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High-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GF-MAS) was employed for determining adsorbable organic chlorine (AOCl) in water. Organic chlorine was indirectly quantified by monitoring the molecular absorption of the transient aluminum monochloride molecule (AlCl) around a wavelength of 261.42 nm in a graphite furnace. An aluminum solution was used as the molecularforming modifier. A zirconium coated graphite furnace, as well as Sr and Ag solutions were applied as modifiers for a maximal enhancement of the absorption signal. The pyrolysis and vaporization temperatures were 600 °C and 2300 °C, respectively. Non-spectral interferences were observed with F, Br, and I at concentrations higher than 6 mg L-1, 50 mg L-1, and 100 mg L-1, respectively. Calibration curves with NaCl, 4-chlorophenol, and trichlorophenol present the same slope and dynamic range, which indicates the chlorine atom specificity of the method. This method was evaluated and validated using synthetic water samples, following the current standard DIN EN ISO 9562:2004 for the determination of the sum parameter adsorbable organic halides (AOX) for water quality. These samples contain 4-chlorophenol as the chlorinated organic standard in an inorganic chloride matrix. Prior to analysis, organic chlorine was extracted from the inorganic matrix via solid-phase extraction with a recovery rate >95%. There were no statistically significant differences observed between measured and known values and for a t-test a confidence level of 95% was achieved. The limits of detection and characteristic mass were found to be 48 and 22 pg, respectively. The calibration curve was linear in the range 0.1–2.5 ng with a correlation coefficient R2 = 0.9986.
Electrochemical noise measurements on unalloyed steel in chloride-containing alkaline environment
(2007)
The investigations discussed in this paper aim to clarify whether electrochemical noise measurements (ENM) are capable for application in concrete and mortar, particularly with regard to pitting initiation in such environment. For these purposes, the results of several different test series are compared and discussed. Based on investigations on passivity and pitting corrosion in alkaline solutions with different chloride contents further results in cement paste, mortar and concrete are evaluated.
Although the complex changes at the steel-concrete interface due to cathodic polarisation are widely acknowledged to have a beneficial influence concerning the cathodic protection (CP) of steel in concrete, some questions concerning the repassivation of carbon steel in consequence of cathodic polarisation are still not satisfactorily clarified. In the recent literature, some indications are presented that repassivation occurs after a certain time of polarisation. Therefore, the investigations discussed in this paper aim to clarify, to what extent the re-passivation of carbon steel due to cathodic polarisation occurs, and if the ennoblement of OCP is a sufficient indication for repassivation. In a first step, the corrosion state of five nominal equal test specimens was determined by electrochemical impedance spectroscopy (EIS). After determining the initial corrosion state by evaluating the charge transfer resistance and the polarisation resistance, respectively, the specimens were polarised cathodically. Impedance data were recorded before, during and after polarisation. The impedance data were evaluated by equivalent circuit fitting with special attention to charge transfer resistances and the impact of diffusion on the corrosion and polarisation behaviour. The results indicate that the reduction of oxides and oxygen diffusion during cathodic polarisation has strong impact on the systems behaviour and that repassivation effects occur after switching off the polarisation current and during depolarisation, respectively.
LIBS is on the step from a laboratory application to on-site analysis. A validated mobile LIBS-system for on-site application on building materials is under development at BAM in cooperation with industrial partners (system developers and companies), who will use this technique for investigation on building structures like bridges and parking decks. The system is designed to measure the content of harmful species like chlorine, sulfur or alkalis, to give the engineer a tool for the estimation of the condition of concrete structures and for quality assurance during concrete repair work on-site. In these work results of on-site measurements on a chloride contaminated bridge are shown. Further work will focus on providing guidelines to establish LIBS as a standard procedure for chemical investigations of building materials.
LIBS is a complementary method to XRF and can detect all elements without the need for vacuum conditions. Automated systems are already commercially available capable of scanning surfaces with a resolution of up to 0.1 mm within a few minutes. In addition to possible applications in R&D, LIBS is also used for practical applications in building materials laboratories and even on-site.
In view of ageing infrastructure facilities, a reliable assessment of the condition of concrete structures is of increasing interest. For concrete structures, the ingress of potential harmful ions is affecting the serviceability and eventually structural performance. Pitting corrosion induced by penetrating chlorides is the dominant deterioration mechanism. Condition assessment based on frequently performed chloride profiling can be useful to identify the extent and evolution of chloride ingress. This could prove to be more economical than extensive repairs, especially for important infrastructure facilities.
Currently the most common procedure for determining the chloride content is wet chemical analysis with standard resolution of 10 mm. The heterogeneity is not considered. LIBS is an economical alternative for determining the chloride content at depth intervals of 1 mm or less. It provides 2D distributions of multiple elements and can locate spots with higher concentrations. The results are directly correlated to the mass of binder and can also be performed on-site with a mobile LIBS-System.
The application of a LIBS-system is presented. Calibration is required for quantitative analysis. Concrete cores were drilled, sliced and analyzed to determine the 2D-distribution of harmful elements. By comparing the chloride ingress and the carbonation, the interaction of both processes can be visualized in a measurement that takes less than 10 minutes for a 50 mm x 100 mm drill core.
A leaflet on the use of LIBS for the chloride ingress assessment has been completed.
Laser-induced breakdown spectroscopy (LIBS) is a combination of plasma generation on the sample surface by a high power laser pulse and optical emission spectroscopy (OES). It is a direct measurement method without an extensive sample preparation. Concrete is a multi phase system. With LIBS it is possible to distinguish the different phases and based on that to correlate the chloride content to the cement mass. This is done by scanning the surface with a resolution of up to 0.1 mm. The high measurement frequency of 100 Hz or even higher allows the in-situ visualization of the chloride content over the measured area. With a calibration a quantification of chloride concentration is possible. As an example the LIBS measurement on a 50 mm by 70 mm area with a resolution of 0.5 mm and the visualization of the chloride distribution takes only 10 minutes. Additionally it is possible to evaluate the carbonation depth from the same measurement. Examples of practical application to determine the chloride-to-cement-content on concrete samples are presented. The possibilities and the limitations of LIBS are discussed.
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.