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Die chemische Analyse von Beton gehört bei der Ermittlung des Ist-Zustandes von Stahl- und Spannbetonbauwerken zu den grundlegenden Untersuchungen bei der Zustandserfassung. Der tiefenabhängige Chloridgehalt sowie der Karbonatisierungsfortschritt müssen bei der Bewertung des Ist-Zustandes, beim Instandsetzungsbedarf und ggf. bei der Planung eines erforderlichen Instandsetzungskonzeptes mit einbezogen werden. Seit Mitte der 1990er Jahre wird an der Bundesanstalt für Materialforschung und -prüfung die laserinduzierte Plasmaspektroskopie (engl. Laser-induced Breakdown Spectroscopy) – kurz LIBS – stetig für die chemische Analyse von Beton weiterentwickelt. In diesem Beitrag wird der aktuelle Stand der Forschung/ Technik und der Normungsarbeit präsentiert, sowie zukünftig mögliche Anwendungen vorgestellt. Mit den aktuellen LIBS-Systemen (mobiles LIBS-System sowie kommerziell erhältliche Laborsysteme) ist es möglich den Chloridgehalt ortsaufgelöst in wenigen Minuten zu quantifizieren, sogenannte Elementlandkarten zu erstellen und somit die Elementverteilung innerhalb des Betons zu visualisieren. Durch das Scannen eines Bohrkernquerschnittes und der simultanen Erfassung von mehreren Elementen mit einer Messung, ist es zudem möglich, die Gesteinskörnung in den Messdaten zu identifizieren und den Chloridgehalt auf die Zementsteinmatrix zu beziehen. Fehlerquellen aus der Umrechnung der betonbezogenen Chloridgehalte können dadurch minimiert werden. Neben den Grundlagen von LIBS werden vor allem aktuelle Praxisbeispiele vorgestellt, die die aktuellen Möglichkeiten des Verfahrens veranschaulichen.
Die Laser induzierte Breakdown Spektroskopie (LIBS) bietet für die Analyse heterogener, mineralischer Baustoffe, wie z. B. Beton, deutliche Vorteile gegenüber konventionellen Methoden. Sie ermöglicht neben der Quantifizierung von Elementgehalten und -verteilungen im Baustoff auch die Differenzierung von Elementkonzentrationen innerhalb einzelner Phasen im Baustoff. So können beispielsweise die für die Alkali-Kieselsäure-Reaktion (AKR) interessanten Natriumkonzentrationen bestimmt und hinsichtlich ihrer Verteilung aufgelöst werden. Es lassen sich Natriumgehalte, welche sich in der Gesteinskörung befinden, separat von denen der Betonmatrix bestimmen. Der vorliegende Artikel befasst sich mit den Vor- und Nachteilen von LIBS als alternative Methode für die chemische Analyse von Baustoffen. Anhand von Beispielen aus der Praxis wird der derzeitige Stand der Technik dargestellt und ein Vergleich mit etablierten Messmethoden vorgenommen. Compared to conventional methods the Laser Induced Breakdown Spectroscopy (LIBS) provides significant advantages for analysis of heterogeneous, mineral building materials as e.g. concrete. Besides providing the possibility to quantify element concentrations and distributions in building materials, this technique enables also to differentiate concentrations within different phases of the material. It is possible to determine sodium concentrations and distribution directly, which e.g. is important when regarding Alkali-Silica-Reaction (ASR). Sodium contents provided by the aggregates can be distinguished from those provided by the concrete matrix. The present article is concerned with the advantages and disadvantages of LIBS as alternative method for chemical analysis of building materials. On the basis of samples from practice the current state of the art is shown and different measurement techniques will be compared.
The laser-induced breakdown spectroscopy (LIBS) is a fast method to provide multi-elemental analysis of any sample. At the Federal Institute for Materials Research and Testing (BAM) the LIBS technique is applied on building materials to measure ingress profiles of harmful species like chloride and alkalis. The ingress depth and the quantitative amount is important for the evaluation of the potential for damage processes like the alkali-silica reaction or chloride-induced corrosion. Concrete as an example is a highly heterogeneous material with 1/7 cement (major component CaO) and 6/7 aggregates (SiO2) with different grain sizes. Due to a scanning procedure a two dimensional element distribution of a concrete surface can be measured. In order to have an automated Separation method to evaluate heterogeneous materials, different cluster algorithm have been tested. Best results have been achieved with the Expectation-Maximization-Algorithm (EM-Algorithm).
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.
Bei der Erhaltung von Stahlbetonbauwerken ist der Chloridgehalt im Beton ein wichtiger Parameter zur Festlegung geeigneter Instandsetzungsmaßnahmen. Die bisher etablierten Verfahren basieren auf der nasschemischen Analyse einer Probe, Bohrmehl oder aufgemahlener Segmente eines Bohrkerns. Das Verfahren liefert einen Chloridgehalt je Tiefensegment, was mit einer starken Homogenisierung der Probe einhergeht, wodurch detaillierte Informationen zu Chloridunterschieden im Millimeterbereich verloren gehen. Eine alternative Methode ist die laserinduzierte Plasmaspektroskopie (LIBS), die nicht nur die quantitative ortsaufgelöste Bestimmung des Chloridgehalts im Bezug zur Zementmasse ermöglicht, sondern auch simultan detaillierte Informationen über die Verteilung vieler anderer chemischer Elemente liefert. Die räumliche Auflösung liegt in der Regel im Bereich von einigen Millimetern, kann aber bei Bedarf auf 0,1 mm oder weniger erhöht werden. Das neue Merkblatt B14 „Quantifizierung von Chlorid in Beton mit der laserinduzierten Plasmaspektroskopie (LIBS)“ der Deutschen Gesellschaft für Zerstörungsfreie Prüfungen (DGZfP) regelt und vereinheitlicht erstmals die zuverlässige und reproduzierbare Ermittlung des Chloridgehalts mit LIBS. In diesem Beitrag wird das Merkblatt vorgestellt und anhand praktischer Anwendungsbeispiele das Potenzial von LIBS für Fragestellungen in der Betonerhaltung verdeutlicht.
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.
The information about the chemical composition of coal is of great interest during mining, sorting and processing. Due to great variations of the soil layers the quality of coal suffers great fluctuations during mining because of adjoining rocks [1-6]. To provide on-site analysis of coal the application of LIBS as a multi-element method has been tested. Therefore different qualities of coal have been chemically analyzed to get reference values for the water content as well as for the major (carbon) and minor components (ash = Ca, Mg, S, Si). For the LIBS analysis a system using a low energy laser with a wavelength of 1064 nm, pulse energy of 3 mJ, pulse length of 1.5 ns and a repetition rate of 100 Hz have been used. A compact czerny turner spectrometer operating in the UV range (Δλ = 170 nm – 350 nm) have been applied. To provide quantitative concentrations different calibration curves have been evaluated using chemometrics. The system has been validated using internal cross-validation as well as an external set of samples. For the evaluation of the method different figures of merit will be presented. After applying LIBS for coal analysis in the laboratory a LIBS system for the on-site analysis has been tested during the mining process.
In civil engineering the information about the quantitative ingress of harmful species like Cl⁻, Na⁺ and SO²⁻₄ is of great interest to evaluate the remaining life time of structures. These species are triggering different damage processes like the alkali-silica reaction (ASR) or the chloride-induced corrosion of the reinforcement. For the evaluation of the heterogeneous concrete it is necessary to discriminate between the different phases mainly cement matrix and aggregates. The transport processes are only proceeding in the cement matrix therefore the measured concentrations should be regarded to the cement content. For the 2D evaluation of element distributions different multivariate cluster-algorithms like k-means and Expectation-Maximization-algorithm (EM-algorithm) have been tested. The methods are compared and different figures of merit will be presented. After phase separation non-relevant information of the aggregates can be excluded. The ingress of harmful species is then quantified using chemometrics. Due to concrete cores from a parking deck the methods have been validated and verified with standard methods of wet-chemistry.
Reinforced concrete structures like bridges and parking decks are subject of corrosion of the reinforcement if chlorides from thawing salts or sea water penetrating into the concrete. For the determination of the expected life time normally samples are taken by borehole cuts or drilling of cores. These samples are taken to the lab and standard chemical methods are used for evaluation. As an alternative a fast and reliable onsite technique which gives results just in time is needed. In cooperation with industrial partners and BAM a mobile LIBS system for the on-site application of LIBS in civil engineering has been developed. The mobile system uses a low energy laser with a pulse energy of < 3 mJ, a wavelength of 1064 nm, a pulse width of 1.5 ns, a repetition rate of 100 Hz and a NIR-spectrometer in combination with a scanner to map areas of up 170 mm x 140 mm. In this work the correlation between exposures of the concrete surface due to chlorides and their ingress profiles will be shown. Quantitative ingress profiles are evaluated and compared with standard analysis.
The Laser-Induced Breakdown Spectroscopy (LIBS) is a laser spectroscopic method which allows a time efficient, minor-destructive, chemical analysis of materials. In principle all elements on the periodic table can be simultaneously analysed by using LIBS, regardless of the state of aggregation. LIBS offers numerous applications in the field of civil engineering; most importantly the analysis of building materials. This work will focus on the evaluation of concrete structures and harmful substances which can penetrate the concrete. A variety of information can be collected through LIBS. Determining the concentration of harmful substances like chloride, sodium or sulphur, the examination of the carbonation depth and the distinction between varying layers of materials (e.g. aggregates, cement paste, metals, etc.) are possible applications. All this information can be provided through one LIBS measurement in the form of a high resolution 2D element map, with resolutions up to 0.1 mm x 0.1 mm. To scan a concrete surface only an optical access is needed. To create a depth profile of an intruding substance the extraction of a drill core is necessary. Onsite measurements via LIBS can be conducted by using a mobile version of the LIBS system. Through using calibration curves LIBS allows not only the qualitative but also quantitative analysis of element concentrations. All those prospects make LIBS a trendsetting method to secure the integrity of infrastructures in a sustainable manner. A variety of examples which show the performance and results of LIBS analysis will be presented.
