Analytische Chemie
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Zur Bestimmung des Feuchtezustands und insbesondere der Belegereife von Estrichfußböden kommen in Deutschland zerstörende Prüfverfahren zum Einsatz, die eine punktuelle Probenahme erfordern. Hierbei ergeben sich immer wieder Fehlinterpretationen, da zum einen die Probenahme selbst zu einer Veränderung des Feuchtezustands führt und zum anderen, weil die Verfahren an sich mitunter ungenau sind (z.B. abhängig von der Estrichzusammensetzung). Zusammen mit vier Forschungsinstituten und dem Industriepartner Bosch wurden an der BAM zerstörungsfreie Prüfverfahren auf deren Tauglichkeit zur Estrichfeuchtemessung untersucht und mit den herkömmlichen zerstörenden Verfahren verglichen.
Für diesen Versuch kamen verschiedene geophysikalische Verfahren zum Einsatz, darunter Nuklear Magnetische Resonanz (NMR), elektrische Widerstandsmessungen und Impulsradar (GPR). Es wurden neun verschiedene Estrichsorten hergestellt und während der Trocknungsphase bei Konstant-Normklima gelagert. Diese wurden sowohl zerstörend als auch zerstörungsfrei mit den o. g. Verfahren untersucht. Gleichzeitig wurden die Masseänderungen der Proben zur Bestimmung des integralen Feuchtehalts aufgezeichnet.
Die Ergebnisse zeigen zum einen, dass das Abtrocknungsverhalten von zementgebundenen Estrichen grundsätzlich unterschiedlich von dem anhydritgebundener Estriche ist. Während sich bei ersteren zügig ein deutlicher Feuchtegradient über die Höhe der Proben einstellt, verläuft dieser bei der zweiten Probengruppe sehr flach. Dies lässt sich vor allem in den NMR Daten räumlich hochaufgelöst nachvollziehen - die Datenakquise erfolgte mit einer NMR MOUSE PM 25. Ein ähnliches Bild ergibt sich auch aus den elektrischen Widerstandsmessungen, die mittels sog. Multi-Ring-Elektroden (MRE) durchgeführt wurden. MRE bezeichnen als Vertikalprofil angeordnete Ringelektroden mit einem Abstand von ca. 1-2 mm, zwischen denen jeweils Zwei-Punkt Widerstandsmessungen durchgeführt werden. Bei sehr geringen Feuchtegehalten (z.T. auch um die Belegereife) waren mit dieser Methode jedoch wegen der zu hohen Übergangswiderstände nur bedingt Messungen möglich. Im Gegensatz zu NMR und MRE sind mit dem Radarverfahren (2 GHz Antenne) keine tiefenbezogenen Aussagen möglich. Jedoch lässt sich über eine Amplitudenauswertung von direkter und an der Rückwand reflektierter Welle teilweise eine Aussage über Restfeuchtigkeit im Volumen treffen. Ebenso zeigt die Laufzeitdifferenz der beiden Wellen eine starke Abhängigkeit vom Feuchtegehalt.
In Germany there is an existing built infrastructure worth about 50 trillion Euros. The expected lifetimes of individual structures are up to 100 years. Considerable costs (annually about 35 billion Euros, the trend continues upwards) are involved in order to maintain and rehabilitate both residential as well as transportation infrastructure buildings. Most damages we observe on our built infrastructure are moisture-induced processes. Consequently reliable moisture measurement tools a highly needed for meaningful building diagnosis investigations. The optimal moisture measuring technique would be non-destructive, fast, repeatable, reliable, independent of steel in the vicinity, the surface condition or possible salt loads of the material under test. Since this is unfortunately not the case for any non-destructive method, it is often very difficult to decide for users which method to use for the particular testing problem. The only standardized methods in Germany are the “direct” and destructive Darr- and the CM tests. Although they can be highly accurate (when handled with care during the sampling), they deliver only punctual information and cannot be used for monitoring. The other, non-destructive methods are based on the change in humidity-dependent physical material properties. The underlying physics, their particular advantages and disadvantages are discussed in this paper.
The surface chemistry / functionalization of nanomaterials and microparticles largely controls the stability of these materials as well as their solubility and subsequent biofunctionalization and their interactions with biological systems. Moreover, in the case of some nanomaterials like semiconductor quantum dots or lanthanide-based upconversion nanocrystals, the ligand shell strongly affects their optical properties, e.g., via passivation of surface states and traps that favor luminescence quenching or the protection of surface atoms from quenching water molecules. This renders analytical methods for the quantification of surface groups like functionalities very important. Targets of broad interest are here amino, carboxyl, alkine and maleimide groups used for common bioconjugation reactions and typical ligands like thiols and polyethylene glycol (PEG) molecules of varying length, used for the tuning of material hydrophilicity and biocompatibility, minimization of unspecific interactions, prevention of biofouling, and enhancement of blood circulation times as well as surface-bound biomolecules like streptavidin or other biomolecules relevant e.g., for diagnostic assays. Here, we focus on simple optical methods relying on standard laboratory instrumentation, validated by method comparison and/or mass balances and present examples for their use for the characterization of different types of nanomaterials and microparticles.
Luminescence-based detection methods, ranging from fluorescence spectroscopy for photophysical and mechanistic studies over sensing applications, chromatographic separation techniques and the microarray technology with fluorescence detection to fluorescence microscopy, flow cytometry, single molecule spectroscopy, and molecular imaging to integrating sphere spectroscopy, are among the most widely used methods in the life and material sciences. This is due to e.g., their unique sensitivity enabling the detection of single molecules, potential for multiplexing, ease of combination with spatial resolution, and suitability for remote sensing. Many of these advantages are closely linked to the choice of suitable molecular and nanoscale fluorescent reporters, typically required for signal generation. This includes organic dyes without and with sensor function, fluorophore-encoded polymeric and silica nanoparticles as well as nanocrystalline systems like semiconductor quantum dots and upconversion phosphors, emitting in the visible (vis), near-infrared (NIR), and IR (infrared). Current challenges present the environment sensitivity of most fluorophores, rendering fluorescence spectra, measured intensities/fluorescence quantum yields, and fluorescence decay kinetics matrix-dependent, and instrument-specific distortions of measured fluorescence signals that need to be considered for quantification and comparability of data, particularly fluorescence spectra.
Here, current applications of luminescence-based methods and different types of reporters will be presented. In this context, suitable spectroscopic tools for the characteri-zation of the optical properties of fluorescent reporters and fluorophore-encoded microparticles, analytical tools for the determination of the surface chemistry of different types of particles, and different multiplexing strategies will be discussed.
The reliability of wheel set axle testing is of high importance because small discontinuities caused during manufacturing or rock fall impacts during operation might cause growing cracks during the operation load cycles. While most of the axles are tested by automated UT-systems today, the basic education of railway NDT operators is still manual testing providing the basic understanding and skills for the operators. In Germany it is a common rule that NDT operators in the railway branch need to refresh their knowledge and skills every five years including a refresh examination. The testing results from these exercises and from a parallel round robin test have been sampled at the DGZfP Railway Education Centre in Wittenberge for a period of about 5 years. The results of the operators written in test record sheets were compared with the “true” test crack or notch position in the axles used for examination. In this way the testing results could be categorized into “hits” and “misses” and the “hits” were further evaluated due to correct position and adequate amplitude height. Considering some thousand indications documented by the operators during the refresh examination and comparing transition bow, shaft and seat it was a highlight to see that the operators reach their best detection rate in the transition bow of the wheel axle set while this is often the most difficult part concerning the UT-echoes. Fortunately this is due to their raised awareness in the transition bow region because this is the most dangerous region with respect to fracture mechanics.
For two selected axles the experimental set up of 45° and 70° inward and outward UT-testing were also simulated showing clearly the difficulties of the UT-echoes detection of some specific test defects.
In the last two decades automated ultrasonic inspection devices took over a lot of applications that prior have been carried out using manual inspection with the evaluation of A-scans only. In parallel phased array systems have been developed and brought to the market which offer detailed and fast control over the sound field. When applying automated inspection phased array systems for UT measurements imaging of the recorded data in combination with the probe positioning data is used for the evaluation of inspections. B-Scan, C-Scan and S-Scan images are typically used with this setup.
For more sophisticated applications with linear arrays echo tomography and syntethic aperture focusing technique (SAFT) are well known methods and often applied for high resolution image reconstruction. Since channel count of phased array systems is constantly rising, matrix arrays with up to 256 elements entered the market. Signal processing in the matrix domain became 3D. Since some years the Total Focusing Method (TFM) is an additional imaging tool for these type of application. It is based on the Full Matrix Capture (FMC) using the elements of phased array probes as separate transmitters and receivers.
In this contribution we discuss the common ground of SAFT and TFM as well as the differences between these imaging tools. The combined use of automated inspection, matrix arrays and signal processing for high resolution measurements is a challenging task where a very long parameter list has to be taken into account. Under which conditions which elements of the full matrix should be taken for the reconstruction for best results?
Based on examples taken from measured and simulated echo signals it will be shown how image resolution can be optimized in dependence of different parameters like the distance between transmitters and receivers and their directivity patterns, the depth of echo source and the specimen geometry.
Ray tracing boudary value problems: simulation and SAFT reconstruction for ultrasonic testing
(2016)
The application of advanced imaging techniques for the ultrasonic inspection of inhomogeneous anisotropic materials like austenitic and dissimilar welds requires information about acoustic wave propagation through the material, in particular travel times between two points in the material. Forward ray tracing is a popular approach to determine traveling paths and arrival times but is ill suited for inverse problems since a large number of rays have to be computed in order to arrive at prescribed end points. In this contribution we discuss boundary value problems for acoustic rays, where the ray path between two given points is determined by solving the eikonal equation. The implementation of such a two point boundary value ray tracer for sound field simulations through an austenitic weld is described and its efficiency as well as the obtained results are compared to those of a forward ray tracer. The results are validated by comparison with experimental results and commercially available UT simulation tools. As an application, we discuss an implementation of the method for SAFT (Synthetic Aperture Focusing Technique) reconstruction. The ray tracer calculates the required travel time through the anisotropic columnar grain structure of the austenitic weld. There, the formulation of ray tracing as a boundary value problem allows a straightforward derivation of the ray path from a given transducer position to any pixel in the reconstruction area and reduces the computational cost considerably.
Quantification of rock structures with high resolution X-Ray μ-CT for laboratory SIP measurements
(2016)
Spectral Induced Polarization (SIP) measurements are used in many different ways to characterize natural rocks and soils. Main foci of interest are the enhanced characterization of the causes of IP-effects in clastic rocks (especially sandstones), the interactions between the matrix-fluid-system and within the electrical double layers as well as the correlation with “classical” petrophysical parameters, such as specific surface area, permeability, mercury intrusion capillary pressure (MICP) and others. Nevertheless, for all of these investigations, knowledge of the inner structure of the sample material is essential in order to create reliable and validated models as well as to interpret and to assess the data most completely. Unfortunately, many of the methods used, to get access to the inner structure of rocks are destructive (e.g. MICP, thin sectioning, etc.) and the valuable sample is lost. In addition, data is either of volume integrated nature or only available for the 2D case and the usage of sister cores does not necessarily lead to reliable results. In this paper, the authors showcase the possibilities of non-destructive and three dimensional X-ray computed tomography and of enhanced image analysis capabilities for the quantification of rock structures at the pore scale.
Permeability estimation from spectral induced polarization (SIP) measurements is based on a fundamental premise that the characteristic relaxation time (t) is related to the effective hydraulic radius (reff) controlling fluid flow. The approach requires a reliable estimate of the diffusion coefficient of the ions in the electrical double layer. Others have assumed a value for the diffusion coefficient, or postulated different values for clay versus clay-free rocks. We examine the link between t and reff for an extensive database of sandstone samples where mercury porosimetry data confirm that reff is reliably determined from a modification of the Hagen-Poiseuille equation assuming that the electrical tortuosity is equal to the hydraulic tortuosity. Our database does not support the existence of 1 or 2 distinct representative diffusion coefficients but instead demonstrates strong evidence for 6 orders of magnitude of variation in an apparent diffusion coefficient that is well correlated with both reff and the specific surface area per unit pore volume (Spor). Two scenarios can explain our findings: (1) the length-scale defined by t is not equal to reff and is likely much longer due to the control of pore surface roughness; (2) the range of diffusion coefficients is large and likely determined by the relative proportions of the different minerals (e.g. silica, clays) making up the rock. In either case, the estimation of reff (and hence permeability) is inherently uncertain from SIP relaxation time.
Moisture measurement methods
(2016)
Moisture can cause imperfect sealings, faulty roof constructions, cracks and other kind of damages. For measuring the moisture in construction materials like concrete and screed, there are destructive(direct) and non-destructive(indirect) methods, that can be used. This presentation gives an overview and a comparison of these methods.