TY - JOUR A1 - Völker, Tobias A1 - Millar, Steven A1 - Strangfeld, Christoph A1 - Wilsch, Gerd T1 - Identification of type of cement through laser-induced breakdown spectroscopy JF - Construction and Building Materials N2 - The composition of concrete determines its resistance to various degradation mechanisms such as ingress of ions, carbonation or reinforcement corrosion. Knowledge of the composition of the hardened concrete is therefore helpful to assess the remaining service life of an existing structure or evaluate the damage observed during inspections. For example, for most existing concrete structures the type of cement originally used is not known and must therefore be determined afterwards. This paper presents a preliminary study on the application of laser-induced breakdown spectroscopy (LIBS) to identify the type of cement. For this purpose, ten different types of cement were investigated. For every type, three cement paste prisms were produced: (i) prisms dried, ground and pressed into tablets, (ii) prisms dried and (iii) prisms untreated. LIBS measurements were performed with a diode-pumped low energy laser (1064 nm, 3 mJ, 1.5 ns, 100 Hz) in combination with two compact spectrometers which cover the UV and NIR spectral range. A reduced subset of spectral features was used to build a classification model based on linear discriminant analysis. The results show that the classification of homogenized pressed cement powder samples provides a high accuracy, however, factors such as a different sample matrix and moisture content can affect the accuracy of the classification. The study demonstrates that LIBS is a promising tool to identify the type of cement. KW - Spectroscopy KW - LIBS KW - Cement KW - Classification KW - Identification PY - 2020 DO - https://doi.org/10.1016/j.conbuildmat.2020.120345 VL - 258 SP - 120345 PB - Elsevier Ltd. AN - OPUS4-51157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Wilsch, Gerd A1 - Gornushkin, Igor B. A1 - Kratochvilo, L. A1 - Pořízka, P. A1 - Kaiser, J. A1 - Millar, S. A1 - et al., T1 - Interlaboratory comparison for quantitative chlorine analysis in cement pastes with laser induced breakdown spectroscopy JF - Spectrochimica Acta Part B N2 - Concrete structures experience severe damage during service, for example due to pitting corrosion of rebars caused by the ingress of chlorine (Cl) into the porous concrete structure. The ingress can be monitored using laser-induced breakdown spectroscopy (LIBS), a recently introduced civil engineering technique used to detect Cl in concrete structures in addition to conventional wet chemistry methods. The key advantages of LIBS are high spatial resolution, which is important when analyzing heterogeneous concrete samples, as well as the almost complete absence of sample preparation. To assess LIBS as a reliable analytical method, its accuracy and robustness must be carefully tested. This paper presents the results of an interlaboratory comparison on the analysis of Cl in cement paste samples conducted by 12 laboratories in 10 countries. Two sets of samples were prepared with Cl content ranging from 0.06 to 1.95 wt% in the training set and 0.23–1.51 wt% in the test set, with additional variations in the type of cement and Cl source (salt type). The overall result shows that LIBS is suitable for the quantification of the studied samples: the average relative error was generally below 15%. The results demonstrate the true status quo of the LIBS method for this type of analysis, given that the laboratories were not instructed on how to perform the analysis or how to process the data. KW - LIBS KW - Interlaboratory comparison KW - Round robin test KW - Cement KW - Chlorine PY - 2023 DO - https://doi.org/10.1016/j.sab.2023.106632 SN - 0584-8547 VL - 202 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-57102 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weise, Frank A1 - Millar, Steven A1 - Wilsch, Gerd T1 - Analyse des Tausalzeintrags in Fahrbahndeckenbetone mit neuartiger Prüftechnik T1 - Analysis of De-icing Salt in Concrete Pavement with a new type of Test Technology JF - Beton- und Stahlbetonbau N2 - In den letzten Jahren sind im deutschen Bundesautobahnnetz vermehrt AKR-Schäden an Betonfahrbahndecken aufgetreten. Ursächlich hierfür ist die Verwendung alkaliempfindlicher Gesteinskörnung. Dies führt bei gleichzeitiger Anwesenheit von Wasser infolge der Exposition der Fahrbahndecke und des alkalischen Milieus durch den Einsatz alkalireicher Portlandzemente bei der Betonherstellung zu einer Alkali-Kieselsäure-Reaktion (AKR). Zusätzlich wird der AKR-Schädigungsprozess in Betonfahrbahndecken durch den externen Tausalzeintrag (primär NaCl) im Winter begünstigt. Vor diesem Hintergrund kommt der Ermittlung des Tausalzeintrags in den Fahrbahndeckenbeton eine große Bedeutung zu. Die Analyse des Tausalzeintrags erfolgte bisher ausschließlich nasschemisch an gemahlenen Bohrkernsegmenten. Nachteilig sind hierbei der relativ hohe prüftechnische Aufwand und die eingeschränkte Ortsauflösung. Der alternative Einsatz von LIBS (Laser-induced breakdown spectroscopy) eröffnet in diesem Kontext neue Möglichkeiten. So wird in diesem Beitrag anhand von Bohrkernen aus einem repräsentativen AKR-geschädigten BAB-Abschnitt exemplarisch die Vorgehensweise bei der LIBS-Analyse zur Ermittlung der Na- und Cl-Verteilung an vertikalen Schnittflächen von Bohrkernen aufgezeigt. Da der Tausalzeintrag primär über den Zementstein erfolgt, wurde der verfälschende Na-Grundgehalt der Gesteinskörnung mittels eines Ausschlusskriteriums (Ca-Gehalt) eliminiert. Vergleichend durchgeführte Cl-Mappings mit Mikroröntgenfluoreszenzanalyse sowie nasschemische Analysen belegen die Güte der durchgeführten LIBS-Messungen. Allerdings bedarf es bei der quantitativen Ermittlung des Natriumgehaltes in der Betonfahrbahndecke noch weitergehender Untersuchungen. N2 - Analysis of the intrusion of de-icing salt into concrete pavements by a novel test method In recent years the German motorway network has seen an increase in the occurrence of damage in concrete pavements. This has been caused by the use of alkali-sensitive aggregates. Given the exposure of the concrete pavement to water and the alkaline environment caused by the use of Portland cement during concrete mixing, this environment can lead to an alkali-silica reaction (ASR) process. This ASR-damage process in concrete pavements is further exacerbated by the external application of de-icing salt in winter. Against this background, the evaluation of the intrusion of de-icing salt becomes of great importance. Until now, the analysis of the intrusion of de-icing salt was carried out in a wet-chemistry process on finely ground segments of drilling cores. The disadvantages of this method are the relatively arduous testing process and the limited depth resolution. The alternative application of LIBS (laser-induced breakdown spectroscopy) offers new possibilities in this context. In this paper, the procedure for the LIBS analysis of sodium and chloride distribution on vertical cut surfaces of drilling cores taken from representative ASR-damaged concrete pavements is presented. Because the intrusion of de-icing salt takes place primarily in the cement matrix, the distorting effect of the sodium content in the aggregates was eliminated by an exclusion criteria (namely, the calcium content). The comparable chloride mappings by micro X-ray fluorescence spectroscopy and wet-chemical analysis confirm the quality of the LIBS measurements. However, additional investigations are necessary for the quantitative analysis of sodium content in concrete pavements. KW - Betonfahrbahndecke KW - Alkali-Kieselsäure-Reaktion KW - Tausalz KW - LIBS KW - MRFA KW - Nasschemie KW - ZfP PY - 2018 DO - https://doi.org/10.1002/best.201800033 SN - 0005-9900 SN - 1437-1006 VL - 113 IS - 9 SP - 656 EP - 666 PB - Wilhelm Ernst & Sohn, Verlag für Architektur und technische Wissenschaften GmbH & Co. KG CY - Berlin AN - OPUS4-46171 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weritz, Friederike A1 - Schaurich, Dieter A1 - Taffe, Alexander A1 - Wilsch, Gerd T1 - Effect of heterogeneity on the quantitative determination of trace elements in concrete JF - Analytical and bioanalytical chemistry N2 - Laser-induced breakdown spectroscopy has been used for quantitative measurement of trace elements, e.g. sulfur and chlorine, in concrete. Chloride and sulfate ions have a large effect on the durability of concrete structures, and quantitative measurement is important for condition assessment and quality assurance. Concrete is a highly heterogeneous material in composition and grain-size distribution, i.e. the spatial distribution of elements. Calibration plots were determined by use of laboratory-made reference samples consisting of pressings of cement powder, hydrated cement, cement mortar, and concrete, in which the heterogeneity of the material is increasing because of the aggregates. Coarse aggregate and cement paste are distinguishable by the intensity of the Ca spectral lines. More advanced evaluation is necessary to account for the effect of the fine aggregate. The three series of reference samples enable systematic study of the effects of heterogeneity on spectral intensity, signal fluctuation, uncertainty, and limits of detection. Spatially resolved measurements and many spectra enable statistical evaluation of the data. The heterogeneity has an effect on measurement of the sulfur and chlorine content, because both occur mainly in the cement matrix. Critical chloride concentrations are approximately 0.04% (m/m). The chlorine spectral line at 837.6 nm is evaluated. The natural sulfur content of concrete is approximately 0.1% (m/m). The spectral line at 921.3 nm is evaluated. One future application may be simultaneous determination of the amount of damaging trace elements and the cement content of the concrete. KW - LIBS KW - Heterogeneity KW - Concrete KW - Chlorine KW - Sulfur PY - 2006 DO - https://doi.org/10.1007/s00216-006-0362-0 SN - 1618-2642 SN - 1618-2650 VL - 385 IS - 2 SP - 248 EP - 255 PB - Springer CY - Berlin AN - OPUS4-12206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weritz, Friederike A1 - Schaurich, Dieter A1 - Wilsch, Gerd T1 - Detector comparison for sulfur and chlorine detection with laser induced breakdown spectroscopy in the near-infrared-region JF - Spectrochimica acta B N2 - Laser-induced breakdown spectroscopy has been employed for the investigation of the sulfur and chlorine content of building materials. Both, chloride and sulfate ions are major damaging species affecting the stability and lifetime of a structure. Chlorine and sulfur are mostly detected in the VUV and the NIR. In case of building materials the main elements like calcium or iron have many strong spectral lines over the whole spectral range, so that trace elements can only be detected in spectral windows unaffected from these lines. With regard to a preferably simply, robust against dust and vibrations and portable setup only the NIR spectral features are used for civil engineering applications. Most detectors, mainly CCD cameras have rapidly decreasing quantum efficiency in the NIR. Also the quantum efficiency of the photocathode of CCD-Detectors with image intensifier is decreasing in the NIR. Different CCD-detectors were tested with respect to high quantum efficiency and high dynamic range, which is necessary for simultaneous detection of weak spectral lines from trace elements and intense spectral lines from main elements. The measurements are made on reference samples consisting of cement, hydrated cement, cement mortar and concrete with well-defined amounts of the trace elements. Experimental conditions are chosen for an optimum intensity of the trace element spectral lines. The detector systems are compared by limit of detections and the signal to noise ratio. KW - LIBS KW - Sulfur KW - Chlorine KW - NIR KW - Building materials KW - Concrete KW - Detector comparison PY - 2007 DO - https://doi.org/10.1016/j.sab.2007.10.017 SN - 0584-8547 SN - 0038-6987 VL - 62 IS - 12 SP - 1504 EP - 1511 PB - Elsevier CY - Amsterdam AN - OPUS4-16507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiggenhauser, Herbert A1 - Taffe, Alexander T1 - Garant für gute Qualität, Werkzeug für fundierte Analysen - Was leisten zerstörungsfreie Prüfverfahren im Bauwesen? JF - Deutsches Ingenieur-Blatt KW - Zerstörungsfreie Prüfung im Bauwesen KW - ZfPBau KW - Übersichtsartikel KW - Bildgebende Darstellung KW - Baustellenscanner KW - LIBS KW - Validierung PY - 2006 SN - 0946-2422 IS - 7/8 SP - 22 EP - 28 PB - Bundesingenieurkammer CY - Berlin AN - OPUS4-12648 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yuan, Huan A1 - Gornushkin, Igor B. A1 - Gojani, Ardian A1 - Wang, X. H. A1 - Rong, Ming Zhe T1 - Laser-induced plasma imaging for low-pressure detection JF - Optics Express N2 - A novel technique based on laser induced plasma imaging is proposed to measure residual pressure in sealed containers with transparent walls, e.g. high voltage vacuum interrupter in this paper. The images of plasma plumes induced on a copper target at pressure of ambient air between 10−2Pa and 105Pa were acquired at delay times of 200ns, 400ns, 600ns and 800ns. All the plasma images at specific pressures and delay times showed a good repeatability. It was found that ambient gas pressure significantly affects plasma shape, plasma integral intensities and expansion dynamics. A subsection characteristic method was proposed to extract pressure values from plasma images. The method employed three metrics for identification of high, intermediate and low pressures: the distance between the target and plume center, the integral intensity of the plume, and the lateral size of the plume, correspondingly. The accuracy of the method was estimated to be within 15% of nominal values in the entire pressure range between 10−2Pa and 105Pa. The pressure values can be easily extracted from plasma images in the whole pressure range, thus making laser induced plasma imaging a promising technique for gauge-free pressure detection. KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2018 DO - https://doi.org/10.1364/OE.26.015962 SN - 1094-4087 VL - 26 IS - 12 SP - 15962 EP - 15971 PB - Optical Society of America under the terms of the OSA Open Access Publishing Agreement AN - OPUS4-45219 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -