TY - JOUR A1 - Bachmann, H. J. A1 - Bucheli, T. D. A1 - Dieguez-Alonso, A. A1 - Fabbri, D. A1 - Knicker, H. A1 - Schmidt, H.-P. A1 - Ulbricht, A. A1 - Becker, Roland A1 - Buscaroli, A. A1 - Buerge, D. A1 - Cross, A. A1 - Dickinson, D. A1 - Enders, A. A1 - Esteves, V.I. A1 - Evangelou, M. W. H. A1 - Fellet, G. A1 - Friedrich, K. A1 - Gasco Guerrero, G. A1 - Glaser, B. A1 - Hanke, U. M. A1 - Hanley, K. A1 - Hilber, I. A1 - Kalderis, D. A1 - Leifeld, J. A1 - Masek, O. A1 - Mumme, J. A1 - Paneque Carmona, M. A1 - Calvelo Pereira, R. A1 - Rees, F. A1 - Rombola, A. G. A1 - de la Rosa, J. M. A1 - Sakrabani, R. A1 - Sohi, S. A1 - Soja, G. A1 - Valagussa, M. A1 - Verheijen, F. A1 - Zehetner, F. T1 - Towards the standardization of biochar analysis: the COST action TD1107 interlaboratory comparison JF - Journal of agricultural and food chemistry N2 - Biochar produced by pyrolysis of organic residues is increasingly used for soil amendment and many other applications. However, analytical methods for its physical and chemical characterization are yet far from being specifically adapted, optimized, and standardized. Therefore, COST Action TD1107 conducted an interlaboratory comparison in which 22 laboratories from 12 countries analyzed three different types of biochar for 38 physical–chemical parameters (macro- and microelements, heavy metals, polycyclic aromatic hydrocarbons, pH, electrical conductivity, and specific surface area) with their preferential methods. The data were evaluated in detail using professional interlaboratory testing software. Whereas intralaboratory repeatability was generally good or at least acceptable, interlaboratory reproducibility was mostly not (20% < mean reproducibility standard deviation < 460%). This paper contributes to better comparability of biochar data published already and provides recommendations to improve and harmonize specific methods for biochar analysis in the future. KW - Biochar KW - Analysis KW - Standardization KW - Ring test KW - Interlaboratory comparison PY - 2016 DO - https://doi.org/10.1021/acs.jafc.5b05055 SN - 0021-8561 SN - 1520-5118 VL - 64 IS - 2 SP - 513 EP - 527 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-35289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martin-Sanchez, Pedro Maria A1 - Miller, A. Z. A1 - Garcia-Sanchez, A. M. A1 - Martin-Sanchez, Pedro Maria A1 - F.C. Pereira, M. A1 - Afonso, M. J. A1 - Saiz-Jimenez, C. A1 - Spangenberg, J. E. A1 - Jurado, V. A1 - Dionísio, A. A1 - Chaminé, H. I. A1 - Hermosin, B. T1 - Origin of abundant moonmilk deposits in a subsurface granitic environment JF - Sedimentology N2 - Subsurface granitic environments are scarce and poorly investigated. A multi-disciplinary approach was used to characterize the abundant moonmilk deposits and associated microbial communities coating the granite walls of the 16th Century Paranhos spring water tunnel in Porto city (north-west Portugal). It is possible that this study is the first record of moonmilk in an urban subsurface granitic environment. The morphology and texture, mineralogical composition, stable isotope composition and microbial diversity of moonmilk deposits have been studied to infer the processes of moonmilk formation. These whitish secondary mineral deposits are composed of very fine needle fibre calcite crystals with different morphologies and density. Calcified filaments of fungal hyphae or bacteria were distinguished by field emission scanning electron microscopy. Stable isotope analysis revealed a meteoric origin of the needle fibre calcite, with an important contribution of atmospheric CO2, soil respiration and HCO3 − from weathering of Ca-bearing minerals. The DNA-based analyses revealed the presence of micro-organisms related to urban contamination, including Actinobacteria, mainly represented by Pseudonocardia hispaniensis, Thaumarchaeota and Ascomycota, dominated by Cladosporium. This microbial composition is consistent with groundwater pollution and contamination sources of the overlying urban area, including garages, petrol stations and wastewater pipeline leakage, showing that the Paranhos tunnel is greatly perturbed by anthropogenic activities. Whether the identified micro-organisms are involved in the formation of the needle fibre calcite or not is difficult to demonstrate, but this study evidenced both abiotic and biogenic genesis for the calcite moonmilk in this subsurface granitic environment. KW - Biomineralization KW - Carbonate precipitation KW - Granite KW - Moonmilk KW - Needle fibre calcite PY - 2017 UR - https://onlinelibrary.wiley.com/doi/full/10.1111/sed.12431 DO - https://doi.org/10.1111/sed.12431 SN - 1365-3091 VL - 65 IS - 2 SP - 1482 EP - 1503 PB - Wiley AN - OPUS4-43622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scala-Benuzzi, M. L. A1 - Soler-Illia, G. J. A. A. A1 - Rabia, J. A1 - Battaglini, F. A1 - Schneider, Rudolf