“Earthen construction can be approached at a technical and even scientific level, just like other construction technologies. The current research effort in this area proves it. This material is not limited in its applications, as long as we know how to use the widest range of its qualities wisely and overcome its shortcomings.”
(Hugo Houben and Hubert Guillaud, Traité de Construction en Terre, (1989), ed. 2006, p. 9)
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The presentation of the results from the experimental work is divided into three main parts related to the key goal aspects of the products’ evaluation in the present project: efficiency, compatibility, and durability. In the first and second parts (efficiency and compatibility), a set of tests was performed to assess the interaction between the selected consolidants and water repellents and the adobe and rammed earth specimens. After the products’ application, the specimens remained in a controlled environment (temperature and humidity at 20 °C and 60%, respectively) for 15 days to guarantee complete stabilization of the specimens and products before testing. The treated specimens and the reference ones (not treated) were then analyzed following the experimental program already presented in the previous chapter. There was always a stabilization period of a minimum of 15 days at the same conditions (20 °C and 60% RH) between each test.
After finishing the efficiency and compatibility assessments, the same specimens were placed inside the climatic chamber to initiate the durability test by exposing them to temperature and humidity cycles. For this part of the study, two main lines of analysis were conducted – a control system, which means a set of tests done in a time span of approximately two months (measured as the number of exposed cycles); and a final assessment, where all tests done before starting exposure were repeated only at the end of the durability test.
All the results from the experimental campaign are presented in the present chapter. The obtained data from each test is reported in the respective section with a bar graph indicating the average value and standard error value. The final data in the bar graphs are the result of the average of five specimens per each group of product and reference. However, in some cases, outliers were identified and excluded from the average calculation. In addition, for each test, a table with the indication of the average values, standard deviation, standard error (calculated as the ratio between the standard deviation and the square root of the number of specimens), and coefficient of variation (further referred to as CoV, calculated as the ratio between the standard deviation and the average, in percentage) is reported. Additionally, all obtained data from each specimen in each test are reported in detail in Appendix III.
5.1. Efficiency
The efficiency of the consolidants and water repellents applied on adobe and rammed earth specimens was assessed by five different methods: contact sponge method, microdrops absorption time, contact angle, water vapor permeability, and colorimetric parameters. The obtained data are presented and discussed herein in the next sections.
147 5.1.1. Water absorption – Contact Sponge Method
Based on the visual inspection of the specimens’ surface, after performing the contact sponge method test, both adobe and rammed earth showed no evidence of material loss, deformation nor cracking. Moreover, by inspecting the surface of the sponge after completing the test, it was also observed the absence of any residual material on it. Observing the examples in Table 5.1, reference specimens exhibit a clear mark by the contact between the wet sponge and the earthen material, whereas in some cases of treated specimens this mark is less evident or even not present such as in the case of ethyl silicate, casein, siloxane, and beeswax. On the contrary, some specimens with applied products, as nanoparticles of silica, limewash, and cactus juice, exhibit a clear mark left by the sponge, corresponding as well, to higher values of water absorption (see Figure 5.1 and Figure 5.2). According to the results of the contact sponge method, in general, untreated adobe specimens absorbed less water than untreated rammed earth specimens, which can be explained by the presence of less active clay.
Table 5.1: Examples of contact sponge method done in adobe and rammed earth specimens with and without treatment.
Adobe Rammed earth
Reference
Ethyl silicate
Nanoparticles of silica
Limewash
Casein
Reference
Ethyl silicate
Nanoparticles of silica
Limewash
Casein
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Cactus juice
Siloxane
Beeswax
Cactus juice
Siloxane
Beeswax
Looking at the treated specimens, as expected, specimens with water repellents revealed a reduction in water absorption, thus suggesting the effectiveness of these treatments. But also, some of the consolidants’ group revealed a significant reduction of water absorption, namely ethyl silicate, Arabic gum, and casein, indicating the possibility of using it simultaneously as a consolidant and a protection layer.
In the case of the adobe specimens treated with ethyl silicate, Arabic gum, casein, aquashield, linseed oil, and beeswax, a similar reduction in water absorption was observed, with a decrease of about 94%, and the siloxane and paraffin wax with even a higher decrease of water absorption, around 97%. These values represent a significant improvement in the water repellence capacity of the adobe surface.
Also, in rammed earth specimens, the same impressive results are observed. There is a decrease of approximately 97% of water absorption after applying siloxane and paraffin wax, 91% in the case of casein and linseed oil, and 95% with ethyl silicate, aquashield, and beeswax.
On the other hand, specimens treated with nanoparticles of silica and limewash seemed to develop a contrary effect, increasing the water absorption, which could promote the material degradation.
