific challenges. For relative determinations of Φf, the sample is analyzed using a conventional fluorescence spectrometer. For absolute determinations of Φf, a calibrated stand-alone integrating sphere setup is used. To reduce standard-related uncertainties for relative measurements, we introduce a series of eight candidate quantum yield standards for the wavelength region of ~350–950 nm, which we have assessed with commercial and custom-designed instrumentation. With these protocols and standards, uncertainties of 5–10% can be achieved within 2 h. PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-294202 DO - https://doi.org/10.1038/nprot.2013.087 SN - 1754-2189 SN - 1750-2799 VL - 8 IS - 8 SP - 1535 EP - 1550 PB - Nature Publishing Group CY - Basingstoke AN - OPUS4-29420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lopez-Heredia, M.A. A1 - Gildenhaar, Renate A1 - Berger, Georg A1 - Linow, Ulf A1 - Wirth, Cynthia A1 - Günster, Jens A1 - Houshmand, A. A1 - Stiller, M. A1 - Knabe-Ducheyne, C. T1 - Effect of stressed and unstressed cell culture environments on the viability of MC3T3 cells with calcium phosphates T2 - ISACB-6 - International symposium on apatite and correlative biomaterials CY - Nantes, France DA - 2013-06-05 KW - Cell culture media KW - Fetal bovine serum KW - Stressed KW - Unstressed KW - Calcium alkaline orthophosphates PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-299387 DO - https://doi.org/10.4172/2090-5025.S1-002 SN - 2090-5017 SN - 2090-5025 N1 - Geburtsname von Wirth, Cynthia: Gomes, C. M. - Birth name of Wirth, Cynthia: Gomes, C. M. SP - 1 EP - 3(?) PB - Ashdin AN - OPUS4-29938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pech, Anja A1 - Wilke, Olaf A1 - Mull, Birte A1 - Horn, Wolfgang A1 - Jann, Oliver T1 - Development of a TDS-GC-FID method for the determination of methanol and ethanol in air N2 - A method for the determination of very volatile organic compounds (VVOC) in air was developed and successfully tested for methanol and ethanol. Carbotrap300® (a multi-bed tube using Carbopack C®, Carbopack B® and Carbosive SIII®) was selected as sorption material for thermal desorption and tested for its suitability for emission test chamber measurements. The adsorption behaviour and the chromatographic results are influenced negatively by spiking aqueous solutions on the adsorption medium for calibration purposes. The latter effect can be reduced by blowing dry air across the adsorbent to remove the adsorbed water. Detection and quantification limits were determined for a GC-FID system and compared to GC-MS. The applicability of the method was tested with a methanol eliminating silane modified polymeric adhesive (SMP-adhesive for parquet) in an emission test chamber N2 - Eine Methode zur Bestimmung von sehr leicht flüchtigen Verbindungen in Luft wurde für Methanol und Ethanol entwickelt und erfolgreich getestet. Dafür wurde Carbotrap300® (Multibettrohr aus Carbopack C®, Carbopack B® und Carbosive SIII®) als Sorptionsmedium für die Thermodesorption ausgewählt und dessen Eignung für Emissionskammermessungen untersucht. Das Adsorptionsverhalten und die chromatographischen Ergebnisse werden negativ durch die Aufgabe von wässrigen Kalibrierlösungen auf das Adsorptionsmedium beeinflusst. Durch das Überleiten von trockener Luft kann dieser Effekt verringert werden, da so das adsorbierte Wasser entfernt wird. Die Nachweis- und Bestimmungsgrenzen wurden für ein eingesetztes GC- FID-System ermittelt und mit einem GC-MS verglichen. Mit einem methanolabspaltenden silanmodifizierten Polymerklebstoff (SMP-Parkettkleber), der in eine Emissionskammer eingebracht wurde, konnte die Tauglichkeit der Methode überprüft werden. PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-297020 UR - http://www.gefahrstoffe.de/gest/article.php?data[article_id]=76019 SN - 0949-8036 SN - 0039-0771 SN - 1436-4891 VL - 73 IS - 11/12 SP - 477 EP - 482 PB - Springer-VDI-Verlag CY - Düsseldorf AN - OPUS4-29702 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -