Addressing the need for standardization of test methods for self-healing concrete: an inter-laboratory study on concrete with macrocapsules.

Development and commercialization of self-healing concrete is hampered due to a lack of standardized test methods. Six inter-laboratory testing programs are being executed by the EU COST action SARCOS, each focusing on test methods for a specific self-healing technique. This paper reports on the comparison of tests for mortar and concrete specimens with polyurethane encapsulated in glass macrocapsules. First, the pre-cracking method was analysed: mortar specimens were cracked in a three-point bending test followed by an active crack width control technique to restrain the crack width up to a predefined value, while the concrete specimens were cracked in a three-point bending setup with a displacement-controlled loading system. Microscopic measurements showed that with the application of the active control technique almost all crack widths were within a narrow predefined range. Conversely, for the concrete specimens the variation on the crack width was higher. After pre-cracking, the self-healing effect was characterized via durability tests: the mortar specimens were tested in a water permeability test and the spread of the healing agent on the crack surfaces was determined, while the concrete specimens were subjected to two capillary water absorption tests, executed with a different type of waterproofing applied on the zone around the crack. The quality of the waterproofing was found to be important, as different results were obtained in each absorption test. For the permeability test, 4 out of 6 labs obtained a comparable flow rate for the reference specimens, yet all 6 labs obtained comparable sealing efficiencies, highlighting the potential for further standardization.

Self-Healing of Cracks in Cementitious Materials as a Method of Improving the Durability of Pre-Stressed Concrete Railway Sleepers.

The article presents research results regarding the possibility of modifying pre-stressed concrete railway sleepers to improve their durability. The cracks that appear in these elements are one of the reasons for shortening the period of safe use. They do not have a significant impact on the load-bearing capacity of these elements, but on their durability. The resulting scratches become an easy way for the external environment to migrate inside the element, including the reinforcement area. Despite efforts to eliminate the possibility of cracking, this phenomenon still occurs in railway sleepers. In order to reduce the negative effects of cracking the cement matrix, a technology for modifying a prefabricated concrete element with resin-filled tubes towards its autonomous self-healing was developed and tested. The tests were divided into three stages, including laboratory tests carried out on cement mortar beams, semi-technical tests carried out on reinforced concrete beams, and industrial tests carried out on pre-stressed concrete and prefabricated railway sleepers. All research conducted on a laboratory and semi-technical scale, preceding the target stage, was intended to ultimately enable the development of tube application technology on an industrial scale while verifying the effectiveness of self-healing at the laboratory level. The use of self-healing cementitious materials potentially reduces the negative effects of cracking railway sleepers, as shown by observations conducted during the research.

Evaluation of Methodologies for Assessing Self-Healing Performance of Concrete with Mineral Expansive Agents: An Interlaboratory Study.

Self-healing concrete has the potential to optimise traditional design approaches; however, commercial uptake requires the ability to harmonize against standardized frameworks. Within EU SARCOS COST Action, different interlaboratory tests were executed on different self-healing techniques. This paper reports on the evaluation of the effectiveness of proposed experimental methodologies suited for self-healing concrete with expansive mineral additions. Concrete prisms and discs with MgO-based healing agents were produced and precracked. Water absorption and water flow tests were executed over a healing period spanning 6 months to assess the sealing efficiency, and the crack width reduction with time was monitored. High variability was reported for both reference (REF) and healing-addition (ADD) series affecting the reproducibility of cracking. However, within each lab, the crack width creation was repeatable. ADD reported larger crack widths. The latter influenced the observed healing making direct comparisons across labs prone to errors. Water absorption tests highlighted were susceptible to application errors. Concurrently, the potential of water flow tests as a facile method for assessment of healing performance was shown across all labs. Overall, the importance of repeatability and reproducibility of testing methods is highlighted in providing a sound basis for incorporation of self-healing concepts in practical applications.

Selection of Method of Chemical Analysis in Measuring the Salinity of Mineral Materials.

The article deals with the issue of salt content in brick buildings, which plays an important role in the assessment of the technical condition, in particular of historic buildings. A question has been asked about the selection of the best research method to determine the salinity of mineral materials. To obtain the answer, the authors conducted some tests on ceramic bricks salted with seven types of salt solutions. Research methods such as: spectrophotometry (UV), ion chromatography (High Performance Liquid Chromatography (HPLC)), X-Ray Fluorescence Spectrometry (XRF) and Energy-Dispersive X-Ray Spectroscopy (EDS) were compared. The above methods belong to two groups: the first is based on aqueous extracts and allows the determination of water-soluble salts, and the second concerns testing directly on the sample so that insoluble salts can also be determined. The results tests indicate that the methods based on solid phases (XRF and EDS) give higher salinity values than those based on aqueous extracts (HPLC and UV). The results were also analysed with regard to the type of salt. Larger differences are observed for sulphate salts while chloride salts are characterised by smaller differences. On this basis, it is concluded that the salt content of the material is best assessed using tests that make it possible to recognise the salt in question and its quantity.

Durability of PS-Polyurethane Dedicated for Composite Strengthening Applications in Masonry and Concrete Structures.

Polyurethane flexible joints (PUFJ) and fiber reinforced polyurethanes (FRPU) have shown great potential in the repair and protection of masonry and concrete structures. However, some questions have been raised about the durability of such solutions. The accelerated weathering and thermal stability tests carried out so far have shown the mechanical stability of PS-polyurethane in temperatures up to 100 °C and some UV-induced surface degradation. The paper reports the results from tensile tests of PS-polyurethane, used in the technologies mentioned above after being subjected to aging in different corrosive factors, a thermal analysis of unaged polymer which consists of DSC-TGA and dilatometry studies, and SEM-microscopy observation of the specimens with the indication of the elemental composition (EDS). PS-polyurethane showed low sensitivity to weathering with exposition to UV-radiation, some reactiveness to aqueous environments of a different chemical nature, and resistivity to soil and freezing in both air and water. SEM observations indicated changes in the composition of mineral fillers as the main effect of immersion in different water solutions. DSC-TGA studies showed the thermal stability of PS-polyurethane up to 200 °C and degradation proceeding in five stages. Dilatometry studies revealed that the first-degree thermal degradation over 200 °C causes a serious loss of mechanical properties.

Forms of Damage of Bricks Subjected to Cyclic Freezing and Thawing in Actual Conditions.

The paper presents the characteristics of damage of bricks in masonry structures of significant historical value as a result of cyclic freezing and thawing. Based on extensive investigation, which included macroscopic description, determination of compressive strength and tensile strength, determination of the mineral composition, scanning microscopy observation and determination of the porosity structure of bricks, three forms of frost damage were distinguished, termed as powdering, flaking and cracking. Bricks were collected from existing historical buildings 70 years after their construction. It was observed that the particular form of frost damage of bricks is highly correlated with the structure of porosity. Additional factors affecting the form of frost destruction are the strength of the material, its mineral composition and the spatial arrangement of the texture elements. Taking the above into account, it is possible to evaluate frost resistance of bricks and specify the form of damage. Predicting frost resistance and forms of damage based on low-destructive methods using small samples is the expected solution in the case of heritage facilities.

Factors Determining the Biodiversity of Halophilic Microorganisms on Historic Masonry Buildings.

The aim of the present study was to obtain insights into the relationship between the chemical (salt content and pH) and physico-mechanical (humidity and compressive strength) properties of mineral-based materials from historic buildings with salt efflorescence and the growth and biodiversity of halophilic microorganisms. Samples were mainly characterized by pH 6.5-8.5 and a moisture content of between 0.12 and 3.3%. Significant variations were also found in the salt content (sulfates, chlorides, and nitrates) of the materials. An SEM/EDS analysis of material surfaces revealed the presence of halite, calcite, gypsum, sodium sulfate, and potassium-sodium sulfate. Culture-dependent and culture-independent (clone library construction) approaches were both applied to detect halophilic microorganisms. Results derived from culturable methods and the materials analysis revealed a correlation between the total halophile count and pH value as well as sulfate content. A correlation was not observed between the concentration of chlorides or nitrates and the number of halophilic microorganisms. The materials studied were inhabited by the culturable halophilic bacteria Halobacillus sp., Virgibacillus sp., and Marinococcus sp. as well as the yeast Sterigmatomyces sp., which was isolated for the first time from mineral materials. Culture-independent techniques revealed the following bacterial species: Salinibacterium, Salinisphaera, Rubrobacter, Rubricoccus, Halomonas, Halorhodospira, Solirubrobacter, Salinicoccus, and Salinibacter. Biodiversity was the highest in materials with high or moderate salinity.

Untargeted Metabolomics Approach in Halophiles: Understanding the Biodeterioration Process of Building Materials.

The aim of the study was to explore the halophile metabolome in building materials using untargeted metabolomics which allows for broad metabolome coverage. For this reason, we used high-performance liquid chromatography interfaced to high-resolution mass spectrometry (HPLC/HRMS). As an alternative to standard microscopy techniques, we introduced pioneering Coherent Anti-stokes Raman Scattering Microscopy (CARS) to non-invasively visualize microbial cells. Brick samples saturated with salt solution (KCl, NaCl (two salinity levels), MgSO4, Mg(NO3)2), were inoculated with the mixture of preselected halophilic microorganisms, i.e., bacteria: Halobacillus styriensis, Halobacillus naozhouensis, Halobacillus hunanensis, Staphylococcus succinus, Marinococcus halophilus, Virgibacillus halodenitryficans, and yeast: Sterigmatomyces halophilus and stored at 28°C and 80% relative humidity for a year. Metabolites were extracted directly from the brick samples and measured via HPLC/HRMS in both positive and negative ion modes. Overall, untargeted metabolomics allowed for discovering the interactions of halophilic microorganisms with buildings materials which together with CARS microscopy enabled us to elucidate the biodeterioration process caused by halophiles. We observed that halophile metabolome was differently affected by different salt solutions. Furthermore, we found indications for haloadaptive strategies and degradation of brick samples due to microbial pigment production as a salt stress response. Finally, we detected changes in lipid content related to changes in the structure of phospholipid bilayers and membrane fluidity.