149 However, it is important to underline that high values of variation were obtained, even after the elimination of outliers. This may be due to the heterogeneity among specimens, with irregularities of the surface, for instance, a greater number of voids, leading to less water absorption. So, according to these data, it is possible to conclude that the surface morphology plays an important role in the homogeneity of results.
Figure 5.1: Obtained data from the contact sponge method test performed on the adobe specimens with the indication of the average values, standard deviation, standard error (marked in the error bars as well), and the coefficient of variation.
Figure 5.2: Obtained data from the contact sponge method test performed on the rammed earth specimens with the indication of the average values, standard deviation, standard error (marked in the error bars as well), and the coefficient
of variation.
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5.1.2. Water repellency – Microdrops absorption time
To assess the water repellency of the applied products on both earthen techniques was the microdrops absorption time. Since this experiment consists of placing drops of water on top of the specimens’ surface, the images captured during the test reflect immediately and in a visual way the results. Therefore, in Table 5.2 it is possible to observe the differences between the water droplets on top of distinct specimens.
In the reference ones (both adobe and rammed earth), the water droplets were spread on the surface and absorbed immediately. While in almost all cases of the treated specimens (ethyl silicate, Arabic gum, casein, siloxane, aquashield, linseed oil, beeswax, and paraffin wax), the drops were compelled to form a spherical shape, showing the hydrophobic effect of these products. In the case of the nanoparticles of silica, cactus juice, and black soap, the drops did not form a sphere but the absorption was slower, whereas in the case of limewash the water droplets spread on the surface and were rapidly absorbed. So, based only on the visual inspection during the test, it is possible to verify that some products showed water repellency properties while others had no hydrophobicity effect.
Looking now to the obtained data, reported in Figure 5.3 and Figure 5.4, similar conclusions can be attained. This test is performed by comparing the microdrops absorption time with a reference surface (glass) and the absorption time (𝑡𝑥), expressed in percentage of the evaporation time of the droplets on the glass surface (𝑡𝑣) through equation:
𝑡𝑥
𝑡𝑣 × 100 (%) (4)
Hence, values over 100% indicate that the product is hydrophobic since only water evaporation is occurring, and no absorption from the surface. It is the case of the casein, siloxane, aquashield, and paraffin wax for the adobe specimens. For the rammed earth specimens only siloxane and paraffin wax exhibit values over 100%.
Regarding specifically the water repellents, the synthetic solutions seem to achieve better results, especially, the siloxane. The specimens treated with aquashield showed a particular condition:
heterogeneity in the product distribution on the surface. In the same specimens’ surface, some water droplets were difficult to be placed due to the high hydrophobicity while others were immediately pulled into the surface forming a sort of a bubble bellow the top layer. This effect can be observed in Table 5.2 in the image of the aquashield in the adobe specimen. In the rammed earth, this effect was not so evident, however, there was a clear difference in some droplets on the same surface, some were absorbed, and others evaporated. This dichotomy of the
151 absorption/evaporation effect of the water droplets in the same specimen resulted in a higher standard deviation value for this product and reveals a lack of complete protection against water.
According to the results of microdrops absorption time, both linseed oil and beeswax created a layer that is not hydrophobic, however, when placing the water droplets, a spherical shape was formed that becomes flat after some time, being absorbed in the end. So, it is possible to state that these products do not block the water absorption but delay it. A similar effect was also observed in specimens treated with black soap, but a flatter drop was formed in this case, contributing only to slower water absorption. In the case of the consolidants, no values over 100% were expected, however, the casein in the adobe specimens revealed a high-water repellency level, which can be an important parameter when choosing this product.
Table 5.2: Images captured during the microdrops absorption test. Examples of treated and untreated (reference) specimens of adobe and rammed earth.
Reference (adobe) Arabic gum (adobe) Casein (adobe) Siloxane (adobe)
Aquashield (adobe) Linseed oil (adobe) Beeswax (adobe)
Reference (rammed earth) Arabic gum (rammed earth) Siloxane (rammed earth) Aquashield (rammed earth)
Linseed oil (rammed earth) Beeswax (rammed earth) Paraffin wax (rammed earth)
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Figure 5.3: Results from the microdrops absorption test performed on the adobe specimens with the indication of the average values, standard deviation, standard error (marked in the error bars as well), and the coefficient of variation.
Figure 5.4: Results from the microdrops absorption test performed on the rammed earth specimens with the indication of the average values, standard deviation, standard error (marked in the error bars as well), and the coefficient of variation.
153 5.1.3. Water repellency - Contact angle
Since the contact angle is a test that evaluates primarily water repellents efficiency, two synthetic and two natural water repellent products applied on the adobe specimens were selected. The selection of the natural products was based on the best results obtained from the microdrops absorption test and the contact sponge method test. Both linseed oil and beeswax present the most promising results in terms of water repellency and water absorption. Even though the paraffin wax also presented good results in those mentioned tests, the visual apparency with the creation of a greasy surface was a key factor for not considering it at the same level as the linseed oil and the beeswax.
An example of a water droplet on the surface of the adobe specimens with each product is presented in Table 5.3. These images were recorded by the software of the equipment. The test was also performed on a reference specimen; however, it was not possible to acquire an image or measure the angle since the drops were immediately absorbed by the surface. On the other hand, the treated adobe specimens exhibit drops with a spherical shape, which means that there is a decrease in the solid-liquid attraction forces compelling the water to form this shape instead of being absorbed.
Additionally, looking at the measured angles the efficiency of all products is evident. The final data (exposed in Figure 5.6) is the result of 10 measurements per specimen and 5 specimens per product.
Table 5.3: Images recorded by the software of the equipment during the contact angle test.
Siloxane Aquashield
Linseed oil Beeswax
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Figure 5.5: Contact angle results for the selected adobe specimens with water repellent products with the indication of the average values, standard deviation, standard error (marked in the error bars as well), and the coefficient of
variation.
5.1.4. Water vapor permeability
One of the main concerns during any intervention is to guarantee that the conservation products do not block the natural exchanges between the building material and the environment. To test the permeability of the products applied to the adobe specimens, water vapor permeability test was performed. This test was done only on a selection of products, based on the best results obtained from the water absorption and water repellency experiments. Thus, from the synthetic ones, ethyl silicate, siloxane, and aquashield were selected, and from the natural ones, Arabic gum, linseed oil, and beeswax were tested. All the products were applied on five adobe specimens each, and five additional specimens were taken as reference (with no product applied). The average values were calculated after excluding the outliers and the results are reported in Figure 5.6.
As observed, none of the products significantly reduced the permeability when compared with the reference specimens. The one with higher changes is the linseed oil, with a decrease in the permeability of 22.4% while the one with less variation was the aquashield with a decrease of 6.3%.
These positive results in terms of water vapor permeability from all selected products emphasize the possibility of using them as consolidants and water repellent solutions. Moreover, the natural products exhibit results similar to the synthetic ones, which underlines their possible use in conservation procedures.
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Figure 5.6: Water vapor permeability results in the adobe specimens, with the indication of the average values, standard deviation, standard error (marked in the error bars as well), and the coefficient of variation.
5.1.5. Colorimetric parameters
The measurement of the color before and after the application of treatments over a surface is of paramount importance, especially when dealing with cultural heritage. The values exposed in Figure 5.7 and Figure 5.8 represent the total color difference (ΔE*) between the reference specimens and the treated specimens, for adobe and rammed earth, respectively. According to the literature (Mokrzycki and Tatol 2011), color variation is clear when ΔE* is between 3.5 and 5, and values larger than 5 are considered a visible color change.
Looking at the obtained values, it is interesting to notice the disparity of results between the adobe and the rammed earth specimens, showing how these products have different interactions in each earthen construction technique and soil type. For the adobe specimens, only three products had color variation less than 5 – Arabic gum, siloxane, paraffin wax, ethyl silicate and black soap. All other consolidants and water repellents induced significant variations in terms of color, being the limewash the product with a higher impact. However, in the case of the rammed earth specimens, almost all products produced significant color differences, with limewash, Arabic gum, and casein with the higher values. Linseed oil and paraffin wax presented values of ΔE* smaller than 3.5, having very low color impact on the rammed earth specimens. Looking specifically to the L*, a*, b*
coordinates (reported in Appendix III, p.281) the major differences occur in the L* axis since it indicates the darkening or brightening that the product induces, except for the casein and cactus juice with a higher variation in the b* axis indicating in both cases a change for bluish tone.
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It is important to underline that these results of color impact are specific for the type of soil presented in both techniques, thus it is not a direct conclusion that these products induce significant changes in terms of color in all earthen substrates. The color measurement should be performed every time a new surface treatment is planned to be implemented on cultural heritage. Usually, preliminary tests are carried out on small areas of the surface to understand the interaction and color impact of the products. So, for the present study, even though some products induced high color changes, it will not be considered as a general indicator of the compatibility of the treatment with the earthen construction. Nevertheless, important conclusions can be extrapolated, as the whitish color produced by the limewash on the adobe soil, or the darkening of the surface of the rammed earth specimens caused by the Arabic gum.
Figure 5.7: Color difference (ΔE*) between the reference specimens and each treated specimen (adobe) with the indication of the average values, standard deviation, standard error (marked in the error bars as well), and the coefficient of
variation.
Figure 5.8: Color difference (ΔE*) between the reference specimens and each treated specimen (adobe) with the indication of the average values, standard deviation, standard error (marked in the error bars as well), and the coefficient of
variation.
157 5.2. Compatibility
5.2.1. Microscopic analysis – SEM
Through the SEM equipment, it was possible to observe at a microscopic level the interaction between the applied products and the earthen material. For this test, a set of treated (ethyl silicate, nanoparticles of silica, Arabic gum, siloxane, aquashield, linseed oil, and beeswax) and untreated (reference) adobe specimens were selected. Table 5.4 reports the surface images of the specimens.
As observed, some products produced significant changes at the surface level, while others have much less interference. Comparing with the reference image, the specimens with ethyl silicate, aquashield, and linseed oil apparently did not change their surface roughness or aspect, creating a layer that seems to be compatible in terms of physical and chemical connection with the earthen material. Moreover, the ethyl silicate appears to promote bonding between the loose particles. The images of the Arabic gum and beeswax revealed a clear layer of both products that fill the lower areas of the surface and apparently create a bond with the bigger grain particles. The adobe specimens treated with siloxane do not exhibit an evident layer of product, but the surface looks powdery and less cohesive. The product that produced higher changes in the surface of the specimens was the nanoparticles of silica, demonstrating a distinct layer entirely cracked and without any bonding to the earthen material, fact that supports the high values of water absorption obtained in the contact sponge method test for this treatment.
Additionally, an analysis of the perpendicular side of the samples was conducted to find if there was a clear difference between the product and the earthen material or the penetration level. However, only in the samples with nanoparticles of silica, a distinct layer was observed. In all the other treated specimens it was not possible to have a visual perception as to where the product was in the sample or if there was a well-defined division between product and earth. An example of a captured image of the perpendicular side of a sample with ethyl silicate and with nanoparticles of silica is exposed in Figure 5.9.
Table 5.4: SEM images (magnification of 50x) of the selected adobe specimens.
Reference Ethyl silicate
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Nanoparticles of silica Arabic gum
Siloxane Aquashield
Linseed oil Beeswax
(a) (b)
Figure 5.9: (a) SEM image of the sample lateral side treated with ethyl silicate (magnification of 30x); (b) SEM image of the sample lateral side treated with nanoparticles of silica (magnification of 150x).
159 5.3. Durability
To test the durability of the products on both earthen techniques, all specimens were placed inside the climatic chamber for a period of approximately one year. During this time, the specimens were subjected to cycles of temperature (from -10 °C to 30 °C) and constant relative humidity of 90% to induce accelerated environmental degradation. Each day, four complete cycles were achieved by the climatic chamber.
For a constant evaluation of the specimen’s behavior inside the climatic chamber, three tests were performed as a control system: material loss, contact sponge method, and microdrops absorption time. These tests were conducted, roughly, every two months, and the number of cycles inside the climatic chamber was calculated to present the results according to the induced artificial aging. The number of days and respective cycles are detailed in Table 5.5.
Table 5.5: Timespan in days and cycles between each set of tests.
Days inside the climatic chamber
Number of cycles
Number of cumulative cycles
1st set of tests 0 0 0
2nd set of tests 69 276 276
3rd set of tests 59 236 512
4th set of tests 65 260 772
5th set of tests 66 264 1036
Besides the control tests, at the end of the artificial aging period (1036 cycles), the specimens were removed from the climatic chamber, and tests were repeated (contact angle, water vapor permeability, colorimetric parameters, and SEM). All the results are exposed and discussed in the next sections. Additionally, the visual aspect before, during, and after the artificial aging of all specimens was registered through photographic records that are reported in Appendix II.
5.3.1. Visual inspection and material loss
Visual inspection
The weight of all adobe and rammed earth specimens was measured before, during, and after the accelerated artificial aging process. With this analysis, plus the visual inspection of each specimen, it was possible to draw some conclusions about the appearance or evolution of possible degradation patterns.
In Appendix II this degradation progress can be seen in the photos of the specimens’ top surface (where the products were applied). Nevertheless, some examples of specimens in which the effects of the temperature cycles were more marked are reported in Table 5.6 and Table 5.7.
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Table 5.6: Visual inspection of the degradation progress of some adobe specimens’ overtime during the artificial aging.
0 cycles 276 cycles 512 cycles 772 cycles 1036 cycles
Adobe ReferenceAdobe CaseinAdobe Cactus juiceAdobe AquashieldAdobe Linseed oil
Table 5.7: Visual inspection of the degradation progress of some adobe specimens’ overtime during the artificial aging.
0 cycles 276 cycles 512 cycles 772 cycles 1036 cycles
Rammed earth ReferenceRammed earth LimewashRammed earth Arabic gum