TY - JOUR A1 - Muelow-Stollin, Ulrike A1 - Lehnik-Habrink, Petra A1 - Kluge, Stephanie A1 - Bremser, Wolfram A1 - Piechotta, Christian T1 - Efficiency Evaluation of Extraction Methods for Analysis of OCPs and PCBs in Soils of Varying TOC N2 - Organochlorine pesticides and polychlorinated biphenyls are toxic, carcinogenic, and have a high potential for bioaccumulation. Due to their stability, they are still considered an environmental problem even though the use of most of them has been phased out several decades ago. Soil is a matrix which can retain these contaminants to a great extent. This ability is often associated with the total organic carbon content (TOC). In order to judge the pollution status of soil and to make monitoring data more easily comparable a simple, yet robust extraction method is needed. Agitation solid-liquid-extraction is well suited for this purpose. However, the influence of TOC on the analyte recovery has to be known. For the presented study, 12 organochlorine pesticides and 7 polychlorinated biphenyls were spiked into four model soils with organic carbon contents between 1.6% - 13.3%. The matrices were extracted using solid-liquid extraction between 45 minutes and 16 hours. For comparison, all soils were also extracted using pressurised liquid extraction and Soxhlet extraction. After clean-up the extracts were measured using a gas chromatography-mass spectrometry (GC-MS) system. Statistical analysis of the results implied that the TOC content of the soils did not have significant influence on the extraction efficiency. A longer solid-liquid extraction time did not necessarily increase analyte recovery: Extraction for one hour resulted in 88% recovery while 16 hour extraction led to 89%. Thus, the efficiency of all the methods was comparable for all model soils. Additional investigations regarding GC liner performance highlighted the need for isotopically labelled standards during the analysis of thermolabile pesticides. KW - POP KW - Soil organic matter KW - Solid-liquid-extraction KW - Pressurised liquid extraction PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-430238 DO - https://doi.org/10.4236/jep.2017.86045 SN - 2152-2219 VL - 08 IS - 06 SP - Article ID:77202, 693 EP - 713 PB - Scientific Research Publishing AN - OPUS4-43023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dong, S. A1 - Leng, J. A1 - Feng, Y. A1 - Liu, M. A1 - Stackhouse, C. J. A1 - Schönhals, Andreas A1 - Chiappisi, L. A1 - Gao, L. A1 - Chen, W. A1 - Shang, J. A1 - Jin, L. A1 - Qi, Z. A1 - Schalley, C. A. T1 - Structural water as an essential comonomer in supramolecular polymerization N2 - Although the concept of structural water that is bound inside hydrophobic pockets and helps to stabilize protein structures is well established, water has rarely found a similar role in supramolecular polymers. Water is often used as a solvent for supramolecular polymerization, however without taking the role of a comonomer for the supramolecular polymer structure. We report a low–molecular weight monomer whose supramolecular polymerization is triggered by the incorporation of water. The presence of water molecules as comonomers is essential to the polymerization process. The supramolecular polymeric material exhibits strong adhesion to surfaces, such as glass and paper. It can be used as a water-activated glue, which can be released at higher temperatures and reused many times without losing its performance. KW - Supra molecular polymerization PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-432728 DO - https://doi.org/10.1126/sciadv.aao0900 SN - 2375-2548 VL - 3 IS - 11 SP - eaao0900, 1 EP - eaao0900, 8 PB - American Association for the Advancement of Science AN - OPUS4-43272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baer, Wolfram A1 - Wossidlo, Peter T1 - Validation of a low blow specimen technique for R-curve determination using a drop tower N2 - Fracture mechanics based component design requires appropriate fracture mechanics toughness data with respect to both, loading rate as well as test temperature. Taking high-rate loading into account such as with accidental scenarios, different standards such as ASTM E 1820 or BS 7448-3 provide some information on dynamic fracture mechanics testing. Nevertheless, the designations differ so that a validation of the own material specific test method used for dynamic R-curve determination is mandatory. In order to address this for ductile cast iron materials an experimental method for the reliable determination of dynamic J-integral crack resistance curves at -40 °C following the multiple specimen approach has been established and validated. The experimental concept offers some additional valuable features. Single values of dynamic