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This paper will address the relevance of chloride measurements in practice for durability condition assessment and a description of the working principle of LIBS will be given. Examples of chloride profiles obtained by the common wet chemical analysis will be shown and compared with results from LIBS measurements as to demonstrate the accuracy of the LIBS-technique. The latter will be supported by clear graphs. In addition examples on the extra information resulting from measurements performed with LIBS for improvement of condition assessment and prediction will be shown.
New possibilities for concrete analysis 4.0 with the Laser-Induced Breakdown Spectroscopy (LIBS)
(2020)
In civil engineering the damage assessment of concrete infrastructures is an important task to monitor and ensure the estimated life-time. The aging of concrete is caused by different damage processes like the chloride induced pitting corrosion of the reinforcement. The penetration depth and the concentration of harmful species are crucial factors in the damage assessment. As a highly cost and time-consuming standard procedure, the analysis of concrete drill cores or drilling by wet-chemistry is widely used. This method provides element concentration to the total mass as aggregates and binder are homogenized. In order to provide a method that is capable to detect the element concentration regarding the cement content only, the laser-induced breakdown spectroscopy (LIBS) will be presented. The LIBS method uses a focused pulsed laser on the sample surface to ablate material. The high-power density and the laser-material interaction causes a laser-induced plasma that emits elemental and molecular line emission due to energy transition of the excited species in the plasma during the cooling phase.
As each element provides element-specific line emission, it is in principle possible to detect any element on the periodic table (spectroscopic fingerprint) with one laser shot. In combination with a translation stage the sample under investigation can be spatially resolved using a scan raster with a resolution up to 100 µm (element mapping). Due to the high spatial resolution, the element distribution and the heterogeneity of the concrete can be evaluated. By using chemometrics the non-relevant aggregates can be excluded from the data set and the element concentration can be quantified and referred to a specific solid phase like the binding matrix (cement) only. In order to analyze transport processes like diffusion and migration the twodimensional element distributions can provide deep insight into the transport through the pore space and local enrichments of elements. As LIBS is a multi-elemental method it is also possible to compare the ingress and transport process of different elements like Cl, Na, K, S, C, and Li simultaneously and evaluate cross-correlations between the different ions. Furthermore, the element mapping allows to visualize the transport along cracks. This work will show the state of the art in terms of hardware and software for an automated LIBS system as well as different application for a concrete analysis 4.0. Focus will be the application of LIBS for a fast concrete analysis.
Laser-induced breakdown spectroscopy (LIBS) is a spectroscopic method for the analysis of the chemical composition of sample materials. Generally, the measurement of all elements of the periodic table is possible. In particular, light elements such as H, Li, Be, S, C, O, N and halogens can be measured. Calibration with matrix-matching standards allows the quantification of element concentrations. In combination with scanner systems, the two-dimensional element distribution can be determined. Even rough surfaces can be measured by online adjustment of the laser focus. LIBS can also be used on-site with mobile systems. Hand-held systems are available for point measurements.
Common applications include the investigation of material deterioration due to the ingress of harmful ions and their interaction in porous building materials. Due to the high spatial resolution of LIBS and the consideration of the heterogeneity of concrete, the determination of precise input parameters for simulation and modelling of the remaining lifetime of a structure is possible. In addition to the identification of materials, it is also possible to assess the composition for example of hardened concrete, which involves the cement or aggregate type used. Other important fields of application are the detection of environmentally hazardous elements or the material classification for sorting heterogeneous material waste streams during dismantling. Non-contact NDT for “difficult to assess” structures as an example application through safety glass or in combination with robotics and automation are also possible.
In this work, an overview of LIBS investigations on concrete is given based on exemplary laboratory and on-site applications.
Laser Induced Breakdown Spectroscopy – A Tool for Imaging the Chemical Composition of Concrete
(2022)
One of the most common causes of damage is the ingress of harmful ions into the concrete, which can lead to deterioration processes and affect structural performance. Therefore, the increasingly aging infrastructure is regularly inspected to assess durability. Regular chemical analysis can be useful to determine the extent and evolution of ion ingress and to intervene in a timely manner. This could prove more economical than extensive repairs for major damage, particularly for critical infrastructure. In addition to already established elemental analysis techniques in civil engineering such as potentiometric titration or X-ray fluorescence analysis, laser-induced breakdown spectroscopy (LIBS) can provide further important complementary information and benefits. The possibilities of LIBS are demonstrated using the example of a drill core taken from a parking garage.
Laser-induced breakdown spectroscopy (LIBS) is a spectroscopic method for detecting the chemical composition of optically accessible surfaces. In principle, the measurement of all elements of the periodic table is possible. System calibrations allow the quantification of element concentrations. In combination with scanner systems, the two-dimensional element distribution can be determined. Even rough surfaces can be measured by online adjustment of the laser focus. To detect element ingress into the concrete, typically cores are taken, cut in half, and LIBS measurements are performed on the cross-section. The high spatial resolution as well as the simultaneous multi-element analysis enables a separate evaluation of the binder-matrix and aggregates. Therefore, the element concentrations can be determined directly related to the cement paste. LIBS measurements are applicable in the laboratory, on-site and also over a distance of several meters.
Common applications include the investigation of material deterioration due to the ingress of harmful ions and their interaction in porous building materials. LIBS is able to provide precise input parameters for simulation and modelling of the remaining lifetime of a structure. Besides the identification of materials, also their composition can be determined on hardened concrete, such as the type of cement or type of aggregate. This also involves the identification of environmentally hazardous elements contained in concrete. Another possible application is the detection of the composition of material flows during dismantling. Non-contact NDT for “difficult to assess” structures as an example application through safety glass or in combination with robotics and automation are also possible.
This work presents the state of the art concerning LIBS investigations on concrete by showing exemplary laboratory and on-site applications.
Laser-induced breakdown spectroscopy (LIBS) is a combination of laser ablation and optical emission spectroscopy. Due to the possibility of direct measurements on the sample surface with a minimum of sample preparation investigations of building materials can be conducted quite fast. In combination with a scanning technique (translation stage or scanning mirrors head) 2D element distributions of harmful species like chlorides and alkalis are evaluated with a sub-mm resolution. By scanning a surface of typically 100 mm x 100 mm the heterogeneity of the material may be considered. LIBS is capable to identify hot spots in element concentration with a resolution of 0.1 mm or even smaller. A LIBS-system for the on-site application on building materials is, in cooperation with system developers and companies which will use this technique for investigation on real structures, under test at BAM. We present an example. Further work will focus on providing guidelines to establish LIBS as a standard procedure for chemical investigations of building materials.
In civil engineering concrete is the most used building material for making infrastructures like bridges and parking decks worldwide. It is as a porous and multiphase material made of aggregates with a defined grain size distribution, cement and water as well as different additives and admixtures depending on the application. Different grain sizes are important to ensure the needed density and compressive strength.
The resulting porous cement matrix contains a mixture of flour grains (aggregates with a grain size below 125 lm) and cement particles (particle size≈50lm). Harmful species like chlorides may penetrate together with water through the capillary pore space and may trigger different damage processes. The damage assessment of concrete structures in Germany is estimated due to the quantification of harmful elements regarding to the cement content only. In the evaluation of concrete using LIBS a two-dimensional scanning is necessary to consider the heterogeneity caused by the aggregates. Therefore, a LIBS system operating with a low energy NdCr:YAG laser, a pulse energy of 3 mJ, a wavelength of 1064 nm, a pulse width of 1.5 ns and a Repetition rate of 100 Hz has been used. Different Czerny-Turner spectrometers with CCD detectors in the UV and NIR range have been used for the detection. Large aggregates (macro-heterogeneity) can be excluded from the evaluation, whereas small aggregates in the range of the laser spot size (flour grains) cannot be spatially resolved. In this work the micro heterogeneity caused by flour grains and their impact on the quantification with LIBS will be discussed. To analyze the effect of changing grain sizes and ratios, the ablation behavior has been determined and compared. Samples with defined grain sizes were made and analyzed using LIBS.
The grain size distributions were analyzed with laser diffraction (LDA).