Evaluation of vibrational spectroscopic techniques for consolidants’ penetration depth determination

Ropret, Polonca; Legan, Lea; Retko, Klara; Špec, Tanja; Pondelak, Andreja; Škrlep, Luka; Škapin, Andrijana Sever

doi:10.1016/j.culher.2016.07.004

Cited by 12 publications

(8 citation statements)

References 28 publications

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“…The formation of calcium carbonate starts after two minutes as shown by the presence of absorption peaks in the region between 1460 and 1415 cm −1 (asymmetric stretching mode υ 3 of carbonate ion), (Figure 1b) [15,25]. Furthermore, also a peak at 3645 cm −1 related to O-H stretching [26], [10] is present at the beginning of the reaction (Figure 1b). After six hours, the peak related to O-H stretching is no longer present and only peaks related to calcium carbonate are evident: 1480-1410, 1074 (symmetric stretching mode υ 1 of carbonate ion) and 864 cm −1 (out of plane bending mode υ 2 of carbonate ion) ( Figure 1c) [27].…”

Section: Study Of Carbonation Processmentioning

confidence: 94%

Calcium Ethoxide as Consolidant for Porous Limestones: Influence of the Solvent

et al. 2019

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Calcium ethoxide nanosuspension, a consolidating product developed during the European Nanomatch project, is here modified by adding two different solvents, 2-butanol and n-butylacetate, chosen for their different boiling points with respect to ethanol, the solvent employed in a previous work to dilute the original product. Fourier transform infrared spectroscopy (µFT-IR) was used to understand how the presence of these new solvents can influence the kinetics of the carbonation process and the pathway reaction. Furthermore, coatings derived from nanosuspensions were maintained for specific time intervals at controlled relative humidity conditions (RH = 50% and RH = 90%); the formed mineralogical phases were characterized by µFT-IR and X-ray diffraction (XRD). Results indicate that the used solvents can influence the kinetic and reaction pathways, while the phases formed at the end of the carbonation process are influenced by both solvents and RH conditions. The effectiveness of calcium ethoxide based product diluted in 2-butanol and n-butylacetate as limestone consolidants was evaluated with drilling resistance measurement system (DRMS) and ultrasound pulse velocity (UPV). The impact on color coordinates was also assessed. The results were compared with those obtained with the same product diluted in ethanol and a commercial nanolime. The use of these solvents gave different and better results in terms of efficacy.

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Section: Study Of Carbonation Processmentioning

confidence: 94%

Calcium Ethoxide as Consolidant for Porous Limestones: Influence of the Solvent

et al. 2019

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“…The catalysts were always mixed into ethanol and added last to the rest of the mixture. The role of addition of the mixture of C11–C13 alkanes has been described in detail elsewhere [11]. The consolidation action of silicate-based consolidant is based on the sol–gel process and occurs through hydrolysis and a water and/or alcoholic condensation reaction which leads to the formation of silica gel [32].…”

Section: Methodsmentioning

confidence: 99%

“…To overcome this problem, a water-based solution of calcium acetoacetate was synthesised and proposed for the consolidation of carbonate-based substrates [10]. As it is a water solution, which means lower evaporation rate of the solvent compared to organic solvents, deeper penetration into the material could be achieved, where a recohesion between particles could be established [11]. Moreover, due to higher concentrations of the consolidant, the number of successive applications of the consolidants can be significantly reduced, without any white haze on the treated surface [9].…”

Section: Introductionmentioning

confidence: 99%

“…For silicate-based substrates, a modified formulation of a commercial product based on silicate ester was developed. Due to a balanced combination of polysilicate, dioxalane, a mixture of C11–C13 alkanes (liquid paraffin) and diethylethanolamine, the consolidant has a low dry mass [10] with uniform consolidation through the profile of the substrate [11].…”

Section: Introductionmentioning

confidence: 99%

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Efficiency of Novel Photocatalytic Coating and Consolidants for Protection of Valuable Mineral Substrates

et al. 2019

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In the process of protection and consolidation of valuable materials, the efficiency is the crucial property that needs to be considered. TiO2/ZnAl layered double hydroxide (LDH) coating and silicate- and carbonate-based consolidants were synthesized and proposed to be used for protection and consolidation of four porous mineral substrates: brick, stone, render and mortar. The photocatalytic efficiency of TiO2/ZnAl LDH coating, as well as consolidation efficiency of two consolidants, both applied on model substrates, were studied. The photocatalytic coating showed significant activity and performed well after the durability tests involving rinsing and freezing/thawing procedures. After treatment with both consolidants, a serious enhancement of consolidation of the used substrates was found. On the other hand, the application of TiO2/ZnAl LDH, as well as consolidants, caused negligible changes in the water vapour permeability values and in appearance of the porous mineral substrates, indicating a high level of compatibility.

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“…To this purpose, complementary structural and compositional investigation of both crystalline and amorphous phases through the substrate stratigraphy can be achieved by exploiting high lateral resolution micro-spectroscopy techniques. At this regard, micro (µ)-FT-IR (either in reflection or ATR mode) and μ-Raman spectroscopies already demonstrated to be valuable tools to probe the distribution (depth profiles and mapping) of consolidants into carbonate and silicate substrates at lateral resolution down to 5–7 μm 8 – 10 . Nevertheless, extended overlapping of the vibrational bands in these techniques may hamper clear distinction of the newly formed phases in the microstructure of the stone matrix.…”

Section: Introductionmentioning

confidence: 99%

Synchrotron radiation Ca K-edge 2D-XANES spectroscopy for studying the stratigraphic distribution of calcium-based consolidants applied in limestones

Monico

Cartechini²,

Rosi³

et al. 2020

Sci Rep

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In Heritage Science, the evaluation of stone consolidation treatments by investigating the nature of in situ newly formed products and their penetration depth within the consolidated matrix is a grand challenge. A number of analytical methods have been proposed, but, currently, most of them are not able to supply a full overview of the spatial, structural and compositional information of the newly formed crystalline and amorphous phases with a submicrometric lateral resolution. Here, we examined, the capabilities of synchrotron radiation (SR)-based two-dimensional X-ray absorption near-edge structure (2D-XANES) spectroscopy at Ca K-edge for determining the structural and compositional properties of the compounds formed after the application of a calcium acetoacetatebased consolidant on a porous carbonatic stone (limestone) and for investigating their stratigraphic distribution at the submicrometric scale length. We evaluated advantages and drawbacks of three Ca K-edge 2D-XANES-based approaches: (i) transmission mode full-field-XANES (FF-XANES) imaging; (ii) micro-X-ray fluorescence (μ-XRF) mapping above the Ca K-edge combined with the acquisition of XRF mode μ-XANES spectra at a limited number of spots; (iii) full-spectral µ-XANES (FS µ-XANES) mapping in XRF mode and its variant called selectively induced X-ray emission spectroscopy (SIXES) mapping. Overall, Ca K-edge 2D-XANES spectroscopy provided accurate qualitative and semiquantitative information on the newly formed calcium carbonates (i.e., amorphous calcium carbonate, vaterite and calcite) and their stratigraphic distribution at the submicrometric scale, thus opening a new scenario to study the carbonatation process of calcium-based consolidants in limestones. Stone consolidation is a major challenge for protection of buildings and stone artefacts from weathering and decay, which usually lead to decohesion of the structural elements of the material. Over the last decades, thanks to the progress in material science and nanotechnology, a wide range of novel materials has been developed, with the aim of re-establishing adhesion, cohesion and stability of the damaged stone as well as to improve efficacy and durability of the treatment 1,2. The effectiveness of a consolidation treatment depends on different aspects, including penetration depth, reaction kinetics and mechanism of formation of the final products, and physical-chemical properties of the consolidant phase in the stone matrix. In consideration of that, tailored analytical tools and methodologies have been developed to characterize newly synthesized consolidation products and to understand the chemistry behind their performances. Although

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Evaluation of vibrational spectroscopic techniques for consolidants’ penetration depth determination

Cited by 12 publications

References 28 publications

Calcium Ethoxide as Consolidant for Porous Limestones: Influence of the Solvent

Calcium Ethoxide as Consolidant for Porous Limestones: Influence of the Solvent

Efficiency of Novel Photocatalytic Coating and Consolidants for Protection of Valuable Mineral Substrates

Synchrotron radiation Ca K-edge 2D-XANES spectroscopy for studying the stratigraphic distribution of calcium-based consolidants applied in limestones

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