Analytische Chemie
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Because of its mobility and ability to investigate exposed surfaces, single-sided (SiS) nuclear magnetic resonance (NMR) technology enables new application fields in geosciences. To test and assess its corresponding potential, we compare longitudinal (T1) and transverse (T2) data measured by SiS NMR with those of conventional geoscientific laboratory NMR. We use reference sandstone samples covering a broad range of pore sizes. Our study demonstrates that the lower signal-to-noise ratio of SiS NMR data generally tends to slightly overestimated widths of relaxation time distributions and consequently pore size distributions. While SiS and conventional NMR produce very similar T1 relaxation data, unbiased SiS NMR results for T2 measurements can only be expected for fine material, i.e. clayey or silty sediments and soils with main relaxation times below 0.05s. This limit is given by the diffusion relaxation rate due to the gradient in the primary magnetic field associated with the SiS NMR. Above that limit, i.e. for coarse material, the relaxation data is strongly attenuated. If considering the diffusion relaxation time of 0.2 s in the numerical data inversion process, the information content >0.2s is blurred over a range larger than that of conventional NMR. However, our results show that principle range and magnitudes of the relaxation time distributions are reconstructed to some extent. Regarding these findings, SiS NMR can be helpful to solve geoscientific issues, e.g. to assess the hydro-mechanical properties of the walls of underground facilities or to provide local soil moisture data sets for calibrating indirect remote techniques on the regional scale. The greatest opportunity provided by the SiS NMR technology is the acquisition of profile relaxation data for rocks with significant bedding structures at the µm scale. With this unique feature, SiS NMR can support the understanding and modeling of hydraulic and diffusional anisotropy behavior of sedimentary rocks.
Integration of fiber reinforcement in high-performance cementitious materials has become widely applied in many fields of construction. One of the most investigated advantages of steel Fiber reinforced concrete (SFRC) is the deceleration of crack growth and hence its improved sustainability.
Additional benefits are associated with its structural properties, as fibers can significantly increase the ductility and the tensile strength of concrete. In some applications it is even possible to entirely replace the conventional reinforcement, leading to significant logistical and environmental benefits.
Fiber reinforcement can, however, have critical disadvantages and even hinder the Performance of concrete, since it can induce an anisotropic material behavior of the mixture if the fibers are not appropriately oriented. For a safe use of SFRC in the future, reliable non-destructive testing (NDT) methods need to be identified to assess the fibers’ orientation in hardened concrete. In this study,
ultrasonic material testing, electrical impedance testing, and X-ray computed tomography have been investigated for this purpose using specially produced samples with biased or random Fiber orientations. We demonstrate the capabilities of each of these NDT techniques for fiber orientation measurements and draw conclusions based on these results about the most promising areas for future research and development.
To date, the destructive extraction and analysis of drilling cores is the main possibility to obtain depth information about damaging water ingress in building floors. The time- and costintensive procedure constitutes an additional burden for building insurances that already list piped water damage as their largest item. With its high sensitivity for water, a ground-penetrating radar (GPR) could provide important support to approach this problem in a non-destructive way. In this research, we study the influence of moisture damage on GPR signals at different floor constructions. For this purpose, a modular specimen with interchangeable layers is developed to vary the screed and insulation material, as well as the respective layer thickness. The obtained data set is then used to investigate suitable signal features to classify three scenarios: dry, damaged insulation, and damaged screed. It was found that analyzing statistical distributions of A-scan features inside one B-scan allows for accurate classification on unknown floor constructions. Combining the features with multivariate data analysis and machine learning was the key to achieve satisfying results. The developed method provides a basis for upcoming validations on real damage cases.
An Ontology-Based Approach to Enable Data-Driven Research in the Field of NDT in Civil Engineering
(2021)
Although measurement data from the civil engineering sector are an important basis for scientific analyses in the field of non-destructive testing (NDT), there is still no uniform representation of these data. An analysis of data sets across different test objects or test types is therefore associated with a high manual effort. Ontologies and the semantic web are technologies already used in numerous intelligent systems such as material cyberinfrastructures or research databases. This contribution demonstrates the application of these technologies to the case of the 1H nuclear magnetic resonance relaxometry, which is commonly used to characterize water content and porosity distri-bution in solids. The methodology implemented for this purpose was developed specifically to be applied to materials science (MS) tests. The aim of this paper is to analyze such a methodology from the perspective of data interoperability using ontologies. Three benefits are expected from this ap-proach to the study of the implementation of interoperability in the NDT domain: First, expanding knowledge of how the intrinsic characteristics of the NDT domain determine the application of semantic technologies. Second, to determine which aspects of such an implementation can be improved and in what ways. Finally, the baselines of future research in the field of data integration for NDT are drawn.
When applying Ground Penetrating Radar (GPR) to assess the moisture content of building materials, different medium properties, dimensions, interfaces and other unknown influences may require specific strategies to achieve useful results. Hence, we present an overview of the various approaches to carry out moisture measurements with GPR in civil engineering (CE). We especially focus on the applied Signal features such as time, amplitude and frequency features and discuss their limitations. Since the majority of publications rely on one single feature when applying moisture measurements, we also hope to encourage the consideration of approaches that combine different signal features for further developments.
The moisture content of the subfloor has to be determined before installation to avoid damages of the floor covering. Only if the readiness for layering is reached, an installation without damages can be expected in all cases. In general, three different approaches exist to measure the residual water content: determination of the moisture content, determination of the water release, or determination of the corresponding relative humidity. All three approaches are tested in laboratory at eight different screed types including two different samples thicknesses in each case. The moisture content and the water release are measured by sample weighing, the corresponding relative humidity is measured by embedded sensors. All three approaches are compared and correlated to each other. The evaluations show only weak correlation and, in several cases, contradicting results. Samples are considered as being ready for layering and not-being ready for layering at the same time, depending on the chosen approach. Due to these contradicting results, a general threshold for the risk of damage cannot be derived based on these measurements. Furthermore, the experiment demonstrates that the measurement of corresponding relative humidity is independent of the considered screed type or screed composition. This makes the humidity measurement to very promising approach for the installation of material moisture monitoring systems in the future.
