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Journal of African Earth Sciences 55 (2009) 1–9

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Journal of African Earth Sciences


journal homepage: www.elsevier.com/locate/jafrearsci

Petrophysical behaviour and durability of the Miocene sandstones


used in the architectural heritage of Tunisia (Roman aqueduct
of Oued Miliane and Uthina Roman site)
K. Zoghlami a,*, D. Gómez-Gras b
a
Université de Carthage, Faculté des Sciences de Bizerte, Département de Géologie, Tunisia
b
Universidad Autónoma de Barcelona, Departamento de Geología, Spain

a r t i c l e i n f o s u m m a r y

Article history: In the present work, the relationship between intrinsic factors, mechanical properties and durability of
Received 29 June 2006 Miocene sandstones used in the architectural heritage of Tunisia, specifically in the Roman aqueduct
Accepted 11 December 2008 of Oued Miliane and Uthina site, are studied. The petrographic study and the characterisation of porous
Available online 9 April 2009
network have been carried out using optical microscopy, mercury intrusion porosimetry and laser scan-
ner confocal microscopy (LSCM). The hygric behaviour has also been determined from water absorption
Keywords: under vacuum, drying, capillary water absorption and water vapour permeability. The mechanical prop-
Sandstone
erties have been assessed from compressive strength and abrasion tests. Rock durability has been eval-
Petrographic characteristics
Hygric and mechanical properties
uated from salt crystallization (sodium sulphate) accelerated aging tests. The results show good hygric
Durability behaviour characterised by a high evaporation rate and almost no retention of water; due to the macro-
Oued Miliane aqueduct porous character of the rock and the good connectivity of the pore network. Because of the poor lithifi-
Uthina Roman site cation, the stone has a very low mechanical strength which makes it very vulnerable to the salt
crystallization effects. The absence of chemically unstable minerals preserves the rock from chemical
alteration. The durability of the building stone is mainly conditioned by salt loading of the monument.
Ó 2009 Elsevier Ltd. All rights reserved.

1. Introduction and aim of the research of this monument present some degradation forms (Cara et al.,
2002). The aim of the present work is the study of the physical
This research is focused on the study of sandstone outcropping behaviour and durability of the sandstone in order to establish cri-
in the north-east of Tunisia which belongs to the Fortuna Forma- teria for the selection of appropriate building stone to be used for
tion (upper Oligocene–lower Miocene; Yaich, 1992), specifically restoration of the Tunisian monuments, particularly with regards
to its fluvial–continental facies of Aquitanian–Burdigalian age to Oued Miliane aqueduct and Uthina Roman site.
(Gómez-Gras et al., 2004). The interest on this type of rock lies in
the fact that it has been frequently used in the architectural heri- 2. Results and discussion
tage of Tunisia (i.e. the Oued Miliane aqueduct and Uthina Roman
site) and its potential use in restoration or intervention works. The The petrography and the porous system of the rock have been
aqueduct of Zaghouan–Carthage is about 132 km long, the largest studied by means of optical microscopy, mercury intrusion poros-
of all the Roman Empire, and represents the most important Ro- imetry, and laser scanner confocal microscopy (LSCM). Studies on
man work in Africa. Most of the aerial constructions (17 km) are hygric behaviour (water absorption and desorption), swelling and
found in the valley of Oued Miliane (Rakob, 1979; Fernández Casa- salt crystallization tests as well as the determination of mechanical
do, 1983). This part shows a critical state of decay mainly due to properties and abrasion were carried out according to RILEM
structural reasons (instability problems, presence of fissures and (1980) and NORMAL (1981, 1985, 1988) recommendations and
cracks) coupled with a weak disintegration of the rock. Uthina city to UNE standards (1995, 1999).
is located 30 km to the south of Tunis and occupies a surface area
of 100 ha. It was founded in the first half of the first century AD and 2.1. Geological setting
is one of the best preserved Roman sites in Africa. Nevertheless, the
Miocene sandstones that constitute most of the building materials The Oligo-Miocene deposits of the central and north-eastern
areas of Tunisia (Fig. 1) are essentially detritic and are constituted
* Corresponding author. Tel.: +216 21155880. by the Fortuna, Messiouta, Grijima and Ain Grab Formations. The
E-mail address: karimazoghlami@hotmail.com (K. Zoghlami). rocks are Oligocene to Langhian in age. They originate from depo-

1464-343X/$ - see front matter Ó 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jafrearsci.2008.12.003
2 K. Zoghlami, D. Gómez-Gras / Journal of African Earth Sciences 55 (2009) 1–9

Fig. 1. Location map.

sition in deltaic to shallow marine or coastal environments (Yaich, vy minerals (tourmaline and zircon) (Gómez-Gras et al., 2004).
1992; Yaich et al., 2000). The modal analyses (Table 1) are obtained by point-counting
The Fortuna Formation has been subdivided into three units of 28 thin-sections of sandstone sampled from the Roman quar-
(Fig. 2). The lower unit is lower Rupelian to lower Chatian in age ries (Level 3 of stratigraphic section) according to Gazzi–Dickin-
(upper Oligocene), and the middle unit is Aquitanian in age (lower son’s method (Ingersoll et al., 1984). Four lithotypes were
Miocene). They are mainly composed of fine sandstones and lutites distinguished:
with interstratified calcareous layers. The upper unit crops out in
the north-eastern part of Tunisia, where this work has been carried 1. Clay-free, extremely to very well-sorted fine-grained sandstone
out (Figs. 1 and 3). It has a thickness of 130 m and includes fine to (Fig. 4A),
coarse-grained sandstones with dispersed boulders of quartz 2. Clay-containing, extremely to very well-sorted fine-grained
deposited in a braided fluvial environment (Gómez-Gras et al., sandstone (Fig. 4B),
2004). Roman quarries located in this unit provided most of the 3. Clay-free, moderately sorted medium-grained sandstone,
material for the construction of the Uthina Roman site and the 4. Clay-containing moderately sorted medium-grained sandstone.
Oued Miliane aqueduct (Fig. 3).
In all sandstone lithotypes cement is scarce and lithification of the
2.2. Petrographic study rock is mainly due to mechanical and chemical compaction. The
degree of compaction has been obtained subtracting the final inter-
These sandstones are quartzarenites (Fig. 4A) mainly com- granular volume value (final VIG) from the initial intergranular
posed of monocrystalline quartz (69–84%) and K-feldspar (0– volume value (initial VIG), as deduced from Beard and Weyl values
1%, orthoclase and microcline). infiltrated clay matrix (0– (1973) (Zoghlami et al., 2004a). Fine-grained sandstones are more
10.2%), essentially mixed layer of illite–smectite and kaolinite. lithified than coarse-grained sandstones due to the larger number
Fragments of plutonic (granitoids), metamorphic (quartzites) of grain contacts, greater pressure dissolution area and the greater
and sedimentary (sands cemented by quartz) rocks appear as intergranular volume compaction loss (compacted VIG) of the fine-
accessories, together with mica (muscovite and biotite) and hea- grained sandstones (Table 2).
K. Zoghlami, D. Gómez-Gras / Journal of African Earth Sciences 55 (2009) 1–9 3

Fig. 2. Geological map and stratigraphic section of the studied area.

2.3. Study of porous network show that pore sizes in fine-grained sandstones range from 50–60
to 120 lm. In the medium-grained sandstones, the main pore size
Effective porosity of the rock, determined by mercury intrusion amounts to about 200 lm on average, reaching up to 600 lm at
porosimetry, shows high values (17.50–25.86%). Macroporosity maximum (Fig. 6A and B).
(pore diameter >15 lm, according to Goñi et al. (1968) and Bous- The 3D reconstruction of the porous network (Fig. 6C and D)
quié et al. (1980) represents a percentage of 82.34–85.52%, illustrates it is made of a single pore system whose configuration
whereas microporosity ranges from 12.82% to 14.65%, which is only depends on grain arrangements and degree of compaction.
indicative of the sandstone’s macroporous character (Table 3). The porous network is constituted by channels (<40 lm in diame-
Variations in porosity and average pore diameter values are related ter) that may occasionally expand, giving rise to megapores, with
to the presence of clay minerals, sorting and degree of compaction diameters up to 300 lm in case of the fine-grained sandstone
(Zoghlami et al., 2004a). The presence of a clay matrix increases the and up to 600 lm for the coarse-grained sandstones.
microporosity values and especially the infraporosity (Table 3). In The combined data from LSCM and mercury intrusion porosi-
samples with similar petrographic features, the presence of clay metry has allowed proving that porosity is present as large pores
minerals reduces the pore size access, as can be observed by com- which are interconnected by channels that constitute pore acces-
paring the pore size distribution in the clay-free and clay-contain- ses. Although of smaller size with respect to the main pores, these
ing samples (Fig. 5A and B). pore accesses are still large (10–40 lm).
Mercury porosimetry results show that most of the pores
(>80%) have a pore access diameter in the range of 10–40 lm, 2.4. Hygric behaviour
depending on grain size, sorting and clay content of the rock. The
rest of the pores (<20%) present a diameter pore access of less than Hygric tests have been carried out on seven samples repre-
15 lm (micropores). senting the different lithotypes previously described. Data in Ta-
As mercury porosimetry only measures pore access, real pore ble 4 correspond to the more significant values of the hygric
size was measured using LSCM (Zoghlami et al., 2004b). The results parameters.
4 K. Zoghlami, D. Gómez-Gras / Journal of African Earth Sciences 55 (2009) 1–9

Fig. 3. Upper unit stratigraphic section of Fortuna Formation.


K. Zoghlami, D. Gómez-Gras / Journal of African Earth Sciences 55 (2009) 1–9 5

Fig. 4. Microphotographs showing some details of the studied sandstones. (A) Clay-free sandstone, scale 400 lm. (B) Clay-containing sandstone, scale 400 lm.

Table 1 Table 2
Petrographic characteristics of sandstone tested samples. Grain size, compactness and compressive strength.

Components (%) Fine-grained Medium-grained Values Fine-grained sandstones Coarse-grained sandstones


sandstones sandstones (mean grain size: (mean grain size:
0.210 mm) 0.420 mm)
Quartz Mean 73.9 Mean 76.08
Max 84 Max 71.6 Pressure- Mean 53.20 20.22
Min 69 Min 81.2 dissolution Max 61.35 22.64
K-feldspar Orthoclase Mean 0.5 Mean 0.23 seams (%) Min 49.6 18.6
Microcline Max 1 Max 0 Number of Mean 24 8
Min 0 Min 0.7 contacts Max 29 12
Rock fragments Plutonic Mean 0.85 Mean 1.83 Min 20 6
Metamorphic Max 1.7 Max 5.5 Initial VIG (%) Mean 41.3 34.2
Sedimentary Min 0 Min 0.2 Max 42.4 34.6
Clay-matrix Mean 4.25 Mean 4.5 Min 40.80 34
Max 10.2 Max 9.2 Final VIG (%) Mean 27.5 23.9
Min 0 Min 0 Max 28.4 24.90
Cement ferruginous Mean 0.1 Mean 0.1 Min 27.64 22.32
Max 0.2 Max 0.3 Compacted Mean 13.4 10.9
Min 0 Min 0 VIG (%) Max 14 11.2
Micas Biotite Mean 0.23 Mean 0.1 Min 12.86 10.7
Muscovite Max 0.5 Max 0.3 Compressive Mean 19.84 4.9
Min 0 Min 0 strength Max 24.32 5.49
Heavy minerals Tourmaline Mean 0.1 Mean 0.08 (MPa) Min 15.69 4.32
Zircon Max 0.4 Max 0.2
Min 0 Min 0
Sorting Moderately to Moderately to well-
extremely-sorted sorted The observed variation in the capillary water absorption curves
is due to the variable presence of clays (0–10.2%). Clays partially or
completely plug the smaller pore accesses causing a decrease in
The porosity (P) and the saturation coefficient (Ws) can be con- the connectivity of the pore network and a reduction in the flux
sidered as very high. The water absorption capillary coefficient (C) of water absorption.
is also elevated as indicated by the curves of capillary water With respect to dry kinetics, the critical water content values
absorption (Fig. 7). The capillary saturation degree (Si) is very high, (Wc), were found to be very low. This explains the high evaporation
accounting for more than 80% of the amount of absorbed water un- rate (Fig. 8), since nearly all the water in the capillaries evaporates
der vacuum, which is indicative of the excellent connectivity of the at the rock surface. These values are also indicative of good connec-
pore network of this sandstone. tivity of the pore network.

Table 3
Sorting, clay content and porosity properties (mercury intrusion porosimetry).
a b c
Samples Values Total porosity (%) Macro-porosity (%) Micro-porosity (%) Infra- porosity (%) Average diameter (lm) Mode (lm)
Clay-containing samples Mean 19.24 82.21 14 14 3.65 10–20
Max 20.80 82.52 14.32 14.32 4.22
Min 17.50 81.68 13.35 13.35 3.37
Clay-free samples Mean 24.39 85.89 12.24 12.24 1.74 20–30
Max 25.86 89.18 14.65 14.65 1.93
Min 22.35 83.47 8.65 8.65 1.36
a
Macroporosity: pore diameter > 15 lm.
b
Microporosity: pore diameter < 15 lm.
c
Infraporosity: pore diameter < 0.1 lm.
6 K. Zoghlami, D. Gómez-Gras / Journal of African Earth Sciences 55 (2009) 1–9

The water vapour permeability is high, as shown by the values


of the respective coefficient (d) given in Table 5; this is consistent
with the results on pore network connectivity described above. The
values differences are due to the variable presence of clays (0–
10.2%) which partially obstruct the throats, modifying the configu-
ration of the pore network and reducing connectivity (Zoghlami
et al., 2004a; López de Azcona et al., 2002; Veniale et al., 2001;
Zoghlami et al., 2005).
Results obtained from swelling test show hygric expansion in
the sandstones to be extremely low, despite the presence of int-
erstratified illite–smectite clay minerals in the samples detected
by XRD.

2.5. Mechanical behaviour

Results gathered from compressive strength (UNE-EN, 1999)


and abrasion (UNE-EN ISO, 1995) tests of the sandstone are shown
in Table 6 for samples with different grain sizes.
Strength and abrasion values vary in dependence on grain size.
Strength of the medium-grained sandstones is lower compared to
the finer-grained, more lithified sandstones. Correspondingly,
abrasion on the medium-grained sandstone is higher than on the
fine-grained sandstones.
Fig. 5. Porosity distribution deduced from mercury porosimetry. (A) Clay-free
sandstone, (B) Clay-containing sandstone. 2.6. Durability

The durability has been studied using the salt (sodium sulphate)
The water content after evaporation (Se) was very low, indicat- crystallization test (RILEM, 1980; Warker and Smith, 2000). An in-
ing that there is almost no retention of water. This characteristic crease of weight during the first cycle can be observed in Fig. 9,
feature of such sandstones results from the high connectivity, which may be related to the crystallization of thenardite within
demonstrated with 3D reconstruction, and the total absence of the pores.
any cementing material.

Fig. 6. LSCM image. (A) General aspect of the sandstone porosity. Scale bar: 80 lm. (B) Detailed image of pores (real size of pores). Scale bar: 40 lm. (C) 3D reconstruction of
the porous network. Scale bar: 40 lm. (D) Pore detail. Scale bar: 40 lm.
K. Zoghlami, D. Gómez-Gras / Journal of African Earth Sciences 55 (2009) 1–9 7

Table 4
Hygric parameters obtained from different sandstone lithotypes.

Petrographic characteristics Values Parameters


P (%) Ws (%) C (kg/m2 s0.5) Si (%) Se (%) Wc (%)
Clay-free grained sandstones Mean 25.05 12.70 0.71 82.57 0.59 3.64
Max 25.42 12.86 0.740 83.13 0.73 3.81
Min 24.59 12.61 0.682 82.10 0.47 3.42
Clay-containing (5–10%) grained sandstones Mean 19.80 9.32 0.125 74.58 1.20 2.17
Max 21.15 10.11 0.149 76.16 1.55 2.57
Min 18.45 8.53 0.100 73.00 0.85 1.76

P: accessible porosity; Ws: water saturation under vacuum; C: water capillary absorption coefficient; Si: capillary saturation degree; Se: final water content at the end of the
dry process; Wc: critical water content.

Table 6
Mechanical properties.

Samples Values Linear abrasion Samples Compressive


(mm) strength (MPa)
Fine-grained Mean 36.70 Mean 19.85
sandstones Max 36.85 Max 24.32
Min 36.48 Min 15.69
Medium-grained Mean 50.01 Mean 4.91
sandstones Max 50.08 Max 5.49
Min 49.94 Min 4.32

Fig. 7. (Sandstone lithotypes). Capillarity water absorption curves.

Fig. 9. Weight-loss during salt weathering test.

During the second cycle of crystallization, the thenardite to


mirabilite hydration (Iñiguez Herreno, 1961; Domaslowski et al.,
1982; Arnold and Kueng, 1985; Alonso, 1986; Arnold and Zehen-
der, 1989; Martín Pérez, 1990) is accompanied by a partial sanding
in the outermost layers of the samples, facilitating the disintegra-
tion of the external surface (Fig. 10A and B).
Fig. 8. (Sandstone lithotypes). Water desorption curves. We: specimen water
Because of their greater degree of lithification and absence of
content; t: time.
sedimentary laminations, the fine-grained samples better resisted
salt attack. Samples of medium to coarse grain size collapsed at
the end of the fourth cycle. In addition, when lamination was pres-
Table 5 ent, samples tended to split and flake along these anisotropies dur-
Water vapour permeability. ing the second and third immersion cycles. This is due to the
Petrographic characteristics a
d (10 9
) (kg/m s Pa) disruptive forces resulting from the accumulation of salts (thenar-
dite) following the discontinuities. The weakness showed by the
Clay free fine-grained sandstones Mean 61.19
Max 68.80 laminated sandstones, particularly when the grains were coarse,
Min 54.52 is due to their lesser bonding cohesion. The presence of clays also
Clay-containing fine-grained sandstones Mean 38.12 favours the decay as they increase the microporosity. However,
Max 41.28 this feature seems to have a smaller effect on durability than the
Min 33.55
grain size and the presence of laminations (López de Azcona
a
Coefficient of water vapour permeability. et al., 2002; Veniale et al., 2001).
8 K. Zoghlami, D. Gómez-Gras / Journal of African Earth Sciences 55 (2009) 1–9

Fig. 10. Forms of decay in studied sandstone. (A) Aspect of samples during the first cycle of salt crystallisation test. (B) Photo showing surface disintegration during the fourth
cycle of salt crystallisation test.

Several authors relate the intensity of rock decay to the micro- Arnold, A., Kueng, A., 1985. Crystallization and habits of salt efflorescence on walls.
Part one: Methods of investigation and habits. In: Fifth International Congress
porosity values (Grossi and Esbert, 1994; Ordoñez et al., 1997; Fort
of Deterioration and Conservation of Stone, Lausanne, Suiza, pp. 255–267.
et al., 2002) and to the size of pores, since the smaller the pore size Arnold, A., Zehender, K., 1989. Salt weathering on monument. The conservation of
the more aggressive the decay (Luxán and Dorrego, 2004). Given monuments in the mediterranean basin. In: Proceedings of the First
the low microporosity and the high pore size of the studied sam- International Symposium, Bari, Italy, pp. 31–58.
Beard, D.C., Weyl, P.K., 1973. Influence of texture on porosity and permeability of
ples (Table 3), the weak rock resistance to salt weathering is attrib- unconsolidated sand. American Association of Petroleum Geologists Bulletin 57,
uted to the absence of cementing phases, the sparse cohesion 349–369.
between the rock components and the low compactness Bousquié, P., Pellerin, F.M., Struillou, R., Arnould, M., 1980. Contribution de la
porosimetrie au mercure a l’etude de quelques proprietes de roches
coefficient. carbonatees. In: Wolters, R., (Ed.), Materials and Engineering Geology, vol. 22.
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Cara, S., Carcangiu, G., Massidda, L., Meloni, P., Sanna, U., Tamanini, M., 2002. I
3. Conclusion
materiali da costruzione: caratterizzazione archeometrica dei lapidei e delle
malte. In: Askòs (Ed.), Scavi archeologici ad Uthina (1995–2001). Rapporto
The integration of petrographic studies with hygric, mechanical preliminare dell’attività di ricerca dell’Institut National du Patrimoine di Tunisie
dell’Università di Cagliari. Italia, Cagliari, pp. 123–142.
and durability tests has shown that the decay of the studied stone
Domaslowski, W., Kozaneccka, O., Krauze J., 1982. La conservation préventive de la
can only be attributed to mechanical processes. Several factors lead pierre. UNESCO, XVIII, Paris.
to the prevention of any chemical alteration of the rock: the over- Fernández Casado, C., 1983. Ingeniería hidráulica romana. Ed. Colegio de Ingenieros
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