crack initiation toughness can be determined using a single specimen technique based on crack sensors. Furthermore, an experimentally independent method is provided according to which CTOD δ5 R-curves can be established. The focus of the present paper is on the validation of the experimental low blow technique using a drop tower test system. A drop tower test system was developed and set up to perform low blow tests at temperatures down to -40 °C. The system allows for a variation of the impact mass and height and was optimized for testing of ductile cast iron at stress intensity rates from approximately 5∙10⁴ to 3∙10⁵ MPa√ms⁻¹. This range of loading rate is characteristic for instance with crash scenarios of heavy sectioned DCI casks for radioactive materials. In order to address characteristic challenges of impact tests (test duration of microseconds up to milliseconds, inertial effects, signal oscillations), an appropriate full bridge strain gage method for the measurement of force directly on the specimen as well as a non-contact measurement of load line displacement using an optical extensometer have been developed and validated. The low blow test requires either to prevent bouncing strikes of the hammer by using the stop block technique or to catch the hammer after its first strike. Both options are not part of the experimental concept and setup which have been realized here. The paper describes investigations which have been performed in order to make sure that bouncing strikes of the hammer do not cause additional crack extension in the specimen. This is necessary to ensure a unique relation between the work done and the achieved crack extension. The investigations covered the analysis of limit loads of the specimen with respect to the measured force. The measured stiffness of the specimen was assessed and signals of crack sensors were analyzed. Furthermore, an analysis of the mechanical behavior of the loading system and the specimen by optical observation was performed. Corresponding results are discussed in the paper. It had finally been proven that additional crack extension in the specimen due to bouncing strikes of the hammer is not to be expected under the given conditions of test setup, material and loading. It can be seen as a major experimental advantage that the striker does not have to be catched after the low blow test. T2 - XXIV Italian Group of Fracture Conference CY - Urbino, Italy DA - 01.03.2017 KW - Dynamic fracture mechanics KW - R-curve KW - Low blow KW - Ductile cast iron PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-437686 DO - https://doi.org/10.1016/j.prostr.2017.04.005 SN - 2452-3216 VL - 3 SP - 25 EP - 32 AN - OPUS4-43768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guehrs, E. A1 - Schneider, M. A1 - Günther, Ch. M. A1 - Hessing, P. A1 - Heitz, K. A1 - Wittke, D. A1 - López-Serrano Oliver, Ana A1 - Jakubowski, Norbert A1 - Plendl, J. A1 - Eisebitt, S. A1 - Haase, A. T1 - Quantification of silver nanoparticle uptake and distribution within individual human macrophages by FIB/SEM slice and view N2 - Quantification of nanoparticle (NP) uptake in cells or tissues is very important for safety assessment. Often, electron microscopy based approaches are used for this purpose, which allow imaging at very high resolution. However, precise quantification of NP numbers in cells and tissues remains challenging. The aim of this study was to present a novel approach, that combines precise quantification of NPs in individual cells together with high resolution imaging of their intracellular distribution based on focused ion beam/ scanning electron microscopy (FIB/SEM) slice and view approaches. KW - Nanoparticles KW - FIB/SEM slice and view KW - Absolute dose KW - Cellular internalization KW - Macrophage PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-400626 DO - https://doi.org/10.1186/s12951-017-0255-8 SN - 1477-3155 VL - 15 SP - Article 21, 1 EP - 11 AN - OPUS4-40062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bender, P. A1 - Bogart, L.K. A1 - Posth, O. A1 - Szczerba, Wojciech A1 - Rogers, S.E. A1 - Castro, A. A1 - Nilsson, L. A1 - Zeng, L. J. A1 - Sugunan, A. A1 - Sommertune, J. A1 - Fornara, A. A1 - Gonzales-Alonso, D. A1 - Fernandez Barquin, L. A1 - Johansson, C. T1 - Structural and magnetic properties of multi-core nanoparticles analysed using a generalised numerical inversion method N2 - The structural and magnetic properties of magnetic multi-core particles were determined by numerical inversion of small angle scattering and isothermal magnetisation data. The investigated particles consist of iron oxide nanoparticle cores (9 nm) embedded in poly(styrene) spheres (160 nm). A thorough physical characterisation of the particles included transmission electron microscopy, X-ray diffraction and asymmetrical flow field-flow fractionation. Their structure was ultimately disclosed by an indirect Fourier transform of static light scattering, small angle X-ray scattering and small angle neutron scattering data of the colloidal dispersion. The extracted pair distance distribution functions clearly indicated that the cores were mostly accumulated in the outer surface layers of the poly(styrene) spheres. To investigate the magnetic properties, the isothermal magnetisation curves of the multi-core particles (immobilised and dispersed in water) were analysed. The study stands out by applying the same numerical approach to extract the apparent moment distributions of the particles as for the indirect Fourier transform. It could be shown that the main peak of the apparent moment distributions correlated to the expected intrinsic moment distribution of the cores. Additional peaks were observed which signaled deviations of the isothermal magnetisation behavior from the non-interacting case, indicating weak dipolar interactions. KW - Numerical inversion KW - Magnetic nanoparticles KW - Iron oxides KW - Magnetic properties KW - Structural properties PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-400952 DO - https://doi.org/10.1038/srep45990 SN - 2045-2322 VL - 7 SP - Article 45990, 1 EP - 14 AN - OPUS4-40095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Babutzka, Martin A1 - Heyn, A. T1 - Dynamic tafel factor adaption for the evaluation of instantaneous corrosion rates on zinc by using gel-type electrolytes N2 - The paper presents a new method for the determination and evaluation of tafel factors using gel-type electrolytes and electrochemical frequency modulation technique (EFM). This relatively new electrochemical method offers the possibility to determine both polarization resistances and tafel factors within one measurement and in short measuring intervals. Starting from a comprehensive parameter study it is shown that a direct relationship between the two values exists that can be described mathematically. This contribution presents the determined tafel factors for the system gel-type electrolyte/zinc and discusses their applicability and their limits. T2 - 19th Chemnitz Seminar on Materials Engineering – 19. Werkstofftechnisches Kolloquium CY - Chemnitz, Germany DA - 16.03.2017 KW - Gel-type electrolytes KW - Gelartige Elektrolyte KW - Zinc KW - Zink KW - Stern Geary constant KW - Stern-Geary-Konstante PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394324 UR - http://iopscience.iop.org/article/10.1088/1757-899X/181/1/012021/pdf DO - https://doi.org/10.1088/1757-899X/181/1/012021 SN - 1757-899X SN - 1757-8981 VL - 181 IS - Conference 1 SP - Article UNSP 012021, 1 EP - 11 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-39432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Dietrich, P. A1 - Thissen, A. A1 - Kulak, N. A1 - Kjaervik, Marit A1 - Unger, Wolfgang T1 - XPS surface chemical analysis of aqueous solutions with EnviroESCA N2 - Water and aqueous reagents are essential in any biological process or system. But apart from a few special low vapor-pressure cases, liquids have not been accessible to any technique requiring UHV conditions. EnviroESCA opens up this exciting field of applications. In this paper first results from water based samples are presented as a proof of concept to demonstrate the special capabilities of EnviroESCA analyzing liquid samples. The following solutions were investigated under near ambient pressure conditions: i.) water, ii.) brine, iii.) an oil in water dispersion, iv.) aqueous iron(II) sulfate heptahydrate, and v.) a suspension of nano silver particles in water. KW - Surface Analysis KW - Near Ambient Pressure XPS KW - Aqueous Solutions PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394603 UR - http://www.enviro.specs.de/cms/upload/bilder/EnviroESCA/Applications/Liquids/Application-Note_EnviroESCA_Aqueous_Solutions.pdf N1 - BAM Mitarbeiter Beitrag im Acknowledgement definiert. IS - #000394 SP - 1 PB - SPECS CY - Berlin AN - OPUS4-39460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Asadujjaman, Asad A1 - Kent, B. A1 - Bertin, Annabelle T1 - Phase transition and aggregation behaviour of an UCST-type copolymer poly(acrylamide-coacrylonitrile) in water: effect of acrylonitrile content, concentration in solution, copolymer chain length and presence of electrolyte N2 - An 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 temperature-induced phase transition and aggregation behaviour studied by turbidimetry, static and dynamic light scattering, small angle neutron scattering (SANS) and cryo-transmission electron microscopy (cryo-TEM) measurements. The