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Paper des Monats
- ja (68)
The duplex stainless steel 1.4062 (X2CrNiN22-2) is used as alternative material to austenitic stainless steels in the construction industry. The corrosion resistance of welded seams is influenced by the base material, the weld filler material, the welding process and also by the final surface treatment. The scale layer next to the weld seam can be removed by grinding, pickling, electro-polished or blasting depending on the application and the requested corrosion resistance. Blasted surfaces are often used in industrial practice due to the easier and cheaper manufacturing process compared to pickled or electro-polished surfaces. Furthermore blasting with corundum-grain is more effective than blasting with glass-beads which also lower the process costs. In recent years, stainless steel surfaces showed an unusually high susceptibility to pitting corrosion after grinding with corundum. For this reason, it is now also questioned critically whether the corrosion resistance is influenced by the applied blasting agent. This question was specifically investigated by comparing grinded, pickled, corundum-grain- and glass-bead-blasted welding seams. Results of the SEM analyses of the blasting agents and the blasted surfaces will be presented and correlated with the different performed corrosion tests (potential measurement, KorroPad-test and pitting potential) on welding seams with different surface treatments.
The novel heat treatment concept, “quenching and partitioning” (Q&P) has been developed for high strength steels with enhanced formability. This heat treatment involves quenching of austenite to a temperature between martensite start and finish, to receive a several amount of retained austenite. During the subsequent annealing treatment, the so called partitioning, the retained austenite is stabilized due to carbon diffusion, which results in enhanced formability and strength regarding strain induced austenite to martensite transformation. In this study a Q&P heat treatment was applied to a Fe-0.45C-0.65Mn-0.34Si-13.95Cr stainless martensite. Thereby the initial quench end temperature and the partitioning time were varied to characterize their influence on microstructural evolution. The microstructural changes were analysed by dilatometer measurements, X-ray diffraction and scanning electron microscopy, including electron backscatter diffraction. Compression testing was made to examine the mechanical behaviour. It was found that an increasing partitioning time up to 30 min leads to an enhanced formability without loss in strength due to a higher amount of stabilized retained and reversed austenite as well as precipitation hardening.
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.
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.
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.
The CCQM-K123 key comparison was organized by the Inorganic Analysis Working Group (IAWG) of CCQM to assess and document the capabilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of sodium, calcium, potassium, magnesium phosphorous and sulfur in biodiesel fuel (BDF). The National Metrology Institute of Japan (NMIJ) and National Institute of Standards and Technology (NIST) acted as the coordinating laboratories.
Results were submitted by 11 NMIs and DIs. The participants used different measurement methods, though most of them used inductively coupled plasma-mass spectrometry (ICP-MS), isotope dilution technique with ICP-MS and inductively coupled plasma-optical emission spectrometry (ICP-OES) with microwave acid digestion.
The material was quite challenging and a number of questions were raised at the IAWG meeting. Concerning S, the variation in S results between participants, particularly those using IDMS methods was discussed at the IAWG meeting. BAM, NIST and NMIJ reviewed their experimental conditions, results and/or uncertainty calculations for IDMS. According to the additional evaluation and investigation, the variances between the revised results became smaller than the original one, the revised results were overlapping between IDMS measurements of S content at the k=2 level. It is not possible to calculate a KCRV with values being modified after submission. It was concluded that this KC does not support S measurements.
Accounting for relative expanded uncertainty, comparability of measurement results for each of Na, Ca, K, Mg and P was successfully demonstrated by the participating NMIs or DIs. It is expected that sodium, calcium, potassium, magnesium and phosphorus at mass fractions greater than approximately 0.1 mg/kg, 0.1 mg/kg, 0.05 mg/kg, 0.05 mg/kg and 0.1 mg/kg respectively in biodiesel fuel and similar matrices (fuels and oils etc.) can be determined by each participant using the same technique(s) employed for this key comparison to achieve similar uncertainties mentioned in the present report. Furthermore, the results of this key comparison can be utilized along with the IAWG core capability approach.
