TY - CONF A1 - Millar, Steven A1 - Gottlieb, Cassian A1 - Wilsch, Gerd A1 - Günther, Tobias A1 - Völker, Tobias T1 - Chemische Zustandsanalyse von Stahlbetonbauwerken mit der laserinduzierten Plasmaspektroskopie (LIBS) N2 - 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. T2 - 9. Kolloquium Parkbauten CY - Esslingen, Germany DA - 04.02.2020 KW - LIBS KW - Chemische Analyse KW - Spektroskopie KW - Beton PY - 2020 UR - https://elibrary.narr.digital/article/99.125005/kpb202010305 SN - 2510-7763 VL - 9 IS - 1 SP - 305 EP - 319 AN - OPUS4-50615 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Millar, Steven A1 - Wilsch, Gerd A1 - Eichler, Thorsten A1 - Gottlieb, Cassian A1 - Wiggenhauser, Herbert T1 - Laser induced breakdown spectroscopy (LIBS) im Bauwesen - automatisierte Baustoffanalyse N2 - 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. KW - Chloride KW - Alkali-Kieselsäure-Reaktion KW - AKR KW - RFA KW - Elementanalyse KW - Natrium KW - Baustoffuntersuchungen KW - Titration KW - Carbonatisierung KW - Baustoffe KW - Dauerhaftigkeit KW - Lebensdauer KW - Messsysteme KW - Qualitätssicherung KW - Alkali-silica-reaction KW - XRF KW - Element analysis KW - Sodium KW - Building materials analysis KW - Potentiometric titration KW - Carbonation KW - Bauwerkserhaltung/Instandsetzung KW - Korrosion PY - 2015 DO - https://doi.org/10.1002/best.201500030 SN - 0005-9900 SN - 1437-1006 VL - 110 IS - 8 SP - 501 EP - 510 PB - Ernst CY - Berlin AN - OPUS4-34580 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Cluster algorithm for the evaluation of heterogeneous materials by LIBS N2 - 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). T2 - Chemometrics in analytical chemistry CY - Barcelona, Spain DA - 06.06.2016 KW - LIBS KW - Concrete KW - Multivariate analysis PY - 2016 AN - OPUS4-36471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Bohling, Christian A1 - Wilsch, Gerd T1 - New possibilities for concrete analysis 4.0 with the Laser-Induced Breakdown Spectroscopy (LIBS) N2 - 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. T2 - SMAR 2019 CY - Potsdam, Germany DA - 27.08.2019 KW - Damage KW - LIBS KW - Concrete KW - Mapping KW - Chlorine PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517282 UR - https://www.ndt.net/?id=24963 SN - 1435-4934 VL - 25 IS - 1 SP - 1 EP - 8 PB - NDT.net CY - Kirchwald AN - OPUS4-51728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Gottlieb, Cassian A1 - Kapteina, Gesa A1 - Wilsch, Gerd A1 - Millar, Steven A1 - Reichling, Kenji T1 - Neues DGZfP-Merkblatt B14: Quantifizierung von Chlorid in Beton mittels LIBS N2 - 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. KW - LIBS KW - Chlor KW - Chlorid KW - Beton KW - Bauwerksdiagnostik PY - 2024 DO - https://doi.org/10.1002/best.202400014 SP - 1 EP - 7 AN - OPUS4-60005 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd A1 - Gottlieb, Cassian A1 - Millar, Steven A1 - Wiggenhauser, Herbert T1 - Laser induced breakdown spectroscopy (LIBS) – automated 2D chemical analysis of concrete N2 - 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. T2 - NDE / NDT for Highway and Bridges: Structural Materials Technology CY - Portland, Oregon, USA DA - 29.08.2016 KW - LIBS KW - Concrete KW - Chloride KW - Chemical analysis PY - 2016 SN - 978-1-57117-392-8 SP - 155 EP - 160 PB - The American Society for Nondestructive Testing, Inc. CY - Columbus, OH 43228-0518, USA AN - OPUS4-37679 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - On-site carbon analysis of coal using a mobile LIBS system N2 - 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. T2 - 9th International Conference on Laser Induced Breakdown Spectroscopy (LIBS2016) CY - Chamonix, Switzerland DA - 12.09.2016 KW - LIBS KW - On-site LIBS KW - Coal PY - 2016 AN - OPUS4-37420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - 2D evaluation of heterogenous building materials using cluster algorithm N2 - 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. T2 - 9th International Conference on Laser Induced Breakdown Spectroscopy (LIBS2016) CY - Chamonix, France DA - 12.09.2016 KW - LIBS KW - Building materials KW - Heterogeneity KW - Clustering PY - 2016 AN - OPUS4-37421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Damage assessment of infrastructures using a mobile LIBS system N2 - 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. T2 - 9th International Conference on Laser Induced Breakdown Spectroscopy (LIBS2016) CY - Chamonix, France DA - 12.09.2016 KW - LIBS KW - Concrete KW - Mobile system KW - On-site analysis KW - Civil engineering PY - 2016 AN - OPUS4-37422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sankat, Nina A1 - Wilsch, Gerd A1 - Gottlieb, Cassian A1 - Millar, Steven T1 - Analysis of concrete structures using Laser-Induced Breakdown Spectroscopy N2 - 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. T2 - CoMS 2017 CY - Zadar, Croatia DA - 19.04.2017 KW - Testing method KW - Concrete KW - LIBS KW - Harmful substances PY - 2017 SN - 978-953-8168-04-8 VL - 1 SP - 334 EP - 340 AN - OPUS4-42630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd A1 - Gottlieb, Cassian A1 - Günther, Tobias A1 - Millar, Steven ED - Forde, Mike T1 - Application of laser induced breakdown spectroscopy N2 - 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. T2 - Structural Faults + Repair-2018 CY - Edinburgh, UK DA - 15.05.2018 KW - Sulphate KW - Chloride KW - Concrete KW - LIBS PY - 2018 SN - 0-947644-86-5 DO - https://doi.org/10.25084/sfr.2018.0030 SP - 1 EP - 7 PB - University of Edinburgh CY - Edinburgh AN - OPUS4-46947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Temporal evaluation and imaging of laser-induced plasmas on cement-based materials N2 - 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. T2 - Xth international conference on Laser-Induced Breakdown Spectroscopy CY - Atlanta, GA, USA DA - 21.10.2018 KW - LIBS KW - Concrete KW - Grain size PY - 2018 AN - OPUS4-46794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd A1 - Gottlieb, Cassian A1 - Günther, Tobias A1 - Völker, Tobias ED - Ludwig, H.-M. T1 - Schnelle quantitative Untersuchung von Elementverteilungen in Beton mittels LIBS N2 - Die Laserinduzierte Plasmaspektroskopie (engl.: Laser-induced Breakdown Spectroscopy, kurz: LIBS) ist eine Kombination aus Laserablation mittels eines energiereichen Laser-Pulses, der Erzeugung eines Plasmas auf der zu untersuchenden Oberfläche und dem quantitativen Nachweis der Elementzusammensetzung durch spektroskopische Untersuchung der vom Plasma emittierten Strahlung. Ein LIBS-Gerät liefert dem sachkundigen Planer Daten für die Bewertung des Ist-Zustandes von Bauwerken unserer Infrastruktur durch die zweidimensionale Erfassung von Elementverteilungen. Typische Anwendungen sind die Erfassung von Chlor, Schwefel, Kohlenstoff, Natrium, Kalium und Lithium in Beton oder als – Qualitätssicherung – der Nachweis der mit einem Marker versehenen Tiefenhydrophobierung. In Zusammenarbeit zwischen Industriepartnern und der BAM wurden ein Labor und ein mobiles LIBS-System für die Vor-Ort-Messungen entwickelt. Die Analyse erfolgt vollautomatisch. Die Ortsauflösung beträgt bis zu 0,1 mm x 0,1 mm. Es können Messflächen von 140 mm x 170 mm gescannt werden. Die Erstellung von 2D-Elementverteilungen im Beispiel unten benötigt weniger als 10 Minuten. T2 - ibausil - 20. Internationale Baustofftagung CY - Weimar, Germany DA - 12.09.2018 KW - LIPS KW - LIBS KW - Beton KW - Chlorid PY - 2018 SN - 978-3-00-059950-7 VL - 2 SP - 2380 EP - 2387 PB - F.A. Finger-Institut für Baustoffkunde, CY - Weimar AN - OPUS4-46779 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Günther, Tobias A1 - Wilsch, Gerd T1 - Impact of grain sizes on the quantitative concrete analysis using laser-induced breakdown spectroscopy N2 - 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). KW - LIBS KW - Concrete KW - Micro heterogeneity KW - Grain sizes PY - 2018 DO - https://doi.org/10.1016/j.sab.2018.02.004 SN - 0584-8547 SN - 0038-6987 VL - 142 SP - 74 EP - 84 PB - Elsevier AN - OPUS4-44595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Millar, Steven A1 - Gottlieb, Cassian A1 - Sankat, Nina A1 - Wilsch, Gerd A1 - Kruschwitz, Sabine T1 - Chlorine determination in cement-bound materials with Laser-induced Breakdown Spectroscopy (LIBS) – A review and validation N2 - 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]. KW - LIBS KW - Chlorine KW - Cement KW - Calibration KW - Validation PY - 2018 DO - https://doi.org/10.1016/j.sab.2018.05.015 SN - 0584-8547 VL - 147 IS - September SP - 1 EP - 8 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-46558 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Visualization of Ion Transport in Concrete T2 - 8th International Conference on Laser Induced Breakdown Spectroscopy, LIBS 2014 CY - Beijing, China DA - 2014-09-08 PY - 2014 AN - OPUS4-31402 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Mobile System for On-site Analysis of Building Materials T2 - 8th International Conference on Laser Induced Breakdown Spectroscopy, LIBS 2014 CY - Beijing, China DA - 2014-09-08 PY - 2014 AN - OPUS4-31404 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Millar, Steven A1 - Günther, Tobias A1 - Wilsch, Gerd T1 - Revealing hidden spectral information of chlorine and sulfur in data of a mobile Laser-induced Breakdown Spectroscopy system using chemometrics N2 - For the damage assessment of reinforced concrete structures the quantified ingress profiles of harmful species like chlorides, sulfates and alkali need to be determined. In order to provide on-site analysis of concrete a fast and reliable method is necessary. Low transition probabilities as well as the high ionization energies for chlorine and sulfur in the near-infrared range makes the detection of Cl I and S I in low concentrations a difficult task. For the on-site analysis a mobile LIBS-system (k = 1064 nm, Epulse ≤ 3 mJ, t = 1.5 ns) with an automated scanner has been developed at BAM. Weak chlorine and sulfur signal intensities do not allow classical univariate analysis for process data derived from the mobile system. In order to improve the analytical performance multivariate analysis like PLS-R will be presented in this work. A comparison to standard univariate analysis will be carried out and results covering important parameters like detection and quantification limits (LOD, LOQ) as well as processing variances will be discussed (Allegrini and Olivieri, 2014 [1]; Ostra et al., 2008 [2]). It will be shown that for the first time a low cost mobile system is capable of providing reproducible chlorine and sulfur analysis on concrete by using a low sensitive system in combination with multivariate evaluation. KW - LIBS KW - Chemometrics KW - Building materials PY - 2017 DO - https://doi.org/10.1016/j.sab.2017.04.001 SN - 0584-8547 VL - 132 SP - 43 EP - 49 PB - Elsevier B.V. AN - OPUS4-40066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - The challenges of on-site LIBS measurements on concrete structures T2 - 8th Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy (EMSLIBS) 2015 CY - Linz, Austria DA - 2015-09-14 PY - 2015 AN - OPUS4-34506 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Improvment of qualitative LIBS analysis for harmful species in building materials due to multivariate analysis T2 - 8th Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy (EMSLIBS) 2015 CY - Linz, Austria DA - 2015-09-14 PY - 2015 AN - OPUS4-34507 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd A1 - Eichler, Thorsten A1 - Millar, Steven A1 - Gottlieb, Cassian T1 - Laser induced breakdown spectroscopy (LIBS) - alternative to wet chemistry and micro-XRF N2 - The laser induced breakdown spectroscopy (LIBS) gives an alternative to the standard techniques for the direct investigation of a building material. It utilize a high energy pulsed laser beam for ablation and vaporization of a small amount of material, a plasma is formed and the plasma radiation is investigated using optical emission spectroscopy. Due to the principal all elements are detectable during one measurement. In combination with a translation stage or scanner system the heterogeneity of concrete is considered in the results. Thus an element concentration may be correlated to the cement content. After calibration with a set of reference samples quantitative results are obtained. The system is automated and allows rapid measurements and minimizes the possibility of errors. At BAM a laboratory LIBS system has been successful applied for the investigation of transport processes of different ions in building materials. The spatial resolution of the measurement may rich 100 μm and the frequency of the measurements is 100 Hz. The concentration of chlorine, sulfur, carbon, sodium, potassium, lithium and hydrogen where quantitatively determined. A mobile system for on-site analysis on bridges or parking decks is available. It is a tool for the estimation of the condition of concrete structures and for quality assurance during concrete repair work on-site. In these work an overview of the possibilities of LIBS for automated investigation of building materials are given. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - LIBS KW - Elemental analysis KW - Heterogeneity KW - Chlorides KW - Sulfates KW - Alkalis KW - Corrosion KW - ASR KW - Carbonation PY - 2015 SN - 1435-4934 SP - 1 EP - 5 AN - OPUS4-34676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -