Frost resistance of concrete surfaces coated

with waterproofing materials

Cite as: AIP Conference Proceedings 1653, 020061 (2015); https://doi.org/10.1063/1.4914252
Published Online: 13 April 2015

A. Klovas, M. Dauksys, and G. Ciuprovaite

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AIP Conference Proceedings 1653, 020061 (2015); https://doi.org/10.1063/1.4914252 1653, 020061

© 2015 AIP Publishing LLC.

 Frost Resistance of Concrete Surfaces Coated
with Waterproofing Materials
A. Klovas1, a), M. Dauksys1, b) and G. Ciuprovaite2
1
Department of Civil Engineering Technologies, Kaunas University of Technology,
Studentu str. 48, LT-51367 Kaunas, Lithuania
2
UAB Markuciai, Žarijų str. 6, LT-02300 Vilnius, Lithuania
a)
Albertas.Klovas@ktu.lt
b)
Mindaugas.Dauksys@ktu.lt

Abstract. Present research lays emphasis on the problem of concrete surface exposed to
aggressive surrounding quality. The test was conducted with concrete surfaces coated with
different waterproofing materials exposed in solution of 3 % of sodium sulphate. Research was
performed according to LST EN 1338:2003 standard requirements. Technological properties of
concrete mixture as well as physical-mechanical properties of formed concrete specimens were
established. The resistance of concrete to freezing – thawing cycles was prognosticated
according to the porosity parameters established by the kinetic of water absorption. Five
different waterproofing materials (coatings) such as liquid bitumen-rubber based, elastic fiber-
strengthened, silane-siloxane based emulsion, mineral binder based and liquid rubber
(caoutchouc) based coatings were used. Losses by mass of coating materials and specimens
surface fractures were calculated based on the results of frost resistance test. Open code program
“ImageJ” was used for visual analysis of concrete specimens. Based on the results, aggressive
surrounding did not influence specimens coated with elastic, fibre-strengthened, mineral
materials. On the other hand, specimens coated with liquid rubber (caoutchouc) based material
were greatly influenced by aggressive surrounding. The biggest losses of specimen surface
concrete (fractures) were obtained with silane-siloxane based emulsion coating. Generally,
specimens coated with waterproofing materials were less influenced by aggressive surrounding
compared with those without.
Keywords: Freezing-thawing cycles; porosity parameters; waterproofing materials; concrete
surface quality.
PACS: 81

INTRODUCTION
Decomposition of concrete due to its freezing-thawing is a big problem in Northern
Europe. There are a number of researches being carried out regarding concrete
resistance to freezing. It must be noted that there is only little information regarding
concrete surfaces coated with waterproofing materials resistance to freezing-thawing
cycles under the aggressive environment surrounding (salt solutions). Concrete is an
artificial material which is obtained from the hardened slurry consisted of binding
material, aggregates, water and admixtures. Concrete is sophisticated structure
composition material. The structure of concrete is complicated due to different sized
particles reaching from few millimeters to few centimeters. Over the course of time
the structure and properties of concrete is changing due to its physical-chemical

4th International Congress in Advances in Applied Physics and Materials Science (APMAS 2014)
AIP Conf. Proc. 1653, 020061-1–020061-8; doi: 10.1063/1.4914252
© 2015 AIP Publishing LLC 978-0-7354-1295-8/$30.00

020061-1
processes [1]. There are many reasons for the air pores appearance in concrete
structure: the addition of air entraining admixtures; various technological impurities;
mistakes in composition of concrete mixture; inappropriate consolidation of mixture
as well as the shrinkage deformation. Two types of porosity should be taken into the
consideration: open (capillary) and closed (air content in a cement stone). Porosity is
the key factor why a concrete is affected by chlorides, oxygen and carbon dioxide and
this could be a cause of corrosion. Certain scientists adopt the position that the level of
concrete porosity, size of pores and capillaries, their distribution and character have
the biggest influence on the resistance to freezing-thawing of concrete [2,3]. Open
pores and capillaries in concrete structure appear because of the evaporation of free
water. The size of these cavities is influenced by water and cement ration of concrete
mixture. A number of researchers argue convincingly that closed concrete structure
porosity establishes because of two factors: the entrainment of air from environment
and the contraction of cement stone [4,5]. Recent studies raise important questions of
how the concrete mixture waterproofing additives such as stearates, oleates, silanes
and silicone lms influence the capillary water absorption of an element [6]. Powdered
silicone and sodium oleate showed the best resistance to water penetration. Many
studies asses the significance of waterproofing materials effect on steel reinforcement
corrosion [7]. Studies suggest that the specimens coated with the polyurethane
elastomer-based waterproofing material performed better than concrete specimens
coated with other waterproong materials. The common case for concrete destruction
is due to the influence of freezing-thawing cycles. The main purpose for the concrete
destruction is water which becomes ice and due to this process the volume increases
significantly (ice volume is 9 % bigger than water). Authors state their opinion that the
pressure of ice crystals can break the inner walls of pores and capillaries and therefore
whole construction can get destructed [8,9]. Few authors lay emphasis on water
freezing temperature [10]. The argument is drawn that water in capillaries or pores
should not necessarily get frozen under the temperature of 0 oC. The size and structure
of cavities can specify this temperature. If the pores are smaller, water will freeze at
lower temperatures as well. For example, if the pores diameter is at least 10 nm then
the water freezing temperature will be -5 oC and on the other hand, if the diameter is at
least 3.5 nm then water will freeze at -20oC. Studies show that ice is a very strong
material and its adhesion to hydrophilic materials such as soil or concrete is also very
high [11]. It is expected that the infiltration of ice in a moist porous body during
freezing will alter its strengths. Ice has both a compressive and a tensile strength under
short-term loading, but because ice is viscoelastic under long-term loading it has none
(ibid). The presence of dissolved materials and solutes affect the strength of ice.
The following methods are used to study changes in concrete characteristics during
freezing and thawing cycles: magnetic resonance imaging technique [12], digital
laminography as a non-destructive inspection X-ray method [13], electrical resistivity
measurements for simultaneous monitoring of temperature and damage in real time
[14]. The glue-spall theory draws a conclusion that concrete is damaged when ice
cracks on the surface of the material, when the thermal expansion exceeds the strength
of the ice [15]. Over the course of time, the technical condition of the element exposed
to freezing-thawing cycles, deteriorates that can influence the life span of certain
construction. It is utmost important to evaluate the water absorption into the element

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[16]. Researches based on concrete resistance to freezing-thawing cycles present a
case that the level of water absorption influences the final compression strength of
concrete element. It is known that the bigger water absorption is the lower
compression strength of concrete element become. Some studies regarding
polyurethane waterproong membrane on mortar substrates haves been carried out
[17]. The results of outdoor exposure and accelerated carbonation tests which were
conducted over the period of 5 years indicate that deterioration of waterproofing
membranes on the cracked area of the element occurs faster compared with non-
cracked areas.
This study strongly lays emphasis on concrete elements coated with waterproofing
materials which are exposed to 3 % sodium sulphate solution under a number of
freezing-thawing cycles.

METHODS AND MATERIALS

In order to conduct following experiments CEM III/B 32.5 N-LH (SR) cement was
used. Table 1 indicates physical and mechanical properties of the cement.
TABLE 1. Physical and mechanical properties of Portland cement, CEM III/B 32.5 N-LH (SR)
Property Unit
Normal consistency of cement paste, % 30.0
Volume stability, mm 0.5
Initial setting time, min 205
Compress strength after 7 days/after 28 days, MPa 19.9/39.4
Loss on ignition, % 1.41
Insoluble materials, % 0.35
SO3, % 2.95
Cl-, % 0.017
Alkalis, calculated by Na2O equivalent, % <0.8

Sand with the fraction of 0/4 and bulk density of 1710 kg/m3 was used as a fine
aggregate. Granite rubble with the fraction of 4/16 and bulk density of 1500 kg/m3 was
used as a coarse aggregate. Polycarboxylate-based plasticizing admixture was used for
the preparation of concrete mixture. The plasticizing admixture was dosed according
to the mass of cement and it was at the limit of 0.8 %. Table 2 indicates the chemical
composition of latter admixture.
TABLE 2. Chemical composition of polycarboxylate-based plasticizing admixture
Property Unit
Specific mass, g/cm3 1.06
Maximum chloride quantity, % 0.10
Maximum equivalent alkali quantity, % 2.5

Table 3 indicates the granulometric composition of aggregates.

