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Study of consolidation effects in carbonate

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6th International Symposium on the Conservation of Monuments in the Mediterranean Basin, Lisbon, Portugal, April 7-10, 2004

STUDY OF CONSOLIDATION EFFECTS IN CARBONATE STONES BY MEANS OF

DRILLING RESISTANCE
Ana Paula Ferreira Pinto*
Jos Delgado Rodrigues**
* Instituto Superior Tcnico, ICIST, 1096 Lisboa Codex, Portugal
** Laboratorio Nacional de Engenharia Civil, 1799 Lisboa Codex, Portugal
ABSTRACT
This paper presents some examples of recent experiences carried out with a portable
instrument, the DRMS device (Drilling Resistance Measurement System), for the assessment of
consolidation performance. This method has been utilized successfully on the study of
consolidation effect of some commercial products when applied on carbonate stones and was
one of the methods extensively used both for characterization of the effectiveness and to
monitor the evolution of treated stones subject to natural exposure. The results prove the
potential and indispensability of this new tool on the study of consolidation treatments.
KEY WORDS
Carbonate stones, consolidation, drilling resistance, penetration depth.

INTRODUCTION
Strength parameters are currently used in the study of stone materials, since they are essential
to understand their properties, decay processes and conservation actions. Several tests for
strength evaluation are used in most research and testing laboratories, such as compression and
bending tests, and hardness tests (Delgado Rodrigues et al., 2002). With few exceptions, these
methods operate in lab conditions and are not suitable for field use. For instance, compression
and bending tests are destructive, require large amounts of material and cannot be used to
characterize materials in the field.
The DRMS devices developed for determining drilling resistance profiles is a quasi nondestructive method (Tiano et al., 2000b)). This device provides concrete information of
extreme importance both in the laboratory and in situ. The profiles of drilling resistance are
very informative and can be used in multiple circumstances in the study of stone conservation.
They provide direct information about the stone mechanical strength, identify the decay
profiles in situ up to significant depth (05cm) and are decisive for the assessment of
effectiveness, harmfulness and durability of consolidation treatments.
In Portugal, the DRMS device has been used successfully with carbonate stones both in the
laboratory and in situ to detect and characterize the consolidation action, alteration profiles,
past consolidation interventions and durability of consolidation treatments. This paper presents
some examples of the recent experience, where DRMS was one of the methods extensively
used both for the characterisation of the effectiveness and to monitor the evolution of treated
carbonate stones subject to ageing in natural exposure conditions (Ferreira Pinto, 2002).

CONSOLIDATION ACTION
The penetration depth is the parameter more widely referred and accepted (Manaresi, 1981),
for performance evaluation of consolidation treatments. Its importance was pointed out by
Schaffer in 1932 (Tabasso, 1993) and, still today, penetration depth continues to be considered

6th International Symposium on the Conservation of Monuments in the Mediterranean Basin, Lisbon, Portugal, April 7-10, 2004

as a fundamental parameter for the assessment of consolidation action (Sasse, Snethlage,

1996).
It is generally accepted that a high penetration capacity is a positive aspect and many authors
have been alerting to the danger of occurrence of highly contrasting interfaces between treated
and non treated zones, (Hosek, 1985), (Amoroso and Fassina, 1983), (Delgado Rodrigues
and Costa, 1995), (Sasse and Snethlage, 1996). However, specific works that discuss in detail
these aspects are relatively scarce.
The penetration depth can be evaluated through the identification of its presence or indirectly
through its influence in the stone properties (Leroux et al., 2000). Chemical analysis,
coloration methods (Kumar and Ginell, 1997), SEM analysis (Ausset and Philippon, 1988),
(Schnabel, 1992), FTIR and other spectroscopy techniques have been used for this purpose.
However, it is important to enhance that the presence of the product by itself is not a direct
estimator of the consolidant performance, in the sense that the product may be present and have
little or nil consolidation action.
The direct evaluation of the mechanical resistance in depth has been little used, given the
difficulty of its measurement. Prim and Wittmann (Prim and Wittmann, 1985) had developed
a method to evaluate tensile strength and the modulus of elasticity in depth, by using 1cm
slices taken from samples with 10cm of diameter.
The drilling resistance measurement is not a new method for evaluation the consolidation
action in depth (Leroux et al., 2000). However, important improvements in the available
equipment have been introduzed in the last decade (Alfes et al., 1992), (Tiano et al., 2000b)).
Recent results (Tiano et al., 2000a)) place this methodology as the most promising for the
evaluation of the consolidation performance, particularly in relatively soft stones (Ferreira
Pinto, 2002), (Marques and Delgado Rodrigues, 2002).

EQUIPMENT AND MATERIALS

DRMS DEVICE
The DRMS (Drilling Resistance Measurement System) is a portable device designed to
perform drilling resistance measurements in stone materials developed under the EC
HARDROCK project (SMT4 CT 96 2065). It can be used in laboratory and transported and
operated in situ, even in scaffolding structures. During the development of the HARDROCK
project the DRMS proved to be a powerful technique for determining the state of conservation
of building materials and for measuring the consolidation action and the impregnation depth.
A detailed description of the DRMS equipment can be found elsewhere (Tiano et al., 2000b)).
The equipment consists of a precision drilling machine equipped with two precision motors
able to keep a predefined rotation speed and to guarantee a predefined advancing rate. The full
operation is controlled by an electronic unit or directly by a computer. The test results are
registered in a data logger or directly exported to the computer. The equipment executes a
small drill hole, typically with 5mm in diameter, down to 5cm, under precisely and controlled
drilling conditions defined by the operator: drilling rotation speed, advancing rate and the hole
depth. The output is a graph of force versus depth.
In this study current tungsten drill bits with 5mm in diameter were used under the following
drilling conditions: 400rpm, 15mm/min.

6th International Symposium on the Conservation of Monuments in the Mediterranean Basin, Lisbon, Portugal, April 7-10, 2004

MATERIALS
The laboratory experiments were carried out on four carbonate stones that correspond to
varieties present in many historic buildings in Portugal:
- An stone a very homogenous, white stone, with an extremely fine grain and high
porosity, almost exclusively formed of calcite. It is quarried in An in Coimbra region;
- Coimbra stone a heterogeneous stone mainly constituted of dolomite, quarried in Coimbra
and its surroundings. It has a yellowish colour and may show some iron spots;
- Lisbon stone a yellowish stone from the Lisbon region, mainly constituted of dolomite;
- Boia stone a very pure calcitic limestone almost exclusively formed of calcite, quarried in
Coimbra region.
Table 1 presents some properties of the tested stones.
Table 1 Stone properties
Stone
An
Coimbra
Lisbon
Boia

Open porosity (%)

27
18
15
10

Real density (kg.m-3)

2710
2850
2850
2710

Compression strength (MPa)

36
89
143
135

Three commercial available consolidation products were selected and applied in each lithotype:
Tegovakon V (TG) (an ethyl silicate in white spirit, by Goldschmidt, ready to use); Paraloid
B72 (B) (an acrylic resin by Rhm and Hass), and EP 2101 (EP) (a cycloaliphatic epoxy resin,
by EUROSTAC). These two latter products were applied with the following formulations:
- Paraloid B72: dissolved at 0.06:0.61:0.09:0.2 (resin:toluene:xylene:acetone);
- EP 2101: diluted in 1:1 in a mixture of toluene/xylene (1:1), in weight.
Specimens with different sizes and forms treated by immersion or by brushing were used
according to the pursued specific objectives. Some specimens were consolidated by total
immersion over 24h (14h for EP) in order to have a maximum penetration and a good
approximation as to what could be expected from a fully impregnated specimen. Stone slabs,
with about 3cm thickness, were consolidated by brushing until apparent refusal in order to
achieve a similar treatment to the one that usually is done in real situations.
The specimens were left in laboratory environment at least for a month and then drilled with a
unique drill bit for each stone variety under the same drilling conditions used to characterise
the stone before treatment.

RESULTS
The study of the consolidation effects disclosed the difficulty in accomplishing a satisfactory
consolidation of this type of supports. In Boia stone we can see that ethyl silicate (TG) is
unable to promote any visible effect, Fig. 1, while the epoxy resin (EP) promotes a very thin
and hard peak near the stone surface, Fig. 2. From these figures it is evident that together with
a small penetration capacity a strong contrast between treated and non-treated stone was
created, fact that immediately raises the question on the risk of the occurrence of subsequent
harmful consequences.

6th International Symposium on the Conservation of Monuments in the Mediterranean Basin, Lisbon, Portugal, April 7-10, 2004

50
40
30
20

before treatment

10

Boia stone

40

treated with T G
Force [N]

Force [N]

50

Boia stone

treated with EP
30
20
10

before treatment

10
15
Depth [mm]

20

Fig. 1 Example of ethyl silicate (TG) action on Boia

stone treated by brushing

10
15
Depth [mm]

20

Fig. 2 Example of epoxy resin (EP) action on Boia

stone treated by brushing

Among the large amount of data gathered with this equipment, the following aspects are
selected to highlight the usefulness of this testing methodology:
Consolidation effect of ethyl silicate:
Ethyl silicate based products are used frequently and pointed out as consolidants with low
capacity to promote high consolidant action. Fig. 3 demonstrates the small consolidation
action promoted by ethyl silicate on Lisbon stone and its difficulty to penetrate inside the
stone. However, when applied on An stone, a very porous one (28%), revealed small
strength increment although almost constant and penetrated quite deep inside the stone
Fig. 4;
50
40

15

treated with T G

30

treated with T G

10

20

before treatment

before treatment
5

10

0
5

10
Depth [mm]

15

Fig. 3 Example of the consolidation action

promoted by ethyl silicate when applied by brushing
on Lisbon stone

Presence and relevance of interfaces:

Besides the consolidation action, the
contrast in properties between treated
and non-treated zones is considered very
relevant for the assessment of the overall
performance of consolidants. Fig. 5
shows the strength graphs obtained with
An stone treated with acrylic (B) and
epoxy (EP) products where a superficial
layer is strongly consolidated although
showing a sharp contrast with the
underlying non-treated zone;

10
De pth [mm]

15

20

Fig. 4 Example of the consolidation action

promoted by ethyl silicate when applied by brushing
on An stone

60

An stone

50
Force [N]

An stone

Force [N]

Force [N]

20

Lisbon stone

treated with EP

40
30

treated with B

20

before treatment

10
0
0

10
15
Depth [mm]

20

Fig. 5 Drilling resistance profiles obtained on An

stone treated by total immersion with acrylic (B) and
epoxy (EP) products

6th International Symposium on the Conservation of Monuments in the Mediterranean Basin, Lisbon, Portugal, April 7-10, 2004

Treatment applicability
The easiness of testing with DRMS allows the characterization at close distances, fact that
may detect variations that heterogeneous materials may exhibit. Fig. 6 shows Coimbra
stone, known for its heterogeneity, where softer zones show a certain consolidation action
while the harder ones show little or no consolidation.

Force [N]

20

Coimbra stone, softer zones

15

Coimbra stone, hard zones

80

treated with B

Force [N]

10
5

treated with B

60
40

before treatment

20

before treatment
0

10
De pth [mm]

15

10
Depth [mm]

15

Fig. 6 Example of the consolidation action promoted by acrylic resin (B) applied by brush on softer and
harder areas of Coimbra stone

Monitoring of treated stones in natural exposure

The data obtained with the drilling resistance measurement enable to monitor the
evolution of the consolidation action. Fig. 7 shows the values of drilling resistance
obtained in specimens of Coimbra stone treated with the epoxy resin (EP), after treatment
and after 1 year of exposure in a marine site. The same protocols for drilling resistance
measurement used in the precedent steps were used for this post-exposure
characterisation. The graph shows a reduction in the consolidation close to the surface, in
agreement with the reduction in the scratch hardness with the Martens indenter, Fig. 8.
The conclusion on the occurrence of some superficial reduction of the consolidation
action obtained with the drilling measurement was confirmed with the scratch
measurement.
40

Coimbra stone treatead with EP

0,6
Scratch width [mm]

before exposure

Force [N]

30

after 1 year of exposure

20
10
0

Coimbra stone treated with EP

0,4

0,2

10
15
Depth [mm]

20

Fig. 7 Example of the drilling resistance

measurement on monitoring treated stones submitted
to natural exposure

before exposure 1 after exposure

Fig. 8 Occurrence of superficial reduction of the
consolidation action, after 1 year of natural exposure,
identified by scratch measurement

FINAL REMARKS
The results demonstrated the potential of the drilling resistance measurement for the
identification, characterization and discrimination of the consolidating capacity of treatment
products when applied on carbonate stones, as well as for monitoring the evolution in time of
the consolidation action.

6th International Symposium on the Conservation of Monuments in the Mediterranean Basin, Lisbon, Portugal, April 7-10, 2004

The results corroborate the known poor consolidating effect of the ethyl silicate based products
and put in evidence the weak penetration capacity of the acrylic resins. It was possible to verify
the possibility of occurrence of dangerous strength contrasts that are created between treated
and non-treated zones when acrylic and epoxy resins are used.

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