Effect of Baltic Seawater and Binder Type on Frost

Durability of Concrete
A. Cwirzen 1; P. Sztermen 2; and K. Habermehl-Cwirzen, D.Sc. 3

Abstract: The effects of Baltic seawater on frost durability of PC concretes using sulfate resistant portland cement and combination of rapid
hardening portland cement with silica fume were studied. The freeze-thaw cycles were performed on specimens exposed to the Baltic
seawater, 3% sodium chloride solution and deionized water. The freeze-thaw cycles appeared to cause the most extensive internal damage
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in specimens based on sulfate resistant cement (SR) and exposed to seawater. The most extensive surface scaling was observed in the case
of concretes containing silica fume and exposed to deicing salts. Based on the thermo gravimetric and X-ray diffraction analyses it was
concluded that extensive internal damage of concrete based on SR was caused by changes of the microstructure due to secondary formation
of ettringite, carbonation, and formation of calcite. The results showed also that low C3 A content of the SR did not fully mitigate formation
of secondary ettringite during freeze-thaw cycles. A combination of rapid hardening portland cement and silica fume appeared to form
more frost resistant concrete when exposed to seawater. DOI: 10.1061/(ASCE)MT.1943-5533.0000803. © 2014 American Society of Civil
Engineers.
Author keywords: Frost attack; Seawater; Microstrcuture; Seawater attack.

Introduction
Concrete structures exposed to seawater in northern environments
are subjected to two interdependent forms of attack, physical and
chemical. Both types of attacks may occur at the same time and
may accelerate the deterioration processes. The deterioration due
to the chemical attack is related to carbonation, sulfate attack, and
alkali-aggregate expansion (Mehta 1980, 1991; Conjeaud 1980).
The physical forms of attack include cycles of heating and cooling,
freezing and thawing, wetting and drying, as well as reinforcement
corrosion. The physical attack such as, for example, wetting and
drying in combination with freeze-thaw cycles can initiate chemical
deterioration. A combination of causes depends on the location of
the concrete element, either being fully submerged, or in the splash
zone or in the atmospheric zone. The most severe conditions can be
found in the splash zone where nearly all types of attacks can occur.
Most of the described deterioration mechanisms were extensively
studied in the past, e.g., described by Taylor (1997). On the con-
trary the amount of available research data on the effects of sea-
water and binder type on the frost durability is still limited.
Some early studies were done at the end of the 80’s by Moukawa
et al. (1989), whose test included specimens exposed to seawater
1 from several laboratory investigations as well as from a number
Adjunct Professor, Aalto Univ., School of Engineering, Dept. of
Civil and Structural Engineering, Concrete Technology Laboratory,
Rakentajanaukio 4, 02150 Espoo, Finland (corresponding author). E-mail:
andrzej.cwirzen@aalto.fi
2 cements having from 4 to 13% of C3 A and water to binder ratios
Graduate Student, Aalto Univ., School of Engineering, Dept. of
Civil and Structural Engineering, Concrete Technology Laboratory,
Rakentajanaukio 4, 02150 Espoo, Finland.
3
Senior Researcher, Aalto Univ., School of Engineering, Dept. of
Civil and Structural Engineering, Concrete Technology Laboratory,
Rakentajanaukio 4, 02150 Espoo, Finland.
Note. This manuscript was submitted on September 27, 2012; approved
on February 14, 2013; published online on February 18, 2013. Discussion
period open until July 1, 2014; separate discussions must be submitted for
individual papers. This paper is part of the Journal of Materials in Civil
Engineering, Vol. 26, No. 2, February 1, 2014. © ASCE, ISSN 0899-1561/
2014/2-283-287/$25.00.
and fresh water in simulate splash zone conditions. The results
showed a strong effect of the surface deterioration on the damage
mechanisms. Specimens exposed to freeze-thaw cycles in seawater
revealed formation of layers rich in calcium and brucite. Dissolu-
tion and leaching of portlandite (P) appeared to occur only in the
external layers. The specimens exposed to freeze-thaw cycles in
fresh water showed only carbonate layer on their surfaces. Newer
studies by Wang and Ayuta (2001) and Wang et al. (2002) showed
that freeze-thaw cycles in seawater caused the enlargement of pores
with radii in from 102 to 103 nm, caused microcracking of the
binder matrix and increased the degree of saturation and led to
a rapid deterioration of the mortar samples. Shui et al. (2010) stud-
ied the effect of frost attack in seawater and in fresh water on con-
cretes with various water to binder ratios and additions of fly ash
(FA) and silica fume (SF). Based on the obtained results authors
concluded that freeze-thaw cycles in seawater caused more internal
damage than when exposed to fresh water. Replacement of cement
by SF and low water to binder ratio resulted in the least damage of
all studied concretes. The causes of more extensive deterioration of
PC based concretes in seawater are not yet fully clarified. For in-
stance the sulfate attack has been indicated as the main form of
chemical attack of seawater on PC concrete resulting in recommen-
dations to use a low C3 A content PC. However, results obtained
of site exposures did not confirm validity of that recommendation.
For instance, Gjörv (1971) investigated the 40-year-old concrete
specimens exposed to seawater. Specimens were produced using
from 0.5 to 0.6. The results showed that the most important factor
was the water to binder ratio, which defined the microstructure of
the hydrated matrix. Concrete having the same water to binder ratio
but being produced with cements containing various C3 A contents
performed in the same way. Malhotra et al. (1988) also obtained
similar results.
The main objective of the present research was to investigate
the effects of a binder type and kind of a freezing medium on
the microstructure and frost durability of concretes. Further aim
was to study changes of the chemical composition of hydrated

