Article in Press: Formulation and Microstructural Evaluation of Tuff Repair Mortar
Article in Press: Formulation and Microstructural Evaluation of Tuff Repair Mortar
Article in Press: Formulation and Microstructural Evaluation of Tuff Repair Mortar
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Original article
Formulation andmicrostructuralevaluationoftuffrepairmortar
Lidija Korata,∗, Breda Mirticˇb, Ana Mladenovicˇa, Alenka Mauko Pranjic´ a, Sabina Kramara
ar ti cl e i nf o a bs tr ac t
Article history: The purpose of this study was to develop a compatible repair mortar for two lithotypes of Peracicaˇ tuff (Slovenia): fine-grained and
Received 10 January 2014 coarse-grained. Mineralogical–petrographic characterization of tuff was carried out via optical microscopy and X-ray powder
Accepted 11 November 2014 Available online diffraction, and the relevant physical–mechanical properties of tuff and repair mortars were determined: capillary water absorption,
xxx water absorption at atmospheric pressure, open porosity, compressive strength and resistance to salt crystallization. A repair mortar
was prepared by mixing crushed Peracicaˇ tuff and quartz sand, with different grain size and mass ratios, and ethyl silicate (KSE 500
STE, Remmers) as a binder. The results showed that with an appropriate combination of crushed tuff, quartz sand and ethyl silicate, a
Keywords: compatible repair mortars can beobtained
Tuff
Repair mortar
a
Slovenian National Building and Civil Engineering Institute, Dimicevaˇ 12,1000 Ljubljana, Slovenia b University of Ljubljana, Faculty of
Natural Sciences and Engineering, Department of Geology, Askerˇ cevaˇ 12,1000 Ljubljana, Slovenia
Silica-based mortars
Microstructure for both lithotypes.
Deterioration
© 2014Elsevier Masson SAS. All rights reserved.
E-mail addresses: [email protected] (L.Korat), [email protected] (B.
Mirtic),ˇ [email protected] (A. Mladenovic),ˇ [email protected] (A.M. Pranjic),´
[email protected] (S.Kramar).
Please cite this article in press as: L. Korat, et al., Formulation and microstructural evaluation of tuff repair mortar, Journal of Cultural Heritage (2014),
http://dx.doi.org/10.1016/j.culher.2014.11.002
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Please cite this article in press as: L. Korat, et al., Formulation and microstructural evaluation of tuff repair mortar, Journal of Cultural Heritage (2014),
http://dx.doi.org/10.1016/j.culher.2014.11.002
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Fig. 1.Two types of Peracicaˇ tuff from the Bogataj (c and d) and Crnivecˇ (a and b) quarries.
The heterogeneous coarse-grained tuff is also mainly light green in matrix is cryptocrystalline.
color, corresponding to light greenish gray (5G 8/1) on the Rock Color According to X-ray powder diffraction results (Fig. 3a and b),
Chart. Smaller grains (1–3 mm) are darker in color and can be divided quartz and plagioclase feldspars are the most abundant phases in both
into two groups: pale green (10G 6/2) and grayish green (5G 5/2). tuff lithotypes, followed by alkali feldspars, illite/muscovite and
Occasional dark fields of smaller inclusions are also present, while analcime. These results are in accordance with those obtained in
open pores, subsequent filling and cracks are macroscopically not [31,32] and are in agreement with similar tuffs examined elsewhere
observed. In some areas a slight grain orientation is noticeable. This [1,33]. Pyrite, chlorite (chlorites group of phyllosilicate minerals) and
welded vitric tuff consists mostly of grains between 2 mm and 3 mm in carbonate levels were beyond the X-ray detection limits; these
size, together with pumice embedded within the matrix. Grains of minerals could only be recognized under the optical microscope. No
quartz are again predominant, most of which are xenomorphic, with significant differences in XRD peaks between the lithotypes were
some idiomorphic. The average quartz grain size is 300 m. Individual observed. As can be seen from Table 3, the major difference between
grains of plagioclase (Fig. 2b) with an average size of 500 m are also tuff lithotypes is in quantity of amorphous phase and in the presence of
observable. Among the femic minerals individual grains of biotite are quartz, where quartz is enhanced in fine-grained tuff and amorphous
present, although in some spots alteration of biotite to chlorite has phase level is smaller than in coarse-grained tuff. In addition, analcime
taken place. The husks of chlorite (chlorites group of phyllosilicate was found in both tuff lithotypes as a consequence of sedimentation
minerals) are located in a group of individual bands and exhibit the processes of volcanic material in aquatic environment [31,34] or
influence from hydrothermalfluid activity [31,33–36].
Composition of the selected mixtures, where t: tuff, q: quartz sand, A: fine-grained tuff, B: coarse-grained tuff and KSE (500 STE): ethyl silicate binder.
Samples Tuff Tuff Tuff Tuff Quartz sand Binder (mass %)
< 63 m (mass %) 63–125 m (mass %) 125–250 m (mass %) 250–500 m (mass %) 63–125 m (mass %)
3t B 6 15 3 6 / 10
4t B 6 6 12 6 / 10
5t B 6 3 15 6 / 10
4t A 6 6 12 6 / 10
1q A 6 6 6 3 9 11
1q B 6 6 6 3 9 11
Table 2
Water absorption, open porosity and compressive strength properties of the two Peracicaˇ tuffs
lithotypes and the developed repair mortars.
Tuff Mortar
Open porosity (wt%) 20.6 0.4 19.7 0.4 39.7 2.8 35.2 1.9 34.0 2.5 34.1 1.3 33.4 1.4 36.8 0.9
± ± ± ± ± ± ± ±
Water absorption coefficient by capillarity 25.5 ± 2.4 28.1 ± 1.5 53.6 ± 8.9 39.8 ± 1.8 36.8 ± 4.1 36.9 ± 3.1 37.5 ± 2.8 45.8 ± 3.5
(gm−2s−0.5)
Please cite this article in press as: L. Korat, et al., Formulation and microstructural evaluation of tuff repair mortar, Journal of Cultural Heritage (2014),
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Fig. 2. Microphotograph of the two tuff lithotypes (fine- and coarse-grained), where (a) is fine-grained tuff with a chlorite (Cl) grain and matrix (m), (b) is coarse-grained tuff with a
plagioclase (Pl) grain, (c) is fine-grained tuff with a plagioclase (Pl) grain, and (d) is coarse-grained tuff with a carbonated (C) plagioclase (Pl) grain.
Fig. 3.The results of X-ray powder diffraction, where (a) is fine-grained tuff (A), (b) is coarse-grained tuff (B).
The SEM-EDS analyses were performed in order to complement were reconfirmed also by the X-ray diffraction method. Also X-ray
the data of both lithotypes of Peracicaˇ tuff. The findings in both tuff diffraction reconfirmed the SEM-EDS analyses of higher amounts of
lithotypes revealed and confirmed by distribution of elements quartz in the finegrained tuff. The coarse-grained tuff contains larger
determined by SEM/EDS high amounts of Si, Al, Na or Ca, indicating matrix content and amounts of amorphous phase, a pattern in
plagioclase feldspars minerals, which were reconfirmed by the X-ray accordance with samples analyzed by Kastelic [31]. Also we can
diffraction method. The SEM-EDS analyses have determined the confirm with results from X-ray powder diffraction and in accordance
presence of felsic and mafic plagioclases. Also, both tuff lithotypes, with classification in the QAPF diagram for volcanic rocks andsamples
beside contain high amounts of Si, and Al, also contained K, which analyzed by Kastelic [31], the Peracicaˇ tuffs have a dacite
indicates alkali feldspar minerals. Besides feldspars minerals both tuff composition.
lithotypes contain illite/muscovite, chlorite content and pyrite. 3.2. Openporosity oftuff andmortar
Analcime crystals are well defined in the matrix and observed by SEM-
EDS analyses, higher amounts are present in fine-grained tuff, which Openporosity valuesrangedfrom19.7 to 20.6wt% for tuff and
Table 3
The results of X-ray powder diffraction, crystalline and amorphous composition of two tuff lithotypes (A: fine-grained tuff, B: coarse-grained tuff) by Rietveld method.
Quartz/% Plagioclase feldspars/% Illite/muscovite/% Analcime/% Alkali feldspars/% Amorphous/%
Please cite this article in press as: L. Korat, et al., Formulation and microstructural evaluation of tuff repair mortar, Journal of Cultural Heritage (2014),
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The results of the water absorption by capillary rise tests for all
tuff and repair mortar samples are reported in Table 2, with the
3.4. Water absorption at atmospheric pressure oftuff andmortar
respective capillary absorption curves presented in Fig. 4. Values
of the capillary absorption coefficient were quite similar in both of
The results of the water absorption tests at atmospheric pressure are
the investigated tuff lithotypes, varying from 25.5gm−2s−0.5 for
shown in Table 2. Analysis of this table shows that water absorption at
fine-grained to 28.1gm−2s−0.5 for coarse-grained tuff.
atmospheric pressure of the investigated tuff samples varied from 8.3
wt% for fine-grained to 8.0wt% for coarse-grained tuff.
Values of the capillary absorption coefficient for the The obtained water absorption data positively correlate with both
investigated repair mortars ranged from 36.9 to 53.6gm−2s−0.5 the open porosity and coefficient of capillarity results, since the higher
(Table 2). The the porosity and coefficient values the greater the water absorption.
The water absorption at atmospheric pressure of the investigated repair
mortars ranged from 14.5 to 22.8 wt%. Among the tested repair
mortars, sample 3tB had the highest absorption and sample 1qB the
highest level of water absorption by capillary rise was exhibited by lowest. Repair mortar sample 1qB exhibited the lowest water
sample 3tB and the lowest by samples 5tB and 4tA. This pattern can absorption value, similar to that of coarse-grained tuff. The
be explained by sample microstructure, with 3tB comprising more investigated fine-grained tuff presented higher values of water
grains smaller than 125 m. The presence of smaller grains thus absorption, resulting in sample 1qA exhibiting greater absorption than
increases capillary absorption in the repair mortars, especially sample 1qB, in which coarse-grained tuff was used in the aggregate.
those composedofgrains smaller than 125m. The opposite situation was again observed in the case of samples 4tB
As can be seen from the above results, the recorded open and 4tA. Nevertheless, it is clearly evident that a higher quantity of the
porosity values positively correlate with those for capillary rise, coarse-grained fraction reduces water absorption, as finer material
with the higher the coefficient the greater the porosity. It is well produces more channels for water penetration.
known that finer pores lead to a higher coefficient of capillarity
Fig. 5.Tuff samples in the process of salt crystallisation (length, width, height: 40 × 40 × 40 mm).
Please cite this article in press as: L. Korat, et al., Formulation and microstructural evaluation of tuff repair mortar, Journal of Cultural Heritage (2014),
http://dx.doi.org/10.1016/j.culher.2014.11.002
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Fig. 6.Repair mortar samples in the process of salt crystallisation (height, radius: 40 mm, 15 mm).
3.5. Compressive strength of tuff and mortar positively correlated with both the capillary absorption coefficient
and water absorption tests, with the higher the mortar porosity the
The results achieved after 60 days of compressive strength tests are greater the coefficient and water absorption values. The addition of
shown in Table 2. As can be seen from this table, values ranged from quartz sand and a higher quantity of the coarse-grained fraction
72.0 MPa for coarse-grained tuff to 85.8 MPa for fine-grained tuff. This thus both reduced water absorption.
range likely reflects differencesin sample microstructure, with coarse- In conclusion, on the basis of the data of salt crystallization, the
grained tuff containing a greater volume of matrix (as well as open most compatible among the repair mortars were sample 5tB, which
porosity). contained an aggregate of tuff and binder, and repair mortar 1qB,
The developed repair mortars exhibited compressive strength which contained an aggregate of tuff, quartz sand and binder.
levels between 3.7 and 8.0 MPa. A repair mortar with fine-grained tuff Whereas mortar sample 5tB exhibited reduced absorption of water
exhibited lower compressive strengths than that with coarsegrained by capillary rise and lower compressive strength, mortar 1qB
tuff aggregate. In particular, this is observed at repair mortars 4tB and presented lower levels of both water absorption at atmospheric
4tA. Samples 1qA and 1qB have fairly similar compressive strength pressure and open porosity. In addition, the samples that seem to
valuesdue to their similar compositions of added quartz sandfraction. exhibit the best physical–mechanical properties (such as capillary
water absorption and compressive strength) are repair mortars 1qB
3.6. Salt crystallization of tuff and mortar and4tB.
Tuff deterioration is a major global problem and thus the
The results of the resistance to salt crystallization tests revealed that development of appropriate repair mortars will be beneficial not
the tuff samples underwent visible change no earlier than the 11th only for Slovenia but also for other countries worldwide. The
exposure cycle, when the surface of the stone began to degrade present study can hopefully contribute to the better conservation
(although not yet fully disintegrated; Fig. 5). The tuff samples treatment of tuff-based sculpturesandbuildings.
deteriorated via the loss of material, with the eventual complete
collapse of the specimens after exposure to salt solution occurring after Acknowledgements
15 cycles. During this process, all samples lost their green color. The
fine-grained tuff samples fissured along their edges and the external This research was supported financially by the Slovenian
surfaces were subjected to scaling. Due to the complete failure of the Research Agency (Grant No. 1000-10-310085). Many thanks go
specimens, it wasimpossible to calculate an accurate weight loss value. to Matej Dolenec (University of Ljubljana, Faculty of Natural
The results of salt crystallization tests for the investigated repair Sciences and Engineering, Department of Geology) for help with
mortars are shown in Fig. 6. During the testing process the repair mortar X-ray diffraction and to Nastja Rogan Smucˇ (University of
samples also gradually deteriorated and by the end of the cycles had Ljubljana, Faculty of Natural Sciences and Engineering,
been completely demolished. The first visible changes were observed DepartmentofGeology) for help with thin sections.
at the 5th cycle, with the loss of stone at the sample edges. Sample 4tA
broke up at the 7th cycle and also at the 10th cycle. Samples 3tB and 1qA References
broke up at the 11th cycle, two samples of mortar 5tB at the 13th cycle,
and1qB and5tB (again) at the 14th cycle (Fig. 5). [1] C.D. Vacchiano, L. Incarnato, P. Scarfato, D. Acierno, Conservation of tuff-
stone with polymeric resins, Constr.Build. Mater. 22 (2008) 855–865.
[2] M.J. Varas, M. Alvarez de Buergo, E. Perez-Monserrat, R. Fort, Decay of the
4. Conclusions restoration render mortar of the church of San Manuel and San Benito, Madrid,
Spain. Results from optical and electron microscopy, Mater. Charact. 56 (2008)
1531–1540.
The main difference between the investigated fine- and [3] O. Rolland, P. Floc’h, G. Martinet, V. Vergès-Belmin, Silica bound mortars for
coarsegrained tuff is microstructural, with the former containing a the repairing of outdoors granite sculptures, in: Proceedings of 9th International
greater amount of quartz and lower amounts of amorphous phase. The Congress on deterioration and conservation of natural stone, Venice, vol. 2,
2000,pp.307–315.
coarse-grained tuff also comprises a lower volume of plagioclase and a
[4] H. Leisen, E. Plehwe-Leisen, S. Warrack, Success and limits for stone repair
larger proportion of matrix material. mortars based on tetra ethyl silicate-conservation of the reliefs at Angkor Wat
The repair mortars containing quartz sand were characterized Temple, Cambodia, in: 12th Triennal Meeting ICOM Committee for
by lower open porosity levels, as were those subject to the addition Conservation, Lyon, 2000, pp. 737–742.
Please cite this article in press as: L. Korat, et al., Formulation and microstructural evaluation of tuff repair mortar, Journal of Cultural Heritage (2014),
http://dx.doi.org/10.1016/j.culher.2014.11.002
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Please cite this article in press as: L. Korat, et al., Formulation and microstructural evaluation of tuff repair mortar, Journal of Cultural Heritage (2014),
http://dx.doi.org/10.1016/j.culher.2014.11.002