A1 - Pereira, S. V. A1 - Messina, G. A. T1 - Immunosensor based on porous gold and reduced graphene platform for the determination of EE2 by electrochemical impedance spectroscopy JF - Journal of Electroanalytical Chemistry N2 - In this work, we report an electrochemical immunosensor to detect ethinylestradiol in water samples, using electrochemical impedance spectroscopy (EIS) as a detection technique. For the development of this immunosensor, the direct modification of the working electrode of a screen-printed carbon electrode was carried out. First, to reduce the resistance of the electrode, electroreduced graphene was incorporated on the surface. Second, a porous gold structure was electrodeposited on reduced graphene by electrodeposition and the dynamic hydrogen bubble template assisted method. Thus, a marked increase in surface area was obtained for anti-EE2 antibodies immobilization. Subsequently, the specific anti-EE2 antibodies were covalently immobilized using α-lipoic acid for attaching them to the gold surface. The electrode modified with the antibodies was incubated for 30 min in the samples containing EE2, producing the specific Antigen antibody binding. As the charge transfer resistance of a redox probe in the electrode surface is governed by the surface blocking effects, the charge transfer resistance was related to the amount of EE2 captured to realize a quantitative determination. For this, the EIS measurements were performed in a 4 mM [Fe(CN)6]4−/3− solution in 0.1 M KCl. The obtained Nyquist diagrams were adjusted using the Randles circuit as an equivalent circuit to obtain the corresponding resistances. The developed methodology showed good selectivity, precision, and sensitivity; although the LOD obtained was higher than those presented in other published articles, it turned out to be an alternative that allows the determination of ethinylestradiol using a simple disposable electrode. KW - Ethinylestradiol KW - Biosensor KW - Elektrochemisch KW - Impedanz PY - 2021 DO - https://doi.org/10.1016/j.jelechem.2021.115604 SN - 1572-6657 VL - 897 SP - 115604 EP - 115611 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-54048 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martínez, N.A. A1 - Pereira, S.V. A1 - Bertolino, F.A. A1 - Schneider, Rudolf A1 - Messina, G.A. A1 - Raba, J. T1 - Electrochemical detection of a powerful estrogenic endocrine disruptor: ethylestradiol in water samples through bioseparation procedure JF - Analytica chimica acta N2 - The synthetic estrogen ethinylestradiol (EE2) is an active component of oral contraceptives (OCs), considered as an endocrine disrupting compound (EDC). It is excreted from humans and released via sewage treatment plant effluents into aquatic environments. EDCs are any environmental pollutant chemical that, once incorporated into an organism, affects the hormonal balance of various species including humans. Its presence in the environment is becoming of great importance in water quality. This paper describes the development of an accurate, sensitive and selective method for capture, preconcentration and determination of EE2 present in water samples using: magnetic particles (MPs) as bioaffinity support for the capture and preconcentration of EE2 and a glassy carbon electrode modified with multi-walled carbon nanotubes (MWCNTs/GCE) as detection system. The capture procedure was based on the principle of immunoaffinity, the EE2 being extracted from the sample using the anti-EE2 antibodies (anti-EE2 Ab) which were previously immobilized on MPs. Subsequently the analyte desorption was done employing a sulfuric acid solution and the determination of the EE2 in the pre-concentrated solution was carried out by square wave voltammetry (SWV). This method can be used to determine EE2 in the range of 0.035–70 ng L-1 with a detection limit (LOD) of 0.01 ng L-1 and R.S.D. < 4.20%. The proposed method has been successfully applied to the determination of EE2 in water samples and it has promising analytical applications for the direct determination of EE2 at trace levels. KW - Magnetic particles KW - Bioseparation KW - Ethinylestradiol KW - Electrochemistry KW - Immunoassay KW - Elektrochemischer Sensor KW - Endokrine Disruptoren KW - Hormone KW - Ethinylestradiol KW - EE2 KW - Östrogene PY - 2012 DO - https://doi.org/10.1016/j.aca.2012.02.033 SN - 0003-2670 SN - 1873-4324 SN - 0378-4304 VL - 723 SP - 27 EP - 32 PB - Elsevier CY - Amsterdam AN - OPUS4-25656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fu, B. A1 - Shen, J. A1 - Suhuddin, U. A1 - Pereira, A. A1 - Maawad, E. A1 - dos Santos, J. A1 - Klusemann, B. A1 - Rethmeier, Michael T1 - Revealing joining mechanism in refill friction stir spot welding of AZ31 magnesium alloy to galvanized DP600 steel JF - Materials & Design N2 - The application of magnesium (Mg) inevitably involves dissimilar welding