phase transition temperature was found to increase with increasing AN content in the copolymer, concentration of the solutions and copolymer chain length. A significant effect was observed onto the phase transition temperature by addition of different electrolytes into the copolymer solution. The copolymer chains were aggregated below the phase transition temperature and disaggregated above it. The size of the aggregates increases with increasing AN contents and concentration of the copolymer solutions below the phase transition temperature. The copolymer chains were expanded and weekly associated in solution above the phase transition temperature. A model is proposed to explain such association–aggregation behaviour of poly(AAm-co-AN) copolymers depending on AN contents and concentration of the copolymer solutions as a function of temperature. KW - Thermoresponsive polymers KW - UCST-type copolymer PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394636 DO - https://doi.org/10.1039/c6sm02262f SN - 1744-683X SN - 1744-6848 VL - 13 IS - 3 SP - 658 EP - 669 PB - RSC AN - OPUS4-39463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abbas, F. A1 - Donskyi, Ievgen A1 - Gholami, M. A1 - Ziem, B. A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Böttcher, C. A1 - Rabe, J. A1 - Haag, R. A1 - Adeli, M. T1 - Controlled covalent functionalization of thermally reduced graphene oxide to generate defined bifunctional 2D nanomaterials N2 - A controlled, reproducible, gram-scale method is reported for the covalent functionalization of graphene Sheets by a one-pot nitrene [2+1] cycloaddition reaction under mild conditions. The reaction between commercially available 2,4,6-trichloro-1,3,5-triazine and sodium azide with thermally reduced graphene oxide (TRGO) results in defined dichlorotriazine-functionalized sheets. The different reactivities of the chlorine substituents on the functionalized graphene allow stepwise post-modification by manipulating the temperature. This new method provides unique access to defined bifunctional 2D nanomaterials, as exemplified by chiral surfaces and multifunctional hybrid architectures. KW - Graphene oxide KW - Bifunctional 2D nanomaterials KW - XPS KW - NEXAFS KW - AFM PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394789 DO - https://doi.org/10.1002/ange.201612422 SN - 1433-7851 VL - 56 IS - 10 SP - 2675 EP - 2679 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-39478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maul, Ronald A1 - Greer, B. A1 - Campbell, K. A1 - Elliott, C.T. T1 - Detection of freshwater cyanotoxins and measurement of masked microcystins in tilapia from Southeast Asian aquaculture farms N2 - Recently, there has been a rise in freshwater harmful algal blooms (HABs) globally, as well as increasing aquaculture practices. HABs can produce cyanotoxins, many of which are hepatotoxins. An ultra-performance liquid chromatography tandem mass spectrometry method was developed and validated for nine cyanotoxins across three classes including six microcystins, nodularin, cylindrospermopsin and anatoxin-a. The method was used to analyse free cyanotoxin(s) in muscle (n = 34), liver (n = 17) and egg (n = 9) tissue samples of 34 fish sourced from aquaculture farms in Southeast Asia. Conjugated microcystin was analysed by Lemieux oxidation to ascertain the total amount of microcystin present in muscle. Some tilapia accumulated free microcystin-LR in the muscle tissue at a mean of 15.45 μg/kg dry weight (dw), with total microcystin levels detected at a mean level of 110.1 μg/kg dw, indicating that the amount of conjugated or masked microcystin present in the fish muscle accounted for 85% of the total. Higher levels of cyanotoxin were detected in the livers, with approximately 60% of those tested being positive for microcystin-LR and microcystin-LF, along with cylindrospermopsin. Two fish from one of the aquaculture farms contained cylindrospermopsin in the eggs; the first time this has been reported. The estimated daily intake for free and total microcystins in fish muscle tissue was 2 and 14 times higher, respectively, than the tolerable daily intake value. This survey presents the requirement for further monitoring of cyanotoxins, including masked microcystins, in aquaculture farming in these regions and beyond, along with the implementation of guidelines to safeguard human health. KW - Harmful algal bloom KW - UPLC-MS/MS KW - Bioaccumulation KW - Human health PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-404669 DO - https://doi.org/10.1007/s00216-017-0352-4 SN - 1618-2642 SN - 1618-2650 VL - 409 IS - 16 SP - 4057 EP - 4069 PB - Springer CY - Heidelberg AN - OPUS4-40466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -