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Organisationseinheit der BAM
- 8 Zerstörungsfreie Prüfung (3)
- 8.6 Faseroptische Sensorik (2)
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- 1.2 Biophotonik (1)
- 4 Material und Umwelt (1)
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Das Basisanliegen - Einleitung
Mit der zunehmenden Zahl akkreditierter ZfP-Firmen und zunehmender Anwendung risikobasierender Konzepte ergibt sich die Notwendigkeit, internationale Standards wie die DIN EN ISO 17025 und darüber hinausgehende Richtlinien bei der Verfahrensauswahl in der ZfP zu berücksichtigen. Dieser Aufsatz soll aufzeigen, welche internationalen Aktivitäten gegenwärtig für die Zuverlässigkeitsbetrachtungen von Bedeutung sind (siehe auch [1]). In Übereinstimmung mit den Vereinbarungen und Definitionen der European-American Workshops zur Zuverlässigkeit [2, 3] gilt: Das Basisanliegen der Zuverlässigkeitsuntersuchungen beliebiger diagnostischer Systeme besteht darin, den Grad festzustellen mit dem das Prüfsystem in der Lage ist, seinen vorgesehenen Zweck zu erfüllen. Im Falle der ZfP besteht dieser Zweck zumeist in der Aufgabe, Bauteildefekte aufzufinden und zu beschreiben bzw. die Defektfreiheit von Bauteilen zu bestätigen, sowie Wanddicken zu messen oder Material zu charakterisieren.
Das Basisanliegen der Zuverlässigkeitsuntersuchungen findet seinen Niederschlag bei folgenden international relevanten Aktivitäten:
neue ISO 17025 als Notwendigkeit mit variablen Möglichkeiten der Verfahrensvalidierung
als Kettenglied in RBLM (Risk Based Life Time Management) (r) EPERC-Initiative
CEN/TC138/WG9 "Qualifizierung von ZfP-Verfahren"
Six-Sigma Strategie: als notwendiger Bestandteil
ASNT-Initiative: Standing Committee on NDE Reliability: als Arbeitspaket
Produkthaftung: als notwendige Voraussetzung für die Handhabung
During the second European-American Workshop on NDE Reliability, September 99 in Boulder, the term NDE reliability was defined as the degree that an NDT system is capable of achieving its purpose regarding detection, characterization and false calls. The most common but also most expensive - way to determine this degree of capability in e.g. defect detection is to make just a performance demonstration using realistic test samples and to count the correct detections and false calls. For a more efficient way of reliability evaluation we propose to decompose the system into main modules e.g. according to the reliability formula set up on the first workshop: into f(IC) a function of IC the intrinsic capability, determined by the physics and the technique of the NDE method representing an ideal upper bound of the reliability and g(AP) a function of AP the industrial application factor like surface state or limited access to a component in general diminishing the ideal capability and finally h(HF) the function of the human factor which is in general also diminishing the ideal capability. The workshop proposed a rather plain mathematical shape for the formula R = f(IC) g(AP) h(HF) which should be considered merely as a philosophical expression but not as exact mathematical formula to be applied for evaluation of e.g. POD data. We propose to decompose the NDE system into modules in terms of functions of IC, AP and HF if appropriate or additional ones if necessary and then to analyze the mutual relationships of the terms via fault tree analysis. Finally the total reliability of the system is composed of the reliability of the subsystems via the rules of statistical systems theory.
First trials for this approach of data analysis will be presented via examples from NDE systems in the aerospace industry.
Struktur des basischen Zink-O,O'-ethylhexyldithiophosphats in unpolar, aprotischen Lösungsmitteln
(1995)
Zwei Verfahren, der Unterwasser-Test und der Plate-Dent-Test, wurden hinsichtlich ihrer Eignung zur indirekten Bestimmung
der Zündstärke von Zündern untersucht. Die Einflüsse verschiedener Sekundärladungsmassen und unterschiedlichen
Hülsenmaterials von Zündern standen hierbei im Vordergrund.
Der Unterwasser-Test, bei dem als Maß für die Zündstärke die Stoß- und Blasenenergie eines Zünders ermittelt werden,
erwies sich als probate und genaue Bestimmungsmethode. Zünder mit unterschiedlichen Sekundärladungsmassen waren
eindeutig differenzierbar. Das Hülsenmaterial hatte nur einen vernachlässigbaren Einfluss auf die Ergebnisse.
Der Plate-Dent-Test, bei dem die Abmaße des gebildeten Kraters zur indirekten Bestimmung der Zündstärke herangezogen
werden, zeigte gegenteilige Effekte. Ab einem Ladungslänge-Durchmesser-Verhältnis von größer zwei war eine Differenzierung
von Zündern verschiedener Sekundärladungsmasse nicht mehr möglich. Außerdem hatte das Hülsenmaterial
einen signifikanten Einfluss auf die Kraterbildung. Der Plate-Dent-Test ist somit nur für den direkten Vergleich der Zündstärken
baugleicher Zünder z. B. unter variierenden Umweltbedingungen geeignet.---------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Two procedures – the underwater test and the plate-dent-test – were examined concerning their applicability for the indirect
determination of the initiating capability of detonators. At this the focus was on the influence of varying explosive masses
and different shell material.
At the underwater test the initiating capability is determined indirectly by measurement and calculation of the shock and
bubble energy. This method proved to be effective and accurate. Detonators with different secondary charge masses could
be distinguished clearly and the shell material had only a negligible influence on the energy release.
The plate-dent-test, at which the dimensions of the formed dent are an indirect measure for the initiating capability, showed
the contrary effects. A differentiation of detonators was proved to be impossible when a relation of charge length to diameter
greater than two was reached. Furthermore, it could be shown that the shell material had significant influence on the
dent formation. Therefore, the plate-dent-test is only suitable for the direct comparison of identical detonators, e. g. under
varying environmental conditions.
The interaction of self-assembled dendritic amphiphiles with drugs and dyes in aqueous solutions is of great significance for designing and optimizing shape-persistent delivery systems. Here we present deeper insight for two examples of low molecular weight (LMW) nonionic dendritic amphiphiles as host molecules and a series of selected aromatic guest model molecules (benzene, naphthalene, biphenyl, terphenyl, anthracene, and pyrene). Aromatic guest molecules were incorporated into the self-assemblies of dendritic nanocarriers, and the resultant complexes were studied by a combination of UV, NMR, computational simulation, and small-angle X-ray-scattering (SAXS) techniques in order to determine the loading capacity, localization, and specific interactions in dendritic amphiphiles with guest molecules. Our findings revealed that the localization of guest molecules in the hydrophobic region and the loading capacity of guest molecules are dependent on their size and the arrangement of aromatic rings instead of the loading amount. Furthermore, the shape of self-assembled host molecules was found to be ellipsoidal and highly persistent even after loading the guest molecules. To the best of our knowledge, this is the first systematic host–guest study, particularly with low molecular weight nonionic dendritic amphiphilies and aromatic guest molecules. Thus, this study opens new possibilities and ways to explore the transport behavior of aromatic drugs with such nanocarriers.
Die Nutzung und Weiterverarbeitung von Sekundärstoffen kann in der Baustoffherstellung einen Beitrag zum nachhaltigen Bauen leisten. Im Rahmen des Teilprojekts B wurde die Bewertung dieser Potenziale anhand von Beispielen ausgebaut und verifiziert. Die Basis dieser Bewertungsgrundlage ist die Erfüllung der grundlegenden technischen Anforderungen (ökobilanzielle Indikatoren, vergleichende ökobilanzielle Betrachtung). Im Teilprojekt E geht es um die Freisetzung umweltrelevanter Stoffe aus zementgebundenen Baustoffen. Überprüft werden sollte die Übereinstimmung zwischen Laborergebnissen, Modellierungen und realen Grundwasserkonzentrationen. Es wurden Schlitzwände errichtet, die in den Grundwasserleiter einbinden und umweltrelevante Parameter bestimmt. Grundsätzlich hat sich selbst bei Großbaustellen nur eine geringe Beeinflussung der Grundwasserqualität durch Beton ergeben.
Raman microspectroscopy provides the means to obtain local orientations on polycrystalline materials at the submicrometer level. The present work demonstrates how orientation-distribution maps composed of Raman intensity distributions can be acquired on large areas of several hundreds of square micrometers. A polycrystalline CuInSe2 thin film was used as a model system. The orientation distributions are evidenced by corresponding measurements using electron backscatter diffraction (EBSD) on the same identical specimen positions. The quantitative, local orientation information obtained by means of EBSD was used to calculate the theoretical Raman intensities for specific grain orientations, which agree well with the experimental values. The presented approach establishes new horizons for Raman microspectroscopy as a tool for quantitative, microstructural analysis at submicrometer resolution.
Neben den EG-Baumusterprüfungen und Konformitätsbewertungen, die von der BAM als Benannte Stelle nach den Richtlinien 2014/28/EU und 2013/29/EU durchgeführt werden, gibt es auch immer wieder Anfragen von Behörden, Herstellern oder Anwendern zur gesonderten Überprüfung von Zündern. Diese Anfragen liegen hauptsächlich in den Bereichen Identifizierung von Fundzündern, Untersuchungen an Versagerzündern/überlagerten Zündern sowie externe Qualitätssicherung von Firmen. Die Vorgehensweise und die Prüfmethoden, die bei solchen Untersuchungen zum Einsatz kommen, werden vorgestellt und an Beispielen erläutert.
Rainfall-triggered runoff is a major driver of pesticide input in streams. Only few studies have examined the suitability of passive sampling to quantify such episodic exposures. In this study, we used Empore-TM styrene-divinylbenzene reverse phase sulfonated disks (SDB disks) and event-driven water samples (EDS) to assess exposure to 15 fungicides and 4 insecticides in 17 streams in a German vineyard area during 4 rainfall events. We also conducted a microcosm experiment to determine the SDB-disk sampling rates and provide a free-software solution to derive sampling rates under time-variable exposure. Sampling rates ranged from 0.26 to 0.77 L d-1 and time-weighted average (TWA) concentrations from 0.05 to 2.11 µg/L. The 2 sampling systems were in good agreement and EDS exceeded TWA concentrations on average by a factor of 3. Our study demonstrates that passive sampling is suitable to quantify episodic exposures from polar organic pesticides.
Magnetic domains have been the subject of much scientific investigation since their theoretical existence was first postulated by P.-E. Weiss over a century ago. Up to now, the three-dimensional (3D) domain structure of bulk magnets has never been observed owing to the lack of appropriate experimental methods. Domain analysis in bulk matter thus remains one of the most challenging tasks in research on magnetic materials. All current domain observation methods are limited to studying surface domains or thin magnetic films. As the properties of magnetic materials are strongly affected by their domain structure, the development of a technique capable of investigating the shape, size and distribution of individual domains in three dimensions is of great importance. Here, we show that the novel technique of Talbot-Lau neutron tomography with inverted geometry enables direct imaging of the 3D network of magnetic domains within the bulk of FeSi crystals.
This overview article provides insight into how to apply Raman spectroscopy in combination with a confocal, optical microscope setup on polycrystalline material systems, in order to obtain quantitative information on phase distribution, grain sizes, crystal orientations and microstrain. Although the present work uses Cu(In,Ga)(S,Se)₂ absorber layers in corresponding thin-film solar cells as a model system to demonstrate the capabilities of Raman microspectroscopy, the approaches discussed may be applied to any organic or inorganic, polycrystalline materials system.
This paper gives a brief overview on3D imaging of magnetic domains with shearing grating neutron tomography. We investigated the three-dimensional distribution of magnetic domain walls in the bulk of a wedge-shaped FeSi single crystal. The width of the magnetic domains wasanalyzed at different locations within the crystal. Magnetic domains close to the tip of the wedge are much smaller than in the bulk. Furthermore, the three-dimensional shape of individual domains wasinvestigated. We discuss prospects and limitations of the applied measurement technique.
More than 5 million non-electric detonators are used annually in Germany for blasting operations. The relative usage of non-electric detonators amounts to about 50% of all civil blasting operations in Germany. BAM, as the notified body for explosives in Germany, tests non-electric detonators for the purpose of EU-type approval under the civil explosives directive, but also in the context of general investigations, e.g. when misfiring occurs. BAM has all facilities to test these detonators according to the European standard EN 13763. The presentation will cover the test facilities of BAM and address some issues of delay time accuracy. Several advantages and disadvantages of the non-electric ignition system will be discussed in the context of case investigations, and conclusions for mining operations and the advoidance of misfiring will be drawn.
In der Abteilung „Chemische Sicherheitstechnik" der BAM wurden mittels Ultra-Hochgeschwindigkeitsvideotechnik Grundlagenuntersuchungen zu Detonationsverhalten und Splitterwirkung von sogenannte "schlagwettersichern” Sprengzündern in normaler und in explosionsfähiger Atmosphäre durchgeführt. Es konnte eine maximale Splittergeschwindigkeit von 2,4 km/s ermittelt werden.
