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Built Heritage 2013 Monitoring Conservation Management

Long-term evaluation of the salt decay susceptibility of NHL commercial mortars
Davide Gulotta1; Cristina Tedeschi2; Sara Goidanich1
1
Politecnico di Milano, Department of Chemistry, Materials and Chemical Engineering “Giulio Natta”, Milan, Italy; 2 Politecnico di Milano, Department of
Civil and Environmental Engineering, Milan, Italy
1. Introduction
The damage induced by salt crystallization is recognized as a primary cause
of degradation of the built heritage [Doehne, 2002]. Outdoor environments
provide a wide range of possible sources for soluble salts, including atmospheric pollutants, de-icing compounds, fertilizers, rising damp from salt-loaded
soils, etc. [Charola, 2000]. Salts may as well be formed as a result of chemical
reactions between construction materials and a chemically aggressive atmosphere [Gulotta et al., 2012], or they can already be contained into the historic
substrate itself.
The mobility of such compounds inside porous materials is strictly related to
the presence of water, both in the liquid or vapour phase, which is able to
solubilize them and then to favour the migration of the saline solution. The
location of the salt crystallization depends on several factors but it is strongly
influenced by the moisture transport processes and by the specific solubility
characteristics of the salt [Sawdy et al., 2008]. In addition, the microstructural
features of the substrate (porosity and pore size distribution) are known to
play a fundamental role in salt damage [Scherer, 2004]. In general, soluble
compounds with high solubility tend to migrate for longer distances and deeper into the material, whereas less soluble ones tend to accumulate and to
progressively clog the porosity. This typically occurs in vertical walls subjected
to rising damp, in which a vertical fractioning of the soluble salts location takes
place [Zehnder, 2007].
The damage mechanism occurring to salt-loaded substrates is triggered by
the periodic repetition of crystallization/dissolution cycles, as a result of the
variation of the environmental parameters (in particular, T and RH). The crystallization pressure of the growing crystals is sustained by the presence of a
thin layer of residual saline solution which transfers the mechanical stresses
to the pore walls. Depending of the degree of supersaturation, the crystallization pressure can overcome the tensile strength of the material and if it
spreads to a region large enough to propagate strength limiting flaws, can
ultimately result in significant damages [Flatt, 2002].
On a macroscopic scale, salt crystallization damage causes the granular disaggregation of the mineral matrix of the substrate, due to the progressive
loss of mechanical strength. In case of either particularly severe exposition
conditions or salts having high crystallization pressure, the evolution of the
damage can be rapid and can lead to significant loss of the original material.
The conservation intervention of historic masonries in such conditions includes the substitution of the deteriorated construction elements and the restoration of the structural integrity by introducing new mortars. A compatible approach is required along the entire intervention and, as far as the selection of the
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Built Heritage 2013 Monitoring Conservation Management restoration materials is concerned. specimens were dried at 60°C. Two types of specimens were prepared: 4 cm cubic specimens (two sets) casted in demountable steel moulds. Mortars were prepared following the technical indications of the suppliers as for water content and mixing operation. Mass varia1126 .5 cm. given the extraordinary character of the conservative intervention and the need for a highly cost-effective approach.80% RH. After each weekly cycle. Fluka). and those belonging to set 1 alone were brushed to remove all the damaged material.. The commercial materials are specifically designed to be used in the conservation of the architectural heritage. Specimens of both types were stored at 20°C . underwent a long-term testing protocol in order to better simulate reliable exposition conditions. Wallettes. are declared totally cement free and having a very low content of soluble salts by the supplier. Each imbibition/drying step was repeated 4 times a week. 2 hours immersion to a 1 cm depth in a 10% sodium sulphate solution (anhydrous Na2SO4 reagent grade. 2. 22 hours drying period at 20°C . Moreover. 2013]. According to the RILEM procedure.1. This class of products actually provide a valuable alternative to traditionally prepared mortar but their compatibility and durability at work still rely on a limited number of study. type “San Marco” (San Marco. Italy). in particular. Crystallization tests Crystallization tests on the two sets of cubic mortar specimens were performed as it follows: sealing of the four lateral faces and drying at 60°C until constant weight. Materials and methods 2. In the present work the evaluation of the salt decay susceptibility of four commercial pre-mixed NHL mortars is presented. which highlighted that supposedly similar material indeed had rather different features.90% RH for 60 days. Products and specimens preparation Four commercial ready-mixed mortars have been selected among the most diffused products in the Italian market. mortar specimens and simplified masonry systems (wallettes) have been tested against sodium sulphate crystallization. The results here presented are focused on the correlation between the mortars characteristics and the salt decay susceptibility. The complete characterization of the anhydrous commercial mortars and of the hardened ones has been discussed in a previous work [Gulotta et al. To this extent. Wallettes were prepared by using traditional fire-clayed red bricks. 25x24x12 cm wallettes with an average thickness of mortar joints around 2. 2.2. 1999]. it implies that the new mortars should not cause any direct or indirect damage to the original masonry [Van Hees. and approx. NHL pre-mixed mortars have been chosen due to their increasing use in the field of built heritage conservation. All products are intended for bedding operations of masonries. data representative of both categories have been analysed by means of Principal Component Analysis. restoration mortars should also assure an adequate overall durability. are based on NHL binders according to the current standard [UNI-EN 459: 2010].

corresponding to a twoweeks testing period.0 by 2. equipped with an Oxford INCA 200 . equipped with a Leica DFC290 digital camera. M2 is the only exception to this trend. or continuous thin crust-like crystallization (M4). In particular.Built Heritage 2013 Monitoring Conservation Management tion was then recorded to obtain the damage extent as loss of material (set 1) and the salt uptake (set 2). The evaporation surface of all other specimens started developing efflorescences since the second cycle in form of either irregular white veils mostly located along the lateral edges (M3 and M1). Scanning laser profilometry was performed by means of a laser sensor with a spot of 1. Seven cycles (1 week per cycle) were performed. The first two cycles. the salt crusts over the evaporation surfaces grew in thickness and tended to progressively detach from the substrate.1 procedure (RILEM 1998). 2.unige. The related general mass increase of almost all samples confirms the progressive accumulation of sodium sulphate within the porous network of the material.Pentafet LZ4 spectrometer in secondary electrons mode. The standard distance of the sensor from the surface is 100 mm with a measure range height of +/.00 mm.3.8%. During this phase the salt uptake due to capillary imbibition of the saline solution can be considered the prevalent mechanism.1 1127 . It showed a rather constant weight along the entire test indicating that the saline solution could hardly penetrate through the porosity and no significant salt accumulation took place in this case. Crust eventually started to crack and to flake. Mercury intrusion porosimetry (MIP) of mortar samples coming from the cubic specimens and from the wallettes were analysed with a Micromeritics AutoPore IV 9500 series mercury intrusion Porosimeter. All significant variations of the upper evaporation surface of the specimens were recorded and photographically documented. The sensor is connected to a vertical steel frame through a dragging trolley. Results and discussion 3. The latter pattern became the most common as the test proceeded. moving on a linear support beam by means of a step by step electric motor. Wallettes were tested according to the RILEM MS-A. The observation of the mortar just beneath showed that the mineral matrixes suffered partial to massive granular disaggregation as a result of the development of a diffused network of elongated fibre-like sodium sulphate crystals (Fig.40 mm.1. along a measurement range of 200 mm. a resolution of 40 μm and a linearity of 0. Ten crystallization cycles (4 weeks per cycle) were carried out. caused no visible damage to the mortars. Analytical technique and data treatment Stereomicroscopy by means of a Leica M205C stereomicroscope. 3.parvus. Salt decay susceptibility of mortars The crystallization patterns and the damage evolution were continuously monitored during the test by means of visual observation. Environmental scanning electron microscopy (ESEM) by an Environmental scanning electron microscope Zeiss EVO 50 EP. Data have been analysed by Principal Component Analysis (PCA) by using V-Parvus 2010 software [www.it] on all the characterization and damage results.

2 right). salt efflorescences and elongated fibrous crystallization (left). M2 developed no damage at all (Fig. The result of M3.Built Heritage 2013 Monitoring Conservation Management Fig. In particular. 2 right). Fig. and photographic documentation of mortar M1 and M2 at the end of the test (right) 1128 . The salt susceptibility of M3 can therefore be defined as medium. The same mechanisms then took place within the outermost portion of the mortar and contributed to the granular disaggregation and flaking. medium to severe loss of material was observed respectively for M4 and M1 (18% and 35% mass decrease respectively) indicating a high salt susceptibility.Stereomicroscopic documentation of the surface of mortar M1 at the end of the test showing massive granular disaggregation. the loss of material of M3 was concentrated along the edges of the upper evaporation surface alone.2 . a similar damage was observed for M4 but to a minor extent. 2 left).Percentage mass variation of the cubic specimen respect to the initial weight (left).1 . As for the visible damage extent of the specimens: flaking and granular disaggregation of M1 lead to massive loss of the upper surface (up to 1 cm depth) and to the damaging of the lower imbibition surface as well (Fig. At a microscopic level. showing a final weight higher than the initial one. M2 suffered no significant mass variation thus demonstrating a low salt susceptibility. The salt decay susceptibility of the tested mortars was evaluated respect to the final mass variation (Fig. ESEM documentation of the same surface showing tabular and prismatic aggregates of Na-sulphates at the interface of a detached mortar scale (right) left). the observed massive formation of well-developed sodium sulphate tabular and prismatic crystallization at the crust-mortar interface (especially for M1) was responsible for the crust detachment (Fig.1 right). indicated that the limited loss of material induced by the crystallization cycles was counteracted and slightly overtaken by the total salt uptake.

corresponding to fourweeks testing period.Salt decay susceptibility of wallettes Salt crystallization over the evaporation surface of the specimens occurred after the first imbibition stage with the sodium sulphate solution. the salt decay susceptibility of the mortars can be defined as low for M3.3 . Few small salt plaques preluding to salt crust were also observed at this stage of the test. Under the aesthetic point of view. Fig.3 left). M2 showed a different deterioration pattern as most of the damage induced by mortar disaggregation took place in the central area of the joints rather than along the border. After this threshold. The overall entity of the damage (loss of material) was calculated as the area of the section defined by the initial profile of the wallette and the one recorded at the end of the test. M2 and M3 also suffered important alteration due to superficial darkening (M2) and yellowing of the joints (M3). The most diffused crystallization pattern was the formation of elongated fibrous crystals growing perpendicularly respect to the surface. According to the final loss of material (Fig. Mortars showed no significant damage until the fourth crystallization cycle was performed. as well as granular disaggregation of the underlying material. medium for M2 and M4 and very high for M1. Blistering and delamination caused loss of material and revealed the presence of a diffused crystallization just beneath the detaching fragments. diffused superficial flaking of M1 joints was observed. These were located on both mortar joints and bricks. and variation of the pores concentration of the mortars within two significant dimensional fractions as a result of the preparation condition (right): cubic specimens (C) and wallettes (W) 1129 . Measurements were conducted by means of scanning laser profilometry on fixed reference positions.Built Heritage 2013 Monitoring Conservation Management 3.2 .Final damage extent of the wallettes as loss of material measured along the longitudinal mortar joint (left). The variation of the surface profile of wallettes was monitored along the horizontal mortar joint (longitudinal damage) and the vertical one (transverse damage) at the end of each cycle. at the expenses of the brick elements. The first occurrence of damage was recorded at the end of the first crystallization cycle. The mechanical stress induced by the crystallization along the brick/joint interface also determined the de-bonding of some of the brick elements of specimens M3 and M4.

01 μm) is concerned.Loading and scores plots from Principal Component Analysis of the characterization and damage data of cubic specimens (left) and wallettes (right). Considering that high crystallization pressure can be developed in materials characterized by the presence of mesopores (Flatt 2002). In Fig. P = portlandite.01 μm thresholds are plotted for mortars prepared in different conditions.1 μm and 0. it can be noted that no variations occurred to M1 and M3. On the other hand. It is worth noting that the use of a porous substrate generally resulted in the increase of the small porosity (below 0. re-wetting operations.1 μm = % of pores below 0. in particular. On the contrary. Ca agg = carbonatic aggregate. Por<0. the former showed a slight improvement in the salt resistance. %Mass var = % mass variation respect to the initial weight. some differences were noticed in the decay extent for M4 and. the microstructural features of mortars are known to strongly influence the crystallization mechanisms (Benavente et al. A preliminary analysis was conducted taking into account all the compositional. L damage = loss of material along the longitudinal joint. 3 (right) the percentages of pores below the 0. the variations in the mortars pore structures can be related to the enhanced and slightly reduced salt susceptibility of respectively M2 and M4. which is particularly noticeable for M2. Si agg = quartz-siliceous aggregate.3. It has to be noted that. Por<0. M4 showed a slight decrease of the pore concentration in this fraction. As a matter of fact. PCA analysis PCA was carried out in order to examine the correlation between the mortars characteristics and the salt decay susceptibility. 3. beside the variation of the specific testing conditions (imbibition procedure. As far as the percentage of pores belonging to the finest fraction (below 0. σC = 60 days compressive strength.01 μm = % of pores below 0.4 . for M2. Changes in the porosimetric structures of the tested mortars were caused by the use of a porous substrate (brick) instead of the standard steel moulding in the wallettes preparation. whereas the only significant increment took place in M2.1 μm. T damage = loss of material along the transversal joint 1130 . and global duration of the test). duration of the cycle. while the latter demonstrated a significant increase of the damage as a result of the different crystallization protocol. mechanical and miFig.01 μm.1 μm).Built Heritage 2013 Monitoring Conservation Management The results of the wallettes confirmed the general behaviour respect to salt susceptibility emerged by the testing of the cubic specimens in the case of mortar M1 and M3. H = Larnite and hydraulic compounds. which results in greater damage. 2004). Med pore rad = median pore radius.

in particular. and. to a lower extent. the above mentioned correlations still applied. but none of these variables was clearly linked to the damage. The vectors represent the original variables and their length is proportional to the contribution to the PCs. In such conditions the durability of the conservative 1131 . therefore this data cannot be directly used for the evaluation of the durability. In Fig. As for the cubic specimens. whereas a high hydraulicity of the binder seemed to increase the durability.4. also to the percentage of pores below 0. The damage evaluation along transversal and longitudinal sections of the joints provided highly correlated results. This confirmed that the final damage extent is related to the absorption of the saline solution through the porous network. As far as the wallettes are concerned. whilst the hydraulic content was again a strengthening factor respect to the damage. Three principal components (PC) were finally obtained for both the testing protocols which accounted for 100% of the total variance. and in at least one case the salt susceptibility was extremely high and caused massive loss of material. Conclusions The tested mortars demonstrated rather different behaviours respect to sodium sulphate attack. the portlandite content. It is worth noting that in both testing conditions. seemed to have a good correlation with the damage. As expected. the percentage of pores below 0. PC1 accounted for 57. suggesting that the two methodologies for the damage assessment are rather comparable. This is most probably related to the influence of the brick substrate which affected the development of the porous network of the mortars.01 μm. PC2 accounted for 38.8% of the total variation and it was mostly linked to porosity. and hydraulic behaviour of the binder fraction. The results allowed to identify the most significant data and to reduce the successive elaborations to a 12 variables dataset. The salt susceptibility was positively related to the presence of fine porosity and mesoporosity. expect for total porosity and median pore radius which appeared less linked. A positive correlation was observed between the mass variation due to loss of material or crust formation and the salt uptake. Such results should be properly considered especially in case of intervention on salt loaded or not completely desalinated substrates. bulk density. porosity and median pore radius were positively correlated. the mechanical resistance of the mortars was not correlated to the damage. and both had a negative correlation with the bulk density of the mortar.2% of the total variation and it was mostly linked to the type of aggregates.Built Heritage 2013 Monitoring Conservation Management crostructural characterization data.01 μm). which was able to describe the specific features and durability of the mortars with no loss of information. A positive correlation existed between the percentages of pores in the two intervals considered (0.1-0. for a total of 24 variables. Pores belonging to the finest fraction. as well as those related to the damage extent. The content of carbonatic aggregate was negatively correlated to the quartz-siliceous one.1 μm. 4. The angle between any couple of variables increases as the respective correlation becomes less significant. loadings of the cubic specimens (left) and of the wallettes (right) are shown for autoscaled data.

2010. «Journal of Crystal Growth». the hydraulic behaviour of the binder seemed to be effective in the damage limitation. J. the percentage of fine pores (<0. The high amount of pores in such porosimetric fraction was generally associated to the worst durability results and can therefore be considered a potential risk factor.Built Heritage 2013 Monitoring Conservation Management operations can still be a critical issue. 31-42. Salts in the deterioration of porous material: an overview. Scherer G. Acknowledgments The Authors wish to thank Professor Luigia Binda for her useful suggestions during the experimental phase. in Siegesmund S. Part 1: Compositional and mechanical characterisation.. (Eds) «Natural Stone.. Toniolo L.M. C. «Journal of the American Institute for Conservation». A review of salt transport in porous media. Hughes... 2007.. Weathering Phenomena. Toniolo L. «International RILEM Workshop on Historic Mortars: Characteristics and Tests».. «Construction and Building Materials» 38..G. 1613-1624. 2-19.. 27-35. 532-544. Fermo P.. Tests for masonry materials and structures. 327-343. Paisley (Scotland). heritage A. Piazzalunga A. Groot.. 2004. J.. specification and conformity criteria.. Role of pore structure in salt crystallisation in unsaturated porous stone.01 μm) was more correlated to the damage respect to the total porosity and the median pore radius. Copenhagen. Gulotta D. del Cura M. Ordóñez S.J. 242 (3-4). Tedeschi C. «Cement and Concrete Research».G.. in Bartos P.. The PCA analyses allowed a better understanding of the relationship between the mortars characteristics and their salt susceptibility. The microstructural features clearly influenced the salt crystallization mechanism.. Pel L. 1-27. 260 (3-4). Gulotta D. UNI-EN 459-1. Commercial NHLcontaining mortars for the preservation of historical architecture. In particular. Goidanich S. 51-64.. «Materials and Structures»...W. 1132 ... Moreover. 52 (2). Under the compositional point of view.. Sánchez-Moral S. Flatt R. (Eds).. Charola A. 1085-1094. Vollbrecht A. 39 (3). RILEM Technical Committee.A. assessment methods and salt reduction treatments. Bertoldi M. Conservation Strategies and Case Studies». «Journal of Crystal Growth». Stress from crystallization of salt. 2000.. whereas the aggregate composition did not show a significant correlation with the decay extent. Weiss T. «Environmental Geology». 22-24 October 2008. Sawdy A. 1998. 2002. Building Lime . 2012. García-Guinea J.J.Definitions. The Angera stone: a challenging conservation issue in the polluted environment of Milan (Italy). Bortolotto S... Nijland T. 2002. Van Hees R. 353-367.. 34 (9). 435-454. The compressive strength seemed not to be directly linked to the mortars durability as well. Geological Society. 2004. «Environmental Earth Sciences». References Benavente D.. 2008. 2013. 1999. RILEM Publications. Long-term monitoring of wall paintings affected by soluble salts.. the salt susceptibilities of some of the mortars were significantly diverse according to the two testing protocols which have been followed (cubic specimens/long term evaluation of wallettes).. Proceedings of the International Conference «Salt Weathering on Buildings and Stone Sculptures». Salt weathering: a selective review. Zehnder K. Damage diagnosis and compatible repair mortars. 69 (4).N. Salt damage in porous materials: how high supersaturations are generated. Doehne E.