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The analysis of the chemical composition of cement-based materials like concrete is a crucial task in civil engineering. Concrete is a multi-phase material made of cement, water, aggregates, additives and admixtures. During the damage assessment of concrete structures, the external ingress of harmful species like chlorine, alkalis or sulfates needs to be determined. In order to provide a fast and precise analysis of concrete the application of LIBS offers unique possibilities as the technique can detect all elements at air atmosphere.
To determine the condition of concrete, the information about the chemical composition, the ingress of harmful species as well as the evaluation of characteristic values like the used cement type or the type of aggregates are needed. This work presents the two-dimensional evaluation of concrete samples using LIBS and multivariate data analysis of atomic and molecular emission. For the evaluation of the main components different classification methods will be applied to identify the heterogeneity of the samples. With respect to their specific phase, different species will be quantified using multivariate regression (PLS) and important figures of merit will be presented. All results will be verified using Standard procedure of wet chemistry (XRF, potentiometric titration and ICP-OES).
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.
A big part of the infrastructure is made of concrete, which is a multiphase system made of cement, aggregates, water and pores. Concrete is often used in combination with steel as reinforced concrete. Environmental influences, especially the ingress of harmful ions in combination with the ingress of water, trigger different damage processes which reduce the designed lifetime of a structure. The ingress of chlorides from de-icing salt or sea water leads to corrosion of the reinforcement. In addition, the carbonation of the concrete may trigger the corrosion of the reinforcement. The ingress of alkalis from deicing salts may cause the expansion of the amorphous silica aggregates (alkali-silica reaction) through
formation of a swelling gel of calcium silicate hydrate if water is present. The ingress of sulphates may cause spalling of the concrete surface due to ettringite formation.
For the standard procedure in civil engineering cores are taken, cut in slices, grinded and the obtained homogenized powder is solved in acid and investigated by standard procedures.
BAM has developed the LIBS technique for the 2D evaluation of the chemical composition of concrete. The technique is established for automated laboratory use with high numbers of samples to investigate transport processes of harmful species (Cl-, CO2 , SO4 2-and alkalis) in concrete. Information about ingress depth and the quantitative values are important to estimate the remaining lifetime of the infrastructure. LIBS is a surface technique. To get information about the ingress depth, a drill core has to be taken and cut in the middle. The measurements are carried out at the cross section. The main advantages of LIBS are the direct measurement on the surface of the concrete, fast analysis (sample rate 100 Hz) with a spatial resolution of up to 100 µm, the consideration of the heterogeneity of the concrete and the possibility of automated measurements which save a lot of manpower and time. As an example the investigation of ingress profiles for standard diffusion and migration tests in civil engineering takes hours in comparison to just a few minutes using LIBS. At the same time a 2D-evaluation provides information about hot spots of elemental concentration which may not be found by standard methods.
The state of the art of LIBS technique for applications in civil engineering will be presented, including typical results of 2D investigation of concrete in laboratory. The performance is also demonstrated by examples for onsite applications using a mobile LIBS system. The road map to standardization is presented as well.
In civil engineering, the laser-induced breakdown spectroscopy has been applied as a fast and reliable method for a quantitative evaluation of concrete cores. Due to a two-dimensional scanning, the heterogeneity of concrete can be evaluated and elements like Cl, Na, and S are related to the cement matrix only. This study deals with the temporal evaluation and imaging of laser-induced plasmas on cement-based materials, in order to investigate the impact of aggregates with diffrent grain size on the spectral response in LIBS.
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).