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TABLE 3. Granulometric composition of aggregates
The radius of sieve mesh, The amount of poured our material, %
mm Sand fraction 0/4 Gravel fraction 4/16
31.5 - 100.0
22.4 - 100.0
16 - 97.4
8 100.0 54.4
4 99.1 3.0
2 89.4 1.5
1 77.9 -
0.5 42.9 -
0.25 16.4 -

Concrete mixture was prepared in laboratory using forced mixing mixer. The
mixing time was set to 3 minutes. Cement and other dry aggregates were dosed based
on mass meanwhile water and chemical admixture based on volume. Admixture was
mixed with the water in the preparation of concrete mixture.
Two different types of specimens were prepared: prisms with the size of
200×100×100 mm and cubes with the size of 100×100×100 mm. Specimens were
consolidated using vibrating platform and cured for 28 days in water which
temperature was 20 ± 2oC. Table 4 lists the standards used in this study.
TABLE 4. The list of standards used for the study
Standard Description
LST EN 12350-6 Testing fresh concrete - Part 6: Density
LST EN 12350-2 Testing fresh concrete - Part 2: Slump-test
LST EN 12350-7 Testing fresh concrete - Part 7: Air content - Pressure methods
LST EN 12390-7 Testing hardened concrete - Part 7: Density of hardened concrete
LST EN 12390-3 Testing hardened concrete - Part 3: Compressive strength

TABLE 4 continuation. The list of standards used for the study

Standard Description
GOST 12730.4-78 Concrete porosity
LST EN 1338 Concrete paving blocks - Requirements and test methods

The surfaces of concrete specimens were coated with five different types of
waterproofing materials (H1 – H2). Table 5 indicates the detailed description of
waterproofing materials used in this research.
TABLE 5. The specifications of waterproofing coatings
Waterproofing coating, mark Specifications
Liquid bitumen-rubber based, H1 Desiccate time - 6 hours (20oC). Yield 0.8÷1.2 kg/m2
Elastic fiber-strengthened based, H2 Specific mass - 1.35 g/cm3 (25oC). Heat resistance <60oC. Yield 0.8÷1.0
kg/m2
Silane-siloxane based emulsion, H3 Specific mass 0.95 g/cm3 (25oC).Viscosity 12 mm2/s. pH value 8.
Mineral binder based, H4 2 components: cement binder and emulsion. Loose material density 1.3
g/cm3. Liquid material density 1.05 g/cm3. Yield 4.0÷5.0 kg/m2
Liquid rubber (caoutchouc) based, H5 Specific mass - 1.40 g/cm3 (25oC). pH value 8.6÷9.5

The surfaces of specimens (prisms size of 200×100×100 mm) were firm and solid
without any impurities such as various fats or oils. Specimens were coated with a
brush in two perpendicular layers according to the requirements of producer. In order
to prognosticate the resistance to freezing thawing the methodology provided in GOST
12730.4-78 standard was used. Firstly, concrete specimens were divided into 4 parts

020061-4
and desiccated for 24 hours in 90oC. Secondly, the kinetics of water absorption was
conducted. Full water absorption of concrete specimens was measured after 48 hours
of keeping them in water. Thirdly, the porosity parameters of concrete were
calculated.
In addition, following parameters of pores size were determined: O – index of
concrete pore rate of medium size and D – index of uniformity rate of concrete pores.
This method is widely used for determination of concrete pores structure and for
resistance to freezing – thawing [18].
“ImageJ” method provided visual information about the quality of concrete surfaces
in respect to the ratio between the top waterproofing coating and the raw concrete
surface area [19].
Methodology of image analysis method:
1. Image of the concrete surface is imported into the “ImageJ” program. In this
research, images of around 200 cm2 of area were analyzed.
2. Picture is set to the 8bit quality. This is done to highlight the different
discoloration of the surface;
3. Image scale is set to the certain known dimension;
4. Image colors are changed into the black and white to highlight the blemishes of
the surface;
5. The areas of coating remains are calculated.

RESULTS AND DISCUSION

Concrete mixture was projected according to LST 1974 standard requirements for
hydro engineering concrete with the foreseen strength class C30/37. Concrete surfaces
of hydro engineering structures are often covered with various waterproofing
materials. This type of structures has a tendency to be influenced by salt solutions
under the influence of freezing and thawing. The slump of projected concrete mixture
was established according to LST EN 12350-2 standard requirements and stayed
within the limits of S4 class (160 mm). The average density of fresh concrete mixture
was 2370 kg/m3. The air content of fresh concrete mixture was established according
to LST EN 12345-7 standard requirements and it was 2.9 %. Table 6 indicates the
concrete mixture composition used in this study.

TABLE 6. Concrete mixture composition

Materials Unit Quantity of materials for 1m3 of concrete mixture
Cement kg 379
Water kg 161
Fine aggregate, sand – 0/4 kg 1172
Course aggregate, gravel – 4/16 kg 728
Superplasticizer, Glenium SKY 628 l 2.86
Water and cement ratio - 0.42

Four specimens were tested to perform an experiment of a resistance to freezing –

thawing. Table 7 indicates the average results of four specimens tested.

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TABLE 7. The results of freezing – thawing prognostication
Factor Result Description
WF,% 4.2 Full water absorption of concrete specimens
O 1.17 Index of concrete pore rate of medium size
D 0.39 Index of uniformity rate of concrete pores
PC , % 1.32 Closed porosity (entrained air)
PO , % 9.87 Open porosity (capillary) of concrete
PF 1.48 Factor of resistance to freezing
NC 200 Concrete resistance to freezing – thawing cycles

According to LST EN 1338 standard requirements, concrete surfaces coated with

different waterproofing materials (H1 – H5) were exposed to 3 % sodium sulphate
solution while performing freezing – thawing procedure for 28 days (cycles). Concrete
specimens were kept in the freezing – thawing machine for 24 hours within the
temperature scheme of -20oC to 20oC. H1 sample before and after the freezing thawing
test is indicated accordingly as Fig. 1.a and Fig. 1.b.

(a) (b)

FIGURE 1. H1 sample before (a) and after (b) the freezing thawing test

Table (8) shows the weight loss of the specimen which appeared due to the
cracking.
TABLE (8). Losses of the specimens due to cracking
Marking of the Surface area of the Weight loss due to Weight loss per m2
specimen specimen, m2 cracking, kg
H0 0.01520 0.00149 0.098
H1 0.01488 0.00054 0.036
H2 0.01615 - -
H3 0.01615 0.00126 0.078
H4 0.01520 - -
H5 0.01615 0.00043 0.027
As can be obtained from table 8, H2 and H4 concrete specimens passed the 28
cycles without any weight loss due to cracking. The evaluation of surface coating
materials was performed by the program “ImageJ’. The main aim was to investigate
how much of the waterproofing material remained on the surface and how much is
gone. Analysis of concrete surface images and the calculation of surface waterproofing
material using program “ImageJ’ is presented in Fig. 2. Figure 2.a shows the raw
image, Fig. 2.b indicates the processed image and Fig. 2.c presents the calculation
results.

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 (a) (b)

(c)

FIGURE 2. The concrete surface image analysis of specimen coated with liquid bitumen-rubber based
waterproofing material. (a) Raw image of concrete surface. (b) Image processed with “ImageJ”. (c)
Calculation of concrete surface area
Table 9 indicates the results of image analysis. In all cases, the remaining area of
the waterproofing material was calculated.
TABLE 9. Losses of the specimens due to cracking
Marking of the Surface area of the Area of the remaining Losses of the surface
specimen specimen, m2 coating, m2 coating, %
H1 0.01488 0.00304 79.6
H2 0.01615 0.01615 -
H3 0.01615 0.00172 89.0
H4 0.01520 0.01520 -
H5 0.01615 0.00404 75.0

As it is indicated in table 8, the biggest weight loss (0.098 kg/m2) is obtained when
testing H0 specimen which was not coated with any of waterproofing material. The
second biggest (0.078 kg/m2) weight loss is for H3 (rubber pellet based waterproofing
material) specimen. On the other hand, the least weight loss is noted with coatings H1
(0.036 kg/m2) and H5 (0.027 kg/m2). It must be noted that specimens coated with H2
and H4 materials passed the 28 freezing – thawing cycles without weight loss.
The biggest loss of the waterproofing material itself (89.0 %) was obtained with
the specimen coated with H3 material (silane-siloxane based emulsion). Based on the
theory [20], silanes and siloxanes react with hydrated cement. The result of this
chemical reaction is products that make the concrete pores to become hydrophobic and
therefore the water is stopped from reaching the inside of the concrete. Silanes and
siloxanes enable to minimize the capillary water absorption without closing pores and
capillaries. H1 and H5 specimens also had a significant loss of the surface coating:
79.6 % - liquid bitumen-rubber based and 75 % - liquid rubber (caoutchouc) based. It
must be noted that the loss of surface coating was not detected for specimens H2 and
H4.

020061-7
 To sum up, the coating of concrete surfaces with different waterproofing materials
is a good solution in order to minimize the weight losses and a number of various
cracks due to the freezing and thawing influence. Based on the results of this study, it
can be noted that the weight loss is reduced within the specimens that were coated
with waterproofing materials versus with those that were not. It is a close link between
the remaining quantities of waterproofing material on concrete surfaces and the weight
loss of tested specimens. It is also obtained that the thickness of waterproofing
materials influences the weight and surface coating losses of the specimens.

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