Relaxation phenomena observed in the electrical low-frequency range (approximately 1 mHz-10 kHz) of natural porous media like sandstones is often assumed to be directly related to the dominant (modal) pore throat sizes measured, for instance, with mercury intrusion porosimetry. Attempts to establish a universally valid relationship between pore size and peak Spectral Induced Polarization (SIP) relaxation time have failed, considering sandstones from very different origins and featuring great variations in textural and chemical compositions as well as in geometrical pore space properties. In addition working with characteristic relaxation times determined in Cole-Cole or Debye decomposition fits to build the relationship have not been successful. In particular, samples with narrow pore throats are often characterized by long SIP relaxation times corresponding to long “characteristic length scales” in these media, assuming that the diffusion coefficients along the electrical double layer were constant. Based on these observations, three different types of SIP relaxation can be distinguished. We present a new way of assessing complex pore spaces of very different sandstones in a multi-methodical approach to combine the benefits of mercury intrusion porosimetry, micro-computed tomography, and nuclear magnetic resonance. In this way, we achieve much deeper insight into the pore space due to the different resolutions and sensitivities of the applied methods to both pore constrictions (throats) and wide pores (pore bodies). We experimentally quantify pore aspect ratios and volume distributions within the two pore regions. We clearly observe systematic differences between three SIP relaxation types identified previously and can attribute the SIP peak relaxation times to measured characteristic length scales within our materials. We highlight selected results for a total of nine sandstones. It seems that SIP relaxation behavior depends on the size difference of the narrow pore throats to the wide pore bodies, which increases from SIP Type 1 to Type 3.
Dehydration is a common process occurring in natural environments, rocks, and building materials. Suitable methods for monitoring the changing moisture content should be identified.
We have investigated the impact of dehydration of sandstones on complex conductivity spectra. Spectral induced polarization measurements were performed on five sandstone samples during evaporative drying. The complex conductivity spectra indicate considerable changes with decreasing saturation. The relationship between conductivity and saturation can be described by a power law known as the second empirical Archie equation. Separate saturation exponents have been determined for the real and imaginary parts of conductivity. The imaginary part of conductivity indicates higher saturation exponents for the investigated sandstones compared to the real part. Obviously, the saturation exponents depend on the method used for changing water saturation. Evaporative drying, which is used in our experiments, causes an increase of pore-water salinity and results in lower saturation exponents for the real part of conductivity but higher exponents for the imaginary part in comparison with the classical imbibition/Drainage technique. We evaluate a theoretical approach that considers the influence of pore water salinity on the saturation exponents of the real and imaginary parts of conductivity. The complex conductivity spectra are processed by a Debye decomposition procedure.
The resulting integrating parameters such as direct current resistivity, total chargeability, normalized chargeability, and mean relaxation time indicate a power law dependence on saturation. Our experiments indicate that the imaginary part of conductivity and normalized chargeability have a high sensitivity related to the drying process of rocks and might be suitable indicators to Monitor the changes of moisture content in sandstones.
The presented work discusses the accuracy of Laser Induced Breakdown Spectroscopy (LIBS) in determining the total chloride content in cement pastes. LIBS as an emission spectroscopy method is used to detect simultaneously several elements present in cement-based materials. By scanning surfaces the variability in the spatial distribution of elements can be visualised. However, for a quantification of the results, studies are necessary to characterise possible influences due to the wide variation of the chemical compositions in which cement can occur. It is shown how the calibration can be done, how the calibration samples were produced, and which statistical parameters are necessary to describe the precision of the regression. The performance of LIBS is estimated by detecting chloride in validation samples. Therefore, 55 samples and 7 ets with changing mix ompositions were produced. The presented study deals with possible influences of different mix compositions, ncluding different cations of chloride, varying w/c-ratios and the artial replacement of Portland cement with last furnace slag (50% BFS) and limestone (30% LS). Comparing the LIBS results with otentiometric titration, n accuracy of±0.05 wt%/total has been determined.
The determination of chloride is still one of the main tasks for the evaluation of reinforced concrete structures.
The corrosion of the reinforcement induced by the penetrating chlorides is the dominant damage process affecting the lifetime of concrete structures. In the recent years different research groups demonstrated that LIBS can be a fast and reliable method to quantify chlorine in cement-bound materials. Because chlorine in concrete can only occur as solved ions in the pore solution or bound in salts or hydrated cement phases, the detected emission of chlorine can be correlated with the chloride concentration determined e.g. with potentiometric titration. This work inter alia describes the production of reference samples and possible side effects during the production process. Due to transport processes in the porous matrix of the cement a misinterpretation of the concentrations is possible. It is shown how to overcome these effects and higher precisions of the single measurements can be realised. Using the calibration method, blank sample method and noise method, three different ways of calculating the limit of detection (LOD) and limit of quantification (LOQ) are compared. Due to the preparation of the reference samples a precision of the whole calibration model of sx0 = 0.023 wt% is determined.
The validation of the model is based on different test sets, which are varying in their composition
(different Cl-salts, water-to-cement ratios and additives). The determined mean error of the validation is
0.595 ± 0.063 wt%, which is comparable to standardised methods like potentiometric titration, direct potentiometry
or photometry (0.40 ± 0.06 wt%) [1].