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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.
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.
One of the most common causes of damage is the ingress of harmful ions into the concrete, which can lead to deterioration processes and affect structural performance. Therefore, the increasingly aging infrastructure is regularly inspected to assess durability. Regular chemical analysis can be useful to determine the extent and evolution of ion ingress and to intervene in a timely manner. This could prove more economical than extensive repairs for major damage, particularly for critical infrastructure. In addition to already established elemental analysis techniques in civil engineering such as potentiometric titration or X-ray fluorescence analysis, laser-induced breakdown spectroscopy (LIBS) can provide further important complementary information and benefits. The possibilities of LIBS are demonstrated using the example of a drill core taken from a parking garage.
In civil engineering, the investigation of existing infrastructure is of major importance for maintaining and ensuring stability of the structures. To ensure durability, uniform regulations and standards apply e.g. the European standard EN 206-1. In some countries, the EN-standard is supplemented by additional standards, as in Germany with DIN 1045-2. Here, specific application rules are described, e.g. for the cement type, to ensure the resistant to different exposures. Therefore, the knowledge of the materials originally used is important in assessing the condition of existing concrete structure. Unfortunately, these are often unknown and must be determined retrospectively. Therefore, we present the application of the laser-induced breakdown spectroscopy to distinguish between different types of cement. Spectral information’s are used to build a classification model. First, the accuracy of the classification is analyzed on ten pure laboratory cement samples. To investigate possible sources of error, the model was then applied to cement samples with different moisture content. The study shows that LIBS is a promising tool for distinguishing between cement types. For further industrial application, however, factors influencing the LIBS signal must be included to ensure a robust model.
Two calibration-free LIBS techniques are used for the quantitative analysis of synthetic cement samples: the CF-LIBS based on the Boltzmann plot method and the Monte Carlo (MC) LIBS based on the iterative spectrum fitting. In CF-LIBS, the inverse problem is solved, i.e. the elemental concentrations are determined by the reconstruction of plasma parameters from spectra. The MC-LIBS technique solves the direct problem by finding the highest correlation between the model-generated and experimental spectrum. The accuracy of both calibration-free LIBS methods suffers from factors such as inaccurately determined instrumental function, the deviation of experimental plasma from the mathematical model used, not taking into account the collection geometry and from the uncertainty of spectroscopic data. Therefore, the both calibration-free LIBS approaches are applied to synthetic spectra which perfectly suit the mathematical model of the method. This test yields the accuracy of both the approaches for the ideal case. In addition, the accuracy of both methods is investigated for non-isothermal plasma, because real laser-induced plasma often has high gradients in temperature. Both methods assume an isothermal plasma.
Sr isotope ratio analysis
(2023)
The presentations gives a short introduction into isotope analysis illustrated by examples from archaeology, food provenancing and metrology. In the main part current projects on the provenance determination of cement, the intercalibration of Mg isotope reference materials and the development of a new calibration approach for isotope measurements are presented.
Fresh cement paste is a suspension consisting of a hydraulic binder (cement), water, and numerous minor components – admixtures. Addition of admixtures aims at specific modification of properties of the fresh cement paste or hardened cementitious building material. Specific admixtures, so-called superplasticizers (SP), are used to improve the flowability of the fresh cement paste with reduced water content. The latter is the starting material for the high-strength concrete. Thus, SPs are essential for the ambitious construction projects.
However, uncontrollable retardation of the setting time in presence of SPs is occasionally observed. Obviously, SPs influence early products of the cement hydration leading to changes in the microstructure development. The hardening is thus delayed, and the quality of the resulting building material suffers. The mechanisms of the admixture action during the hydration process are still intensively investigated [1-7]. A detailed understanding of the admixture effects during the early hydration stage is the key to control and individual adjustment of the cement-based construction materials.
We use the unique combination of the wall-free sample holder and the time-resolved X-ray scattering analysis to achieve the full information about the hydrate phases formed under the influence of admixtures. We use ultrasonic levitator to start the cement hydration in levitated cement pellets [8, 9]. The sample levitation allows collection of the unimpaired information about cement hydrate phases. The most beneficial is the avoiding of the contributions of the sample holder material to the data signal.
We induce the cement hydration by adding water to unhydrated Portland cement during the data acquisition. The full phase composition of the hydrating cementitious system can be gathered in situ using wide angle X-ray scattering (WAXS). During the hydration of cement both crystalline and amorphous hydrate phases are formed. WAXS data contain the information about crystalline phases behind the Bragg reflections, whereas the amorphous hydrates influence the appearance of the background. Application of the data analysis specific for crystalline or amorphous phases is needed. The data quantification by the Rietveld method allows to conclude about the changes of the phase amounts due to the presence of admixture. The calculation of the pair distribution functions allows analysis of the amorphous hydrates. Based on this information, the SP effects and the extent of their involvement into the ongoing reactions can be concluded. A detailed understanding of the complex cement hydration process is envisioned.
While today, engineers can choose from a wide range of rheology modifying admixtures, in some parts of the world, these are difficult to access, due to their complex processing. However, alternatives can be bio‐based polymers such as polysaccharides from various sources. These are easily accessible all over the world, do not demand for complicated processing, and typically they are more sustainable than many established materials, which are crude oil‐based.
The paper presents the effects of acacia gum, cassava starch and the gum of triumfetta pendrata A. Rich on the rheological performance of cementitious systems. It is shown that acacia gum can be as efficient as polycarboxylate based superplasticisers, cassava starch can reduce the yield stress slightly with little effect on the plastic viscosity, and the gum of triumfet ta pendrata A. Rich increases the thixotropy of cement pastes with plasticizing polymers significantly.
The African cement, concrete and construction business is growing at rapid pace. The cement sales are expected to grow rapidly until 2050. The number of newly built cement plants increases dramatically and in addition more cements are being imported from outside the continent, e.g. from Turkey, Pakistan, Indonesia, and China, driven by overcapacities in the countries of origin. This causes a high number of potentials and challenges at the same time. Newly built cement plants can operate directly at best technological state of the art and thus incorporate more sustainable technologies as well as produce new and more sustainable products such as cements blended with sustainable supplementary cementitious materials such as calcined clays, and industrial or agricultural by products. At the same time the new variety of binding agent as well as the international imports, which are driven by price considerations, make the cement market prone to quality scatter. This puts pressure on the quality control regulations and institutions to ensure safety of construction, healthy application, and environmental safety for the population. The paper presents possible solutions to build up the rapidly increasing African cement production more sustainably than in the rest of the world as well as the related challenges and obstacles that need to be overcome. Based on experiences with a series of pan-African cement testing laboratory proficiency schemes conclusions are made on technical, regulative and political level.