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J. Mater. Civ. Eng., 2014, 26(2): 283-287

 binders and formation of new phases within the airvoids and their
influences on the frost damage.
Experimental Setup
Two types of PC and one type of secondary binder (SB) were used
in this study. Concretes marked as SR used sulfate resistant PC type
CEM I 42.5N while concretes marked as SF used rapid hardening
PC type CEM I 52.5R, with 5-wt% replacement by SF. Finnse-
mentti produced both PCs. The used SF type 920D produced by
Elkem was electrostatically densified. These types of binders were
chosen following a common practice and recommendation regard-
ing choice of binders for marine structures. The chemical compo-
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Baltic seawater (SW). However, due to equipment limitation the SF
mix was not tested in DW exposure. The DA and DW are standard
freezing mediums used in CIF/CDF test and were used as referen-
ces to the SW. The chemical composition of Baltic seawater SW is
shown in Table 3.
The specimens for freeze-thaw tests had dimensions of 7 × 11 ×
15 cm3 and for compressive strength measurements 10 × 10 ×
10 cm3 . In both cases three specimens for each mix were studied.
The pore size distribution, spacing factor, and pore-specific surface
area were measured using Air-Void Analyzer (AVA) produced by
Germann Instruments A/S. The measurements were done using
fresh concrete samples.

sition of PCs and SF is shown in Table 1. The water to binder ratio Test Results and Discussion
was 0.45 while the amount of superplasticizer (SP) and air entrain-
ing agent (AEA) varied, Table 2. The used SP was a polycarbox- The pore structure was studied on fresh concretes by AVA analyzer
ylate type Glenium Sky 600 while the AEA was Mischöl LP 71; and pressure method. The results are shown in Table 4. The SR
BASF produced both admixtures. concrete appeared to contain less entrained air, 4.7 versus 6.5%
The chemical composition of hydrated binders after freeze-thaw in the case of SF concrete, but at the same time the detected airvoids
cycles was studied using X-ray diffraction (XRD) and thermo gra- were finer and more densely distributed throughout the paste. The
vimeter (TG). The XRD analysis was done using the XRD diffrac- spacing factors were 0.219 μm in the case of SR concrete and
trometer type PW1830 produced by Philips. The TG analysis was 0.233 μm for SF concrete. Both values should provide very good
done using a TG analyzer type 951 produced by Du Pond Instru- frost durability (Pigeon and Pleaau 1995). The pores-specific sur-
ments, updated with a Temperature Programmer Interface (TPI) face area of SR concrete was higher in comparison with SF con-
controller. The TG measurements were done in helium protective crete. This can be related to the presence of SF, which is known to
atmosphere using a flow rate of 40 L= min. All materials for XRD increase viscosity of the fresh concrete mix and cause problems
with air entrainment (Aiticin 1998). As a result the SF concrete
and TG studies were obtained from concrete specimens subjected
required higher addition of SP and AEA.
to freeze-thaw cycles. Samples were crushed and larger aggregates
Mechanical properties of concretes were defined only based on
and sand particles were manually extracted before final grinding.
1 and 28-day compressive strength values, Fig. 1. The SF concrete
The frost durability was assessed using the CIF/CDF test pro-
showed higher 1-day compressive strength values in comparison
cedure, which followed the CEN/TC 51 N772 (2003) standard.
with SR concrete. The 28-day compressive strength was similar
Duration of each freeze-thaw cycle (þ20°C= − 20°C= þ 20°C)
for both concretes; 51 and 58 MPa, respectively, for SR and SF
was 12 h. The internal damage was determined by measurements
concretes. Higher strengths of SF concrete are related to the com-
of the ultrasonic transit time. All test specimens for freeze-thaw
bined effects of the used rapid hardening PC and presence of SF,
testing were prepared following the CEN (2003) standard. Three
which accelerated hydration processes and densified the binder ma-
types of freezing mediums were used; 3% sodium chloride solution
trix (Cwirzen and Penttala 2005). Slightly lower workability of SF
simulating deicing agent (DA), deionized water (DW), and natural concrete can be linked to a finer particle size distribution of the used
rapid PC as well as to the effect of SF itself which particles diameter
Table 1. Chemical Composition of Used Cements and Silica Fume is 100 times smaller in comparison with PC. Furthermore, the used
SF was electrostatically densified and contained some carbon,
CEM I 52,5 R CEM I 42,5 Elkem Microsilica
Component (OPC) (%) (SR) 920D (SF)
which are known to decrease the efficiency of SP (Cwirzen et al.
2009).
CaO 64.9 63.1 <1 The result of capillary suction test, which began 7 days prior to
SiO2 22.6 20.2 96.6 the actual freeze-thaw cycles, is shown in Fig. 2. The specimen
Al2 O3 3.4 2.2 0.3
bottoms were immersed in liquids, which were later used during
Fe2 O3 4.2 4 0.6
MgO 0.9 2 1.3 freeze-thaw cycles. The highest total capillary water uptake was
Na2 O 0.05 0.18 0.6 observed in the case of SR concretes immersed in SW followed
K2 O 0.6 0.31 2.05 by SR concretes immersed in DA. All SF concretes showed lower
SO3 2.2 — 1.3 water uptake regardless of the used liquid. Based on these results
Cl 001 — 0.125 and supplemented by the AVA analysis, it can be concluded that the
C2 S 23.9 68 — water uptake depended only on the microstructure of the hydrated
C3 S 54.2 13 — binder matrix. As shown in Table 4, the SR concrete had signifi-
C3 A 2 1 — cantly higher specific pores surface area but lower total porosity in
C3 AF 12.7 13 — comparison with SF concrete, which in combination with higher
LOI 2.1
water uptake indicates a presence of fine interconnected capillary

Table 2. Concrete Mix Composition

Total aggregate content
Mix W/B Cement type Cement (kg=m3 ) SF (kg=m3 ) (kg=m3 ) SP (wt% of binder) AE (wt% of binder)
SR 0.45 CEM I 42,5 N 400 0 1,798 1.5 0.15
SF 0.45 CEM I 52,5 R 388 12 1,798 2 0.4

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J. Mater. Civ. Eng., 2014, 26(2): 283-287

 1.4
Table 3. Composition of Baltic Seawater [adapted from Lahdes and
SF-SW
Karjala (2007)] SF-DA
1.2
Type of water Mg2þ Ca2þ Naþ Kþ SO2− Cl− SF-DW
4

Water uptake [wt%]

SR-SW
1 SR-DA
Baltic seawater (mg=L) 240 98 1,800 67 410 3,000
0.8

Table 4. Fresh Concrete Porosity and Air Content Measured by AVA 0.6
Analyzer and Pressure Method
0.4
Pore structure SF SR
Airvoids specific surface (m2 =kg) 25.5 32.4 0.2
Airvoids spacing factor (μm) 0.233 0.219
Total air content (%) 11 7.5 0
0 20 40 60 80
Air content (<0, 3 mm) (%) 1.8 1.5
Number of freeze-thaw cycles
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Total air content (%) (pressure method) 6.5 4.7

Fig. 3. Water uptake measured until 84 freeze-thaw cycles

1d compressive strength
70 65
28d compressive strength 110
Slump 64
60

Relative Dynamic Modulus [%]

Compressive strength (MPa)

63 100
50
62
Slump (mm) 90
40 61
80
30 60 SF-SW

59 70 SF-DA
20 SF-DW
58
60 SR-SW
10
57
SR-DA
0 56 50
SR SF 0 20 40 60 80
Number of freeze-thaw cycles
Fig. 1. One and 28-day compressive strength values and workability
measured by means of slump Fig. 4. Internal damage measured until 84 freeze-thaw cycles