with steel. A novel solid state spot welding method, refill friction stir spot welding (refill FSSW), was utilized to weld AZ31 Mg alloy to galvanized DP600 steel. Although Mg/Fe is an immiscible alloy system, defect-free welds with high strength were successfully obtained in a wide parameter window. The results of microstructure, interfacial reactions, and mechanical properties are reported to reveal the underlying joining mechanism. Due to the melting of Zn coating and subsequent Mg-Zn reactions, Mg-Zn eutectic and intermetallic compounds were detected within welds. Heterogeneous interfacial reactions occur along Mg/steel interface, and the relationship between interfacial structure and fracture behavior was investigated. The joining mechanism is associated with Zn coating and Fe-Al layer: 1) the presence of Zn coating is beneficial for achieving high-quality welding between Mg and steel, it protects the interface from oxidation and contributes to brazing of the weld; 2) the Al present in Mg alloy reacts with Fe, resulting in the growth of Fe-Al layer, which contributes to the diffusion bonding in the interface. The overall results clearly show that Refill FSSW is a competitive welding method for joining Mg and galvanized steel. KW - Refill friction stir spot welding KW - Multi-materials joining KW - Magnesium alloy KW - Galvanized steel KW - Mechanical properties KW - Microstructure PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536878 DO - https://doi.org/10.1016/j.matdes.2021.109997 SN - 0264-1275 VL - 209 SP - 109997 PB - Elsevier Ltd. AN - OPUS4-53687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kern, Simon A1 - Wander, Lukas A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gottu Mukkula, A. R. A1 - Holtkamp, M. A1 - Salge, M. A1 - Fleischer, C. A1 - Weber, N. A1 - Engell, S. A1 - Paul, Andrea A1 - Pereira Remelhe, M. A1 - Maiwald, Michael T1 - Flexible automation with compact NMR spectroscopy for continuous production of pharmaceuticals JF - Analytical and Bioanalytical Chemistry N2 - Modular plants using intensified continuous processes represent an appealing concept for the production of pharmaceuticals. It can improve quality, safety, sustainability, and profitability compared to batch processes; besides, it enables plug-and-produce reconfiguration for fast product changes. To facilitate this flexibility by real-time quality control, we developed a solution that can be adapted quickly to new processes and is based on a compact nuclear magnetic resonance (NMR) spectrometer. The NMR sensor is a benchtop device enhanced to the requirements of automated chemical production including robust evaluation of sensor data. Beyond monitoring the product quality, online NMR data was used in a new iterative optimization approach to maximize the plant profit and served as a reliable reference for the calibration of a near-infrared (NIR) spectrometer. The overall approach was demonstrated on a commercial-scale pilot plant using a metal-organic reaction with pharmaceutical relevance. KW - NMR Spectroscopy KW - NIR Spectroscopy KW - Real-time process monitoring KW - Real-time quality control KW - Continuous processes KW - CONSENS KW - Data Fusion PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-480623 DO - https://doi.org/10.1007/s00216-019-01752-y SN - 1618-2642 SN - 1618-2650 VL - 411 IS - 14 SP - 3037 EP - 3046 PB - Springer Nature CY - Heidelberg AN - OPUS4-48062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Wander, Lukas A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gottu Mukkula, A. R. A1 - Holtkamp, M. A1 - Salge, M. A1 - Fleischer, C. A1 - Weber, N. A1 - King, R. A1 - Engell, S. A1 - Paul, Andrea A1 - Pereira Remelhe, M. A1 - Maiwald, Michael T1 - Flexible Automation with compact NMR instruments N2 - Modular plants using intensified continuous processes represent an appealing concept to produce pharmaceuticals. It can improve quality, safety, sustainability, and profitability compared to batch processes, and it enables plug-and-produce reconfiguration for fast product changes. To facilitate this flexibility by real-time quality control, we developed a solution that can be adapted quickly to new processes and includes a compact Nuclear Magnetic Resonance (NMR) spectrometer for online quality monitoring as well as a new model-based control approach. The NMR sensor is a benchtop device enhanced to the requirements of automated chemical production including ro-bust evaluation of sensor data. Here, we present alternatives for the quantitative determination of the analytes using modular, physically motivated models. These models can be adapted to new substances solely by the use of their corresponding pure component spectra, which can either be derived from experimental spectra as well as from quantum mechanical models or NMR predictors. Modular means that spec-tral models can simply be exchanged together with alternate reagents and products. Beyond that, we comprehensively calibrated an NIR spectrometer based on online NMR process data for the first time within an industrial plant. The integrated solution was developed for a metal organic reac-tion running on a commercial-scale modular pilot plant and it was tested under industrial conditions. T2 - 7th Annual PANIC Conference CY - Hilton Head Island, South Carolina, USA DA - 03.03.2019 KW - Online NMR Spectroscopy PY - 2019 AN - OPUS4-47715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oliveira, D.F. A1 - Moreira, E.V. A1 - Silva, A.S.S. A1 - Rabello, J.M.B. A1 - Lopes, R.T. A1 - Pereira, M.S. A1 - Zscherpel, Uwe T1 - Application of the digital radiography in weld inspection of gas and oil pipelines T2 - 10th European conference on non-destructive testing (Proceedings) N2 - The aim of this work is to evaluate the feasibility of the direct radiography on weld inspection in oil pipelines and gas pipeline during the manufacturing process. To that, 6 specimens with 6 different thickness and varied height of reinforced weld with 5 different kinds of defects were made. All samples were radiographied using Class I films and flat panel. For all specimens the inspection length was 8''. Thus, with the flat panel the detector-to-object distance varied so that it may adequate to several diameters of the tubes. The detector-to-object distance was calculated based on the physical size of the detector taking into consideration a safe distance between the tube curvature and the flat panel extremities, keeping the lowest possible magnification factor so that it could be obtained the length of the inspection. Images with 6 integration time for each experimental arrangement were obtained. The images obtained with the Flat Panel/YXLON system were analyzed according to their quality by using the Contrast parameters (essential wire) (DNV 2007/ IS0 12096 – with reinforcement and ISO 10893-7 – basis material), Basic Spatial Resolution – BSR (ISO 10893-7) and normalized signal-to-noise ratio - SNRN (ISO 10893-7) and by detectability using as reference the conventional radiography. The results showed that for all thickness, the exposure time used to meet the image quality requirements were below with direct radiography. However the BSR were not reached for thickness of 4.85, 6.40 and 9.67 mm, therefore the compensation principle established by ISO 10893-7 was considered, that is, one more contrast wire for a less wire pair. The digital technique proved to be more sensitive to real defects found on welds than the conventional technique. Then it can be conclude that the digital radiography utilizing the flat panel can be applicable to the oil and gas segment with advantages over conventional technique as to quality aspects, productivity, environment, safety and health. T2 - 10th European conference on non-destructive testing CY - Moscow, Russia DA - 2010-06-07 KW - Zerstörungsfreie Prüfung KW - Durchstrahlungsprüfung KW - Digitale Radiologie PY - 2010 UR - http://www.ndt.net/article/ecndt2010/reports/1_04_01.pdf IS - Paper 4.02.18 SP - 1 EP - 11(?) AN - OPUS4-22502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rocha, S. A1 - Thünemann, Andreas A1 - Pereira, M.C. A1 - Coelho, M.A.N. A1 - Möhwald, H. A1 - Brezesinski, G. T1 - The Conformation of B18 Peptide in the Presence of Fluorinated and Alkylated Nanoparticles JF - ChemBioChem KW - Small-angle-X-ray scattering KW - Circular dichroism PY - 2005 SN - 1439-4227 SN - 1439-7633 VL - 6 SP - 1 EP - 4 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-6064 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pereira, P.M.R. A1 - Carvalho, José Joao A1 - Silva, S. A1 - Cavaleiro, J.A.S. A1 - Schneider, Rudolf A1 - Fernandes, R. A1 - Tomé, J.P.C. T1 - Porphyrin conjugated with serum albumins and monoclonal antibodies boosts efficiency in targeted destruction of human bladder cancer cells JF - Organic & biomolecular chemistry N2 - The synthesis of a novel PS conjugated with bovine and human serum albumin (BSA and HSA) and a monoclonal antibody anti-CD104 is reported, as well as their biological potential against the human bladder cancer cell line UM-UC-3. No photodynamic effect was detected when the non-conjugated porphyrin was used. Yet, when it was coupled covalently with the mAb anti-CD104, BSA and HSA, the resulting photosensitizer conjugates demonstrated high efficacy in destroying the cancer cells, the mAb anti-CD104 efficacy overruling the albumins. KW - Rinderserumalbumin KW - BSA KW - Monoklonale Antikörper KW - Blasenkrebs KW - Konjugate KW - Conjugates KW - Therapeutische Antikörper KW - CD104 PY - 2014 DO - https://doi.org/10.1039/c3ob42082e SN - 1477-0520 SN - 1477-0539 VL - 12 IS - 11 SP - 1804 EP - 1811 PB - RSC CY - Cambridge AN - OPUS4-30451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -