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Biomineralization for Limestone Consolidation

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Biomineralization for Limestone Consolidation Biomineralization for Limestone Consolidation Science and Engineering of Natural Stones and Glass HS 2019 Letizia Caderas ETH Zürich, December 2019 Contents 1. INTRODUCTION .................................................................................................................. 3 2. BACKGROUND BIOMINERALIZATION ............................................................................. 4 3. ONSITE TESTS OF THE GRANADA METHOD ................................................................. 5 The gardens of Queluz Palace ............................................................................................. 5 Loulé church main portal ...................................................................................................... 6 4. EVALUATION OF THE BIOMINERALIZATION TECHNIQUE ........................................... 7 5. CONCLUSION ..................................................................................................................... 8 REFERENCES ......................................................................................................................... 9 1. Introduction Carbonate stones have been used for many millennia as a building material, which has led to a heritage of buildings and monuments of cultural significance that is considered worth preserving today. However, physical, chemical and mechanical processes lead to a degradation of the carbonate stone structures [1]. The strength of carbonate stones is given trough cohesion, which is provided by either mineral bridges or a mechanical interlocking effect [2]. Therefore, a major problem is the dissolution of the calcareous substrate, which decreases the cohesion of the building material and increases the porosity of the stone [3]. Consolidation treatments aim to restore the cohesion between grains of the deteriorated layer of the stone [4]. For the choice of a suitable consolidation treatment, some criteria should necessarily be taken into account. The factors “effectiveness – harmfulness – durability” of the treatment need to be regarded as a magic rule. The effectiveness is a measure of the strengthening effect of the consolidation, whereas the harmfulness considers whether an incompatibility between the treatment and the stone can induce additional damage. Unfortunately, effectiveness or compatibility can often only be increased at the expense of the other [5]. One of the most widely used and commercial available consolidation products nowadays are based on alkoxysilanes. In general, these consolidation products achieve to re-establish the cohesion of the loosened grains through Si─O─Si network by either filling the interspace and thus locking the grains, or by glueing the grains together via adhesive bridges [6][7]. The Si ─ O ─ Si network is formed after a sol-gel process. Apart from the effectiveness of alkoxysilanes consolidation treatments, an increased penetration depth due to low viscosity, reduced visual alterations, low material costs and a simple application are among the advantages of this consolidation treatment [1]. However, two issues limit the successful application of alkoxysilanes based treatments on porous carbonate stone. First, it had been observed that the polymerisation process is altered in the environment of the carbonate substrate. Second, on carbonate substrate, a lack of strong bonds to the Si─O─Si network attenuates the consolidation effect. The silica network and the loosened grain cannot establish a strong chemical bond since anchor points on the carbonate substrate are missing, that could react with the hydrolysed species [8][9].The choice of the right coupling agents can improve the adhesion between the silica network and carbonate substrate. This way, improvements in strength are reported, although the role of the coupling agents on the consolidation is not fully investigated yet [1]. An alternative option to consolidate carbonate stone is given by biomineralization. Biomineralization is the formation of minerals by living organisms. The phenomena are widespread and occur in almost all groups of organisms [10]. It was shown that under suitable environmental conditions, all bacteria can form calcium carbonate precipitates [11]. In 1990 Adolphe et al. were among the first to test biomineralization as a consolidation technique for ornamental stone and applied for the patent of the so-called Calcite Bioconcept technique. From this point on, much research has been done to find suitable bacteria, and different consolidation approaches were developed in research based on the biomineralization. This report deals with the principles of biomineralization and presents two different consolidation methodologies: Calcite Bioconcept technique and the Granada method. Two application examples of the Granada method are examined. Based on this, biomineralization as a viable consolidation technique is evaluated. 2. Background biomineralization In biomineralization, two general mechanisms are considered: biologically controlled mineralization (BCM) and biologically induced mineralization (BIM). In the controlled precipitation mechanism, the organism is responsible for the nucleation and growth of the minerals. The minerals are deposited on or within the cells of the organism. Mineral structures like bones or shells are formed by BCM. Different to that, BIM describes a process where the precipitation of minerals is a consequence of the microbial metabolic activity. The minerals are deposited in the environment, whereby the precipitation of the minerals is highly dependent on environmental conditions. In the case of calcium carbonate precipitation, the governing factors are the pH, the amount of dissolved inorganic carbon, the calcium concentration and the availability of nucleation sites [12]. It was shown that under suitable environmental conditions, all bacteria can form calcium carbonate precipitates [11]. Many metabolic pathways induce the precipitation of calcium carbonate. One example is the hydrolysis of urea, which leads to fast precipitation of calcium carbonate. In this pathway, urea is degraded to dissolved inorganic carbon and ammonium. A simplification of this process is illustrated in Figure 1. It is their negatively charged bacterial cell wall, that attracts the positively charged calcium ions. Along with the dissolved inorganic carbon in the close environment, this leads to an oversaturation and calcium carbonate is precipitated. This is one out of many possible metabolic pathways. Further pathways are not discussed in this report. Through the various studies on biomineralization as a consolidation technique, two basic approaches have evolved. One is covered by the Calcite Bioconcept patent and the other by the Granada method. In the approach of Calcite Bioconcept bacterial strains are inoculated to the stones substrate. Contrary to this method, in the Granada method, only a nutritional medium is inoculated, such that the resident bacterial strains are activated. This method relies on the findings that under suitable conditions, most bacteria induce the precipitation of calcium carbonate [5]. Figure 1: Simplified illustration of the hydrolysis of urea that induces the precipitation of calcium carbonate. (A) Through the metabolic pathway of the bacteria, dissolved inorganic carbon and ammonium (DIC) and ammonium (AMM.) accumulate in the surrounding of the bacteria. Due to the negatively charged cell wall of the bacteria, calcium ions gather around the bacteria. Due to a local supersaturation, calcium carbonate precipitates. (B) Precipitated calcium carbonate amasses around the cell. (C) The cell becomes encapsulated, limiting the nutrient transfer, which leads to the death of the cell. [4] 3. Onsite tests of the Granada method In a study by J. Delgado Rodrigues and A.P. Ferreira Pinto, the Granada method was tested onsite. The commercial product MYXOSTONE M3P of a nutritional medium was used. The nutritional medium was applied by spraying several times for one week to keep the damaged surface wet. Moreover, the treated area was sheltered from sunlight and in some cases, additionally from extreme temperature or relative humidity conditions. The shelters were installed for one month [5]. This way, two already greatly deteriorated structures were treated. Trial tests were conducted on Ançã stone, a very soft and porous limestone, in the garden of Queluz Palace in Portugal. Further tests were then conducted on some parts of the main portal of the Loulé church, made of limestone of moderate porosity [5]. The assessment of the consolidation performance was obtained with non-destructive characterization methods. Water absorption tests by the pipe and sponge and tape peeling tests were performed. Colour variations were investigated as well. Concerning the stones in the garden of Queluz palace, drilling resistance measurements were accepted additionally. The gardens of Queluz Palace The trial tests in the gardens of Queluz Palace showed that the biomineralization processes lead to a hardening of the treated surfaces. In Figure 2 the transition between an untreated and treated surface can be seen. It can be recognised, that the treatment led to a yellowish colouring. Additionally, some grey spots were visible, possibly the formation of fungi was promoted. The results of drilling resistant measurement in Figure 3 demonstrated that the treatment led to a surface of increased drilling resistance with a 2-4 mm depth. In areas where the stone was already greatly deteriorated, a strengthening
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