Der durch Kräfte senkrecht zur Stabachse belastete Balken ist eines der Haupttragelemente des Stahlbetonbaus. Biegebalken finden unter anderem Anwendung in Form von Brückenträgern oder Unterzügen. Die bei maximaler Beanspruchung auftretenden Versagensformen unterteilen sich dabei in Biege- und Querkraftversagen (Schubversagen). Ein Versagen des Balkens kann je nach Versagensmechanismus mit oder ohne Vorankündigung erfolgen. Gebräuchliche Bemessungskonzepte der Baupraxis zur Dimensionierung entsprechender Tragelemente zielen auf ein Versagen mit ausreichender Vorankündigung (große Verformungen oder breite Risse) ab, wie es z.B. beim sekundären Biegedruckversagen entsteht. Für die Zustandsüberwachung von Bauwerken (z.B. Brücken) mittels zerstörungsfreier Prüftechniken sind fundierte Kenntnisse zu den bei Biegebeanspruchung auftretenden Schadensmechanismen erforderlich. Im Rahmen eines BAM-internen Projektes sollen durch praxisnahe Untersuchungen an einer brückenähnlichen Referenzstruktur unterschiedliche auf das Tragwerk einwirkende thermische und mechanische Belastungen untersucht werden und in die Entwicklung eines Monitoringsystems einfließen. Anhand der aus Biegeversuchen vorliegenden Ergebnisse wird der Einsatz unterschiedlicher Methoden der zerstörungsfreien Materialprüfung gezeigt und deren Anwendbarkeit für die Analyse des Verformungsverhaltens von Stahlbetonbalken diskutiert. Hierzu wurde das Verformungsverhalten eines Stahlbetonbalkens (L = 2,75 m) in einem Vierpunkt-Biegeversuch im Labormaßstab untersucht. Das Hauptaugenmerk liegt dabei auf der Charakterisierung der ausschlaggebenden Versagensmodi durch die einzelnen zerstörungsfreien Prüfverfahren und der Vergleich zu klassischen Messmethoden (z.B. Verformungsmessung mittels induktiver Wegaufnehmer (IWA)). Die Biegeversuche wurden dazu durch Schallemissionsanalyse (SEA) und optische Verformungsanalyse mittels Stereo-Fotogrammetrie (SF) und Bildkorrelationsverfahren (BKV) begleitet.
This work demonstrates that phase-segregated poly(ester urethane) (PEU) with switching segments of crystallizable poly(1,4-butylene adipate) (PBA) can be programmed to generate two separate stress recovery events upon heating under constant strain conditions. For programming, two elongations are applied at different temperatures, followed by unloading and cooling. During the adjacent heating, two-step stress recovery is triggered. The results indicate that the magnitude of the stress recovery signals corresponds to the recovery of the two deformation stresses in reverse order. As demonstrated by further experiments, twofold stress recovery can be detected as long as the elongation at higher temperature exceeds the strain level of the deformation at lower temperature. Another finding includes that varying the lower deformation temperature enables a control over the stress recovery temperature and thus the implementation of so-called “temperature-memory effects”. Moreover, exerting only one elongation during programming enables a heating-initiated one-step stress recovery close to the deformation temperature. Based on these findings, such polymers may offer new technological opportunities in the fields of active assembly when used as fastening elements and in functional clothing when utilized for compression stockings.
Referee Report 06 March 2017
(2017)
Driven mostly by the search for chemical syntheses under biocompatible conditions, so called "click" chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques possessing short set-up times. Here, we report on a fast and reliable calibration-free online NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement of 1H spectra with a time interval of 20 s per spectrum, and a robust, fully automated algorithm to interpret the obtained data. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in a variety of non-deuterated solvents while its time-resolved behaviour was characterized with step tracer experiments. Overlapping signals in online spectra during thiol-ene coupling could be deconvoluted with a spectral model using indirect hard modeling and were subsequently converted to either molar ratios (using a calibrationfree approach) or absolute concentrations (using 1-point calibration). For various solvents the kinetic constant k for pseudo-first order reaction was estimated to be 3.9 h-1 at 25 °C. The obtained results were compared with direct integration of non-overlapping signals and showed good agreement with the implemented mass balance.
Structural relaxation phenomena in binary and multicomponent lithium silicate glasses were studied upon irradiation with femtosecond (fs) laser pulses (800 nm central wavelength, 130 fs pulse duration) and subsequent thermal annealing experiments. Depending on the annealing temperature, micro-Raman spectroscopy analyses evidenced different relaxation behaviours, associated to bridging and non-bridging oxygen structures present in the glass network. The results indicate that the mobility of lithium ions is an important factor during the glass modification with fs-laser pulses. Quantitative phase contrast imaging (spatial light interference microscopy) revealed that these fs-laser induced structural modifications are closely related to local changes in the refractive index of the material. The results establish a promising strategy for tailoring fs-laser sensitivity of glasses through structural mobility.
Matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) is a well-implemented analytical technique for the investigation of complex biological samples. In MS, the sample preparation strategy is decisive for the success of the measurements. Here, sample preparation processes and target materials for the investigation of different pollen grains are compared. A reduced and optimized sample preparation process prior to MALDI-TOF measurement is presented using conductive carbon tape as target. The application of conductive tape yields in enhanced absolute signal intensities and mass spectral pattern information, which leads to a clear separation in subsequent pattern analysis. The results will be used to improve the taxonomic differentiation and identification, and might be useful for the development of a simple routine method to identify pollen based on mass spectrometry.
This author interview is by Dr Michael G. Weller, Head of Division 1.5 Protein Analysis at Federal Institute for Materials Research and Testing (BAM). BAM (www.bam.de/en) is a senior scientific and technical institute with responsibility to the German Federal Ministry for Economic Affairs and Energy. Dr Weller's review paper, Quality issues of research antibodies is available for download in Analytical Chemistry Insights.
Immunoassays are suitable tools for high-throughput screenings. The prerequisite for accurate determinations by these methods is the selection of an excellent antibody. The production and selection of monoclonal antibodies is usually a tedious process. In this study, new strategies for improving antibody production and characterization were applied. This includes the monitoring of the immunization progress in mice through antibodies extracted from feces, which allows a time-resolved and animal-friendly monitoring of the immune response. Additionally, fluorescence polarization immunoassay (FPIA) could be successfully applied for fast and easy examination of cell culture supernatants and the investigation of antibody/antigen interactions including kinetics and fluorescence properties. These methods simplify the selection of the optimal antibody. As a target analyte, carbamazepine was chosen. This is a widely used antiepileptic drug which also frequently occurs in the environment. The new antibody enables CBZ determination in the concentration range 0.66–110 µg L-1 within 10 min using a high-throughput microtiter plate-based FPIA, and between 1.4 and 79 µg L-1 within 5 min applying an automated cuvette-based FPIA instrument, and from 0.05–36 µg L-1 using ELISA. The measurements were performed at a non-equilibrium state which improved the sensitivity and selectivity of the assays. Due to low cross-reactivity especially towards the main CBZ metabolite and other pharmaceuticals (<1%), this antibody gives the opportunity for application in medical and environmental analyses.
This article provides an impression on potentials in applying nowadays welding simulation tools in construction design. This is carried out exemplary on plate girders from two structural steel grades. The calculated residual stresses are compared with measurements by sectioning method. It has been repeatedly stated that present Eurocode models fail to approximate the residual stresses. Especially for high strength steel (HSS) only limited information is available on realistic occurring residual stresses in typical I-girders. The investigations are aimed to give further guidance on these values. A few proposals on advanced models are discussed.
In the quest for finding the ideal synchrotron-radiation-induced imaging method for the investigation of trace element distributions in human bone samples, experiments were performed using both a scanning confocal synchrotron radiation micro X-ray fluorescence (SR-mXRF) (FLUO beamline at ANKA) setup and a full-field color X-ray camera (BAMline at BESSY-II) setup. As zinc is a trace element of special interest in bone, the setups were optimized for its detection. The setups were compared with respect to count rate, required measurement time and spatial resolution. It was demonstrated that the ideal method depends on the element of interest. Although for Ca (a major constituent of the bone with a low energy of 3.69 keV for its K alpha XRF line) the color X-ray camera provided a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-µXRF setup was able to sufficiently image the distribution.
Investigation of manuscripts found in sites along the Silk Road shows the history of communication and exchange between Asia and the Mediterranean over the centuries. Different scripts and languages preserved on paper in certain styles provide information about traditions and provenance.
To get an idea of the cultural background of the highly developed painting techniques obvious in some illuminated manuscripts, the material used for writing and painting is analyzed. Singular Sogdian and Tocharian manuscripts from Turfan show text on one side with a colorful painting on the other side of the document. In comparison with other productions of different periods or usages from the site, special features are worked out to characterize cultural roots or influence in the network of relationships. Details analyzed in the most elaborated documents Show various influences led to the colorful masterpieces.
Designing artificial macromolecules with absolute sequence order represents a considerable challenge. Here we report an advanced light-induced avenue to monodisperse sequencedefined functional linear macromolecules up to decamers via a unique photochemical approach. The versatility of the synthetic strategy—combining sequential and modular concepts—enables the synthesis of perfect macromolecules varying in chemical constitution and topology. Specific functions are placed at arbitrary positions along the chain via the successive addition of monomer units and blocks, leading to a library of functional homopolymers, alternating copolymers and block copolymers. The in-depth characterization of each sequence-defined chain confirms the precision nature of the macromolecules. Decoding of the functional information contained in the molecular structure is achieved via tandem mass spectrometry without recourse to their synthetic history, showing that the sequence information can be read.We submit that the presented photochemical strategy is a viable and advanced concept for coding individual monomer units along a macromolecular chain.
Reliable nanomaterial classification of powders using the volume-specific surface area method
(2017)
The volume-specific surface area (VSSA) of a particulate material is one of two apparently very different metrics recommended by the European Commission for a definition of "nanomaterial" for regulatory purposes: specifically, the VSSA metric may classify nanomaterials and non-nanomaterials differently than the median size in number metrics, depending on the chemical composition, size, polydispersity, shape, porosity, and aggregation of the particles in the powder.
Here we evaluate the extent of agreement between classification by electron microscopy (EM) and classification by VSSA on a large set of diverse particulate substances that represent all the anticipated challenges except mixtures of different substances. EM and VSSA are determined in multiple labs to assess also the level of reproducibility. Based on the results obtained on highly characterized benchmark materials from the
NanoDefine EU FP7 project, we derive a tiered screening strategy for the purpose of implementing the definition of nanomaterials. We finally apply the Screening strategy to further industrial materials, which were classified correctly and left only borderline cases for EM.
On platelet-shaped nanomaterials, VSSA is essential to prevent false-negative classification by EM. On porous materials, approaches involving extended Adsorption isotherms prevent false positive classification by VSSA. We find no false negatives by VSSA, neither in Tier 1 nor in Tier 2, despite real-world industrial polydispersity and diverse composition, shape, and coatings. The VSSA screening strategy is recommended for inclusion in a technical guidance for the implementation of the definition.
Die im Forschungsvorhaben erzielten Ergebnisse zeigen konkrete technische Lösungen für die automatisierte Anwendung des MSG Engspaltschweißen, sowohl mittels optischer als auch prozessorientierter Sensorik, und sprechen damit ein breites Spektrum möglicher Anwender, insbesondere KMU, an.
Die Seitenführung des Brenners auf Basis der optischen Messgrößen stellt eine robuste und einfach zu implementierende Möglichkeit zur Nahtverfolgung dar. Für die Höhenführung über der Schweißnaht wurde neben der Lösung mittels optischer Messverfahren zusätzlich eine direkt darauf aufbauende Möglichkeit zur Implementierung eines Lichtbogensensors abgeleitet. Das Vorgehen konnte sowohl für Sprühlichtbogenprozesse als auch bei Verwendung von Impulslichtbogenprozessen erfolgreich angewendet werden.
Die zur Sicherstellung eines gleichmäßigen Flankeneinbrandes entwickelte Pendelregelung ist ebenfalls für unterschiedliche Lichtbogenarten einsetzbar und muss vom Anwender auch beim Einsatz einer großen Bandbreite unterschiedlicher Prozessparameter nahezu nicht konfiguriert werden. Neben der im Rahmen der Verfahrensprüfung untersuchten Pendelraupentechnik konnte die Übertragbarkeit des Vorgehens auch auf die Strichraupentechnik anhand von gezielten Schweißversuchen aufgezeigt werden.
Die zunächst auf Basis der optischen Messwerte ausgelegte Füllgradregelung konnte die vorgesehenen Spaltvariationen von 18 bis 24 mm im Rahmen der durchgeführten Verfahrensprüfung ausgleichen. Die Ableitung eines äquivalenten Lichtbogensensors durch Kopplung beider Messprinzipien wurde am Laufzeitende des Vorhabens aufgezeigt, konnte jedoch durch zeitliche Beschränkung nicht für die Verfahrensprüfung berücksichtigt werden.
In Absprache mit dem projektbegleitenden Ausschuss wurde die Entwicklung der Prozessregelung für das Vorhaben auf Schweißungen in Wannenlage und Grundwerkstoffe der Güte S355J2 beschränkt.
Die Qualifizierung des Verfahrens unter Einsatz der beschriebenen Regelalgorithmen nach DIN EN ISO 15614-1 konnte für alle betrachteten Spaltbreiten zwischen 18 und 24 mm anhand einer 50 mm dicken Demonstratorprobe nachgewiesen werden.