0.5 concrete exposed to DA and not for concretes exposed to SW as

SF-SW observed during the initial capillary suction.
SF-DA
SF-DW
The development of the internal damage of concretes exposed to
0.4
SR-SW freeze-thaw cycles is shown in Fig. 4. The SF concrete exposed to
Water uptake [wt%]

SR-DA DW showed marginal damage after 84 cycles. The highest internal

0.3
0.2
0.1
0 for concrete exposed to SW as well as to DA. The most interesting
-7 -6 -5 -4
Days
Fig. 2. Capillary water uptake measured before freeze-thaw cycles
(“-”denotes number of days before initiation of the freeze-thaw cycles)
pores. The type of freezing liquid most probably did not have any
impact on the water uptake due to a short duration of exposure.
Similar trends regarding the water uptake were initially observed
during the subsequent freeze-thaw cycles, Fig. 3. However, later
measurements revealed significant alterations related to other phe-
nomena, which will be described later. For example the highest
water uptake after 84 freeze-thaw cycles was measured for SR
damage was measured in the case of SR concrete exposed to SW.
After initially good performance the damage started to develop rap-
idly after 40 freeze-thaw cycles. In the case of remaining concretes
the internal damage appeared to be very similar and reached be-
tween 80 and 88% changes of the RDM after 84 cycles. In the case
of these samples the damage appeared to be very low until 56
cycles, followed by its rapid increase. This trend was recorded
-3 -2 -1 0 results can be seen when comparing the development of internal
damage of SR concrete exposed to SW and DA. In this case,
the recorded RDM dropped from 85% in DA exposure to below
75% when SW was used. Initially the reason for this result was
unclear especially due to the short time exposure to SW; therefore,
additional TG and XRD studies were done on concrete specimens
after freeze-thaw cycles and results will be discussed later in this
article.
The recorded surface scaling test results, shown in Fig. 5,
revealed that the most extensive deterioration occurred in all
specimens exposed to DA. The specimens exposed to SW and
DW showed very little damage even after 84 freeze-thaw cycles.
The scaling mechanism in the presence of SW appeared to reassem-
ble more DW then DA. Shui et al. (2010) reported similar results

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J. Mater. Civ. Eng., 2014, 26(2): 283-287

 1000
SF-SW
SF-DA
800
SF-DW
Surface scaling [g/m2]

SR-SW
600 SR-DA

400

200

°
0
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0 20 40 60 80 Fig. 7. DTG of SF concrete after freeze-thaw cycles in seawater (SF-

Freeze-thaw cycles SW) and deicing salts (SF-DA) (D = structural OH groups+carbonates,
P = portlandite, B = brucite)
Fig. 5. Surface scaling measured until 84 freeze-thaw cycles

°
(a) θ
Fig. 6. DTG of SR concrete after freeze-thaw cycles in seawater (SR-
SW) and deicing salts (SR-DA), D = structural OH groups+carbonates,
P = Portlandite, B = brucite

that comparable ultimate surface scaling values of concretes ex-

posed to fresh water and SW. In the present case the surface scaling
was initiated slightly earlier when exposed to SW.
The TG test results of concrete specimens exposed to freeze-
thaw cycles are shown in Fig. 6 for SR concrete and Fig. 7 for
SF concrete. The first recorded decomposition peak observed at
around 120°C represents ettringite (Ramachandran 2001; Taylor
1997). In the case of SR concrete, the results indicated a slightly
higher amount of ettringite present in specimens exposed to SW in
comparison with DA. These results comply with a commonly ob- (b) θ
served phenomenon of secondary ettringite formation in concrete
exposed to SW. In this case the magnesium sulfate from SW can Fig. 8. XRD after freeze-thaw cycles of (a) SR concrete; (b) SF
attack the P and C-S-H phases of the hydrated binder matrix. The concrete (E = ettringite, Q = quartz, P = portlandite, B = brucite,
interaction with P will result in formation of secondary gypsum M = microline, and A = albite) (spectra for SF-DA and SR-DA have
and brucite. The formed gypsum can be later consumed to form been shifted vertically by 300 to clarify the figure)
ettringite with aluminates from C3 A. Furthermore, it will transform
C-S-H into a hydrated calcium magnesium silicate (Regourd 1980;
Pratt and Onabolu 1992). According to, for example, Neville by XRD studies, Fig. 8. The lowest peak was observed for SF con-
(2004), Pratt and Onabolu (1992), or Taylor (1997), formation cretes exposed to freeze-thaw in DA. The interesting peak at 27.5°
of secondary ettringite can cause microcracking of the binder ma- corresponding to ettringite appeared to be significantly higher in
trix. However, the results obtained from this research cannot indi- specimens exposed to freeze-thaw cycles in SW. The obtained re-
cate whether the ettringite caused microcracking or only filled sults showed secondary ettringite formation during freeze-thaw
the airvoids during freeze-thaw cycles. The presence of increased cycles also when using low C3 A content portland cement (SR
amount of ettringite in samples exposed to SW was also confirmed type). The 1% of present C3 A provided a sufficient amount of