Microstrain distributions were acquired in functional thin films by high-resolution X-ray microdiffraction measurements, using polycrystalline CuInSe2 thin films as a model system. This technique not only provides spatial resolutions at the submicrometre scale but also allows for analysis of thin films buried within a complete solar-cell stack. The microstrain values within individual CuInSe2 grains were determined to be of the order of 10^-4. These values confirmed corresponding microstrain distribution maps obtained on the same CuInSe2 layer by electron backscatter diffraction and Raman microspectroscopy.
The investigation of the microstructure in functional, polycrystalline thin films is an important contribution to the enhanced understanding of structure–property relationships in corresponding devices. Linear and planar defects within individual grains may affect substantially the performance of the device. These defects are closely related to strain distributions. The present work compares electron and X-ray diffraction as well as Raman microspectroscopy, which provide access to microstrain distributions within individual grains. CuInSe₂ thin films or solar cells are used as a modelsystem. High-resolution electron backscatter diffraction and X-ray microdiffraction as well as Ramanmicrospectroscopy were applied for this comparison. Consistently, microstrain values were determined of the order of 10⁻⁴ by these three techniques. However,only electron backscatter diffraction, X-ray microdiffraction exhibit sensitivities appropriate for mapping local strain changes at the submicrometer level within individual grains in polycrystalline materials.
We present a combined experimental and theoretical study to solve the unit-cell and molecular arrangement of the tetracene thin film (TF) phase. TF phases, also known as substrate induced phases (SIP), are polymorphs that exist at interfaces and decisively impact the functionality of organic thin films, e.g., in a transistor channel, but also change the optical spectra due to the different molecular packing. As SIPs only exist in textured ultrathin films, their structure determination remains challenging compared to bulk materials. Here, we use grazing incidence Xray diffraction and atomistic simulations to extract the TF unit-cell parameters of tetracene together with the atomic positions within the unit-cell.
The impact of fracture geometry and aperture distribution on fluid movement and on non-reactive solute transport was investigated experimentally and numerically in single fractures. For this purpose a hydrothermally altered and an unaltered granite drill core with axial fractures were investigated. Using three injection and three extraction locations at top and bottom of the fractured cores, different dipole flow fields were examined. The conservative tracer (Amino-G) breakthrough curves were measured using fluorescence spectroscopy. Based on 3-D digital data obtained by micro-computed tomography 2.5-D numerical models were generated for both fractures by mapping the measured aperture distributions to the 2-D fracture geometries (x-y plane). Fluid flow and tracer transport were simulated using COMSOL Multiphysics®.
By means of numerical simulations and tomographic imaging experimentally observed breakthrough curves can be understood and qualitatively reproduced. The experiments and simulations suggest that fluid flow in the altered fracture is governed by the 2-D fracture geometry in the x-y plane, while fluid flow in the unaltered fracture seems to be controlled by the aperture distribution. Moreover, we demonstrate that in our case simplified parallel-plate models fail to describe the experimental findings and that pronounced tailings can be attributed to complex internal heterogeneities. The results presented, implicate the necessity to incorporate complex domain geometries governing fluid flow and mass transport into transport modeling.
A thorough characterization of base materials is the prereq- uisite for further research. In this paper, the characterization data of the reference materials (CEM I 42.5 R, limestone pow- der, calcined clay and a mixture of these three components) used in the second funding phase of the priority program 2005 of the German Research Foundation (DFG SPP 2005) are presented under the aspects of chemical and min- eralogical composition as well as physical and chemical properties. The data were collected based on tests performed by up to eleven research groups involved in this cooperative program.
We performed spatially resolved synchrotron-induced x-ray fluorescence analyses (SY-XRF) of five silverpoint drawings from the famous `Karlsruhe sketchbook´ and a silverpoint, which is assumed to be an original one used by the Renaissance artist Hans Baldung Grien (1484-1545) himself. The silverpoint, one out of a very small number of ancient styli conserved nowadays, is fixed on the so-called `Karlsruhe sketchbook´. Measurements were executed at the FLUO-TOPO beamline at the electron storage ring ANKA. It has been shown, that SY-XRF at this beamline is nondestructive and sensitive enough for the analysis of minor and major elements in the silver strokes. This study provides new insights into this graphical technique and ancient drawing instruments: results are that three drawings have been created with a common type of silverpoint containing about (10.4 ± 0.7) wt% of Cu. In all the cases, Hg at a 10% level by weight was identified in the strokes. Presence of Hg is not due to the original silver alloy, but is a result of a general alteration phenomenon of silverpoint drawings. This fact is confirmed by the analysis of the original silverpoint, which contains only small traces of Hg. The result for the copper content of the silverpoint (10.4 ± 1.7) wt% is in good agreement with that of these three drawings. It is supposable that the silverpoint found attached today served for the creation of the corresponding drawings. Moreover, the graphical technique of Baldung is found to be continual over three decades. Only one very late drawing dated to 1543 was probably realized with another silverpoint, containing about 3 wt% of Cu. This difference in the chemical composition of drawings from the late period might be used as a more precise dating indicator of Baldung drawings that are not clearly attributed to a certain period.
We compare standard and inverted bulk heterojunction solar cells composed of PCPDTBT:PC70BM
blends. Inverted devices comprising 100 nm thick active layers exhibited short circuit currents of
15 mA/cm², 10% larger than in corresponding standard devices. Modeling of the optical field distribution
in the different device stacks proved that this enhancement originates from an increased absorption of
incident light in the active layer. Internal quantum efficiencies (IQEs) were obtained from the direct
comparison of experimentally derived and modeled currents for different layer thicknesses, yielding IQEs
of ~70% for a layer thickness of 100 nm. Simulations predict a significant increase of the light harvesting
efficiency upon increasing the layer thickness to 270 nm. However, a continuous deterioration of the
photovoltaic properties with layer thickness was measured for both device architectures, attributed to
incomplete charge extraction. On the other hand, our optical modeling suggests that inverted devices
based on PCPDTBT should be able to deliver high power conversion efficiencies (PCEs) of more than
7% provided that recombination losses can be reduced.
One-pot covalent functionalization of 2D black phosphorus by anionic ring opening polymerization
(2022)
In this work, a one-pot approach for the covalent functionalization of few-layer black phosphorus (BP) by anionic ring opening polymerization of glycidol to obtain multifunctional BP-polyglycerol (BP-PG) with high amphiphilicity for near-infrared-responsive drug delivery and biocompatibility is reported. Straightforward synthesis in combination with exceptional biological and physicochemical properties designates functionalized BP-PG as a promising candidate for a broad range of biomedical applications.
Organic and inorganic nanoparticles (NPs) are increasingly used as drug carriers, fluorescent sensors, and multimodal labels in the life and material sciences. These applications require knowledge of the chemical nature, total number of surface groups, and the number of groups accessible for subsequent coupling of e.g., antifouling ligands, targeting bioligands, or sensor molecules. To establish the concept of catch-and-release assays, cleavable probes were rationally designed from a quantitatively cleavable disulfide moiety and the optically detectable reporter 2-thiopyridone (2-TP). For quantifying surface groups on nanomaterials, first, a set of monodisperse carboxy-and amino-functionalized, 100 nm-sized polymer and silica NPs with different surface group densities was synthesized. Subsequently, the accessible functional groups (FGs) were quantified via optical spectroscopy of the cleaved off reporter after its release in solution. Method validation was done with inductively coupled plasma optical emission spectroscopy (ICP-OES) utilizing the sulfur atom of the cleavable probe. This comparison underlined the reliability and versatility of our probes, which can be used for surface group quantification on all types of transparent, scattering, absorbing and/or fluorescent particles. The correlation between the total and accessible number of FGs quantified by conductometric titration, qNMR, and with our cleavable probes, together with the comparison to results of conjugation studies with differently sized biomolecules reveal the potential of catch-and-release reporters for surface analysis. Our findings also underline the importance of quantifying particularly the accessible amount of FGs for many applications of NPs in the life sciences.
We demonstrate the use of a 3D printed radial collimator in X-ray powder diffraction and surface sensitive grazing incidence X-ray diffraction. We find a significant improvement in the overall Signal to background ratio of up to 100 and a suppression of more than a factor 3⋅10⁵ for undesirable Bragg reflections generated by the X-ray “transparent” windows of the sample environment.
The background reduction and the removal of the high intensity signals from the windows, which limit the detector’s dynamic range, enable significantly higher sensitivity in experiments within sample environments such as vacuum chambers and gas- or liquid-cells. Details of the additively manufactured steel collimator geometry, alignment strategies using X-ray fluorescence, and data analysis are also briefly discussed. The flexibility and affordability of 3D prints enable designs optimized for specific detectors and sample environments, without compromising the degrees of freedom of the diffractometer.