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J. Mater. Civ. Eng., 2014, 26(2): 283-287

 aluminates, which combined with sulfates formed ettringite. As a
result the spacing factor was altered due to filling of some of the
voids, which resulted in more extensive internal damage in SW
environment.
In the case of SF concretes, despite a nearly the same extend of
the initial damage shown in Fig. 4, a higher amount of ettringite
was detected in specimens subjected to freeze-thaw cycles in
DA, Fig. 8. Formation of ettringite without additional sulfate origi-
nating from SW could be related to the freeze-thaw cycles in
deicing salts. As studied by Stark (1995) and Bollman (2000),
freeze-thaw cycles cause movement of moisture, which leads to
release of additional sulfate ions from monosulfate. The monosul-
fate is less stable in freeze-thaw cycles and consequently can be
partially transformed through monochlorides, into Friedel’s salts
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which belong to AFm phase, the required chlorides are provided
by deicing salts (Cwirzen 2004). Gypsum liberated during hydro-
thermal processes forms additional ettringite with monosulfate,
which is not yet decomposed. The regular PC used for SF mixes,
Table 1, had higher content of sulfates, 12-wt% versus 0-w%, in
comparison with SR cement. Furthermore, its C3 A content was
two times higher in comparison with the SR cement. All these fac-
tors in combination with the freeze-thaw cycles could contribute to
formation of higher amount of ettringite in SF concrete exposed to
DA. The salt concentration of the used Baltic seawater was less
than 2 wt% (Lahdes and Karjala 2007).
The results showed also a significantly higher amount of P in the
case of SR concrete in all exposures. This trend can be directly
linked to the presence of SF in SF concrete and its pozzolanic
activity (Taylor 1997). The XRD test revealed also presence of mi-
croline (M) and albite (A). P and calcite (C) were detected in all
studied samples regardless of the used freezing medium.
The TG results revealed a presence of other phases too. For in-
stance the decomposition at around 700 °C can be related to OH
groups and carbonated phases (Gabrovsek et al. 2006). The amount
of these phases appeared to be slightly higher for all concretes ex-
posed to SW. The XRD studies also revealed peaks corresponding
to calcite, Fig. 8, which might indicate a higher carbonation in SW.
The carbonates formed within the pore structure could further lower
the frost durability by increased of the capillary suction.
Conclusions
The effects of seawater on frost durability of PC concretes were
studied. The sulfate resistant PC and combination of rapid harden-
ing PC with SF were used as binders. A natural Baltic seawater and
3% sodium chloride solution were used as freezing mediums. After
freeze-thaw cycles all specimens were investigated using XRD and
TG. The freeze-thaw cycles appeared to cause the most extensive
internal damage in specimens based on SR cement exposed to SW.
The most extensive surface scaling was observed in the case of SF
concretes exposed to DA. The TG and XRD analysis of the deterio-
rated concretes specimens revealed presence of ettringite and C in
all specimens but with varying amounts. Based on the obtained re-
sults it was concluded:
• The extensive internal damage of SR concrete was caused by
carbonation of the binder matrix, higher capillary porosity,
and formation of ettringite and C in the airvoids.
• Alteration of the microstructure led to increase of the spacing
factor and capillary porosity as well as decrease of the total
porosity, which resulted in more extensive frost damage.
• The results showed also that low C3 A content of the SR cement
did not fully mitigate formation of secondary ettringite, which
JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / FEBRUARY 2014 / 287
J. Mater. Civ. Eng., 2014, 26(2): 283-287
was possible due to combination of the chemical composition of
seawater, carbonation, and freeze-thaw cycles.
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