Cement & Concrete Composites 56 (2015) 115120

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Cement & Concrete Composites

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

Evaluation of the effect of tricalcium aluminate content on the severity

of sulfate attack in Portland cement and Portland limestone cement
mortars
Ashlee M. Hossack , Michael D.A. Thomas 1
Department of Civil Engineering, University of New Brunswick, 17 Dineen Drive, Fredericton, New Brunswick E3B 5A3, Canada

a r t i c l e i n f o a b s t r a c t

Article history: It is widely understood that the tricalcium aluminate content of Portland cement is inversely related to
Received 23 January 2014 the concretes ability to resist external sulfate attack. Furthermore, recent research has demonstrated a
Received in revised form 19 October 2014 link between elevated levels of interground limestone and accelerated sulfate attack, particularly thaum-
Accepted 22 October 2014
asite sulfate attack at low-temperatures (below 10 C). In this paper the relationships between Portland
Available online 15 November 2014
cement C3A-content, interground limestone content and supplementary cementitious materials (Type F
y ash and silica fume) are explored. The mortar bars cast with high-C3A cement failed much earlier than
Keywords:
the same bars cast with moderate-C3A cement. External sulfate attack occurred more rapidly at 5 C than
Tri-calcium aluminate
Portland cement
at 23 C. Limestone content did not affect the rate of external sulfate attack.
Portland limestone cement 2014 Elsevier Ltd. All rights reserved.
Thaumasite
External sulfate attack
Low-temperature

1. Introduction Tricalcium aluminate (C3A) within the matrix of hydrated

The durability of a concrete structure is an essential criterion to
consider when evaluating the suitability of a concrete mix for its
intended environment. If a structure is to be exposed to sulfate-
bearing groundwater, seawater, or another potentially sulfate-
bearing environment, its ability to resist external sulfate attack is
critical. External sulfate ions can enter the matrix of hardened
cement paste and interact with hydrated cement compounds, lead-
ing to cracking and softening of the hardened paste [1].
The interaction between external sulfates and hydrated cement
compounds can lead to the formation of ettringite (3CaO
Al2O3-

3CaSO4
32H2O), gypsum (CaSO4
2H2O) [2] and thaumasite
(CaSiO3
CaCO3
CaSO4
15H2O) [3]. This is commonly known as
external sulfate attack (ESA). In the presence of limestone (calcium
carbonate, CaCO3), monocarbonate may replace some of the mono-
sulfate that would have formed during hydration [4]. Furthermore,
increased carbonate content may facilitate the formation of
thaumasite rather than ettringite, or ettringite may be transformed
to thaumasite [5]. The prior existence of ettringite from external
sulfate attack may be necessary for thaumasite to form [6].
Corresponding author. Tel.: +1 (506) 447 9419.
E-mail addresses: Ashlee.Hossack@unb.ca (A.M. Hossack), mdat@unb.ca
(M.D.A. Thomas).
1
Tel.: +1 (506) 458 7789.
cement paste will interact with external sulfates, forming ettring-
ite, and in many cases thaumasite [7]. The formation of ettringite
causes expansion and cracking of the hardened cement paste,
followed by the formation of thaumasite which disintegrates the
calcium-silicate hydrates (CSH) structure [3,8] thus damaging
the concrete and compromising its long-term durability. For this
reason, low-C3A cements are required in sulfate environments in
Canada and elsewhere.
Thaumasite formation is more frequently observed at lower
temperature (below 15 C) [9]; however, it has been reported at
temperatures in excess of 20 C [10]. This may be attributed to
the kinetics of thaumasite formation; thaumasite formation is a
kinetically slow process, particularly at elevated temperatures
[11]. Due to the carbonate ion (CO23 ) required for thaumasite for-
mation, cements produced with higher limestone (CaCO3) replace-
ment levels can be at greater risk for thaumasite sulfate attack
(TSA). In several laboratory trials, a correlation has been observed
between limestone content and increased deterioration due to TSA
[5]. However, limestone content has rarely been linked to thaum-
asite in eld conditions [12].
The current study examines the effect of C3A, supplementary
cementitious material (SCM) and limestone content on the perfor-
mance of mortar bars stored in sulfate solutions at temperatures of
5 C and 23 C. The performance of the mortar bars is compared to

http://dx.doi.org/10.1016/j.cemconcomp.2014.10.005
0958-9465/ 2014 Elsevier Ltd. All rights reserved.
116 A.M. Hossack, M.D.A. Thomas / Cement & Concrete Composites 56 (2015) 115120

the current physical performance (expansion) requirements of the
Canadian standards.
In Canada, concrete exposed to sulfate environments must meet
the requirements of CSA A23.1-09 [13] that imposes maximum
limits on the water-to-cementitious-materials ratio (w/cm) and
permits only sulfate-resistant Portland cements and/or suitable
blends of Portland cement (PC) with supplementary cementitious
material. Sulfate-resisting cements are, in turn, dened in CSA
A3001-13 [14] that imposes C3A and expansion limits on Portland
cement (which may contain up to 5% limestone), and expansion
limits on blended Portland cement (PC + SCM). The requirements
are summarized in Table 1. Sulfate-resisting Portland cements
must pass a 14-day mortar-bar expansion test, whereas blended
Portland cements must pass a 6-month mortar-bar expansion test.
Portland limestone cement (PLC), which may contain up to 15%
limestone, is not permitted for use in concrete exposed to sulfates
unless it is combined with a sufcient level of SCM to meet the pre-
scriptive and performance requirements for sulfate-resisting
blended Portland limestone cements which are summarized in
Table 1. These requirements include testing mortar bars stored in
5% sodium sulfate solution at 5 C to evaluate the potential for
TSA at established minimum SCM replacement levels.
at 0.485 for all mixes) and exposed to 5% Na2SO4 solution at both
23 C and 5 C and tested according to CSA A3004-C8. The mortar
bars were measured regularly (according to CSA A3004-C8, proce-
dure A and B), and the solution was renewed regularly. When dete-
rioration was observed, mortar samples were studied with X-ray
diffraction (XRD) to evaluate which sulfate-bearing phases were
present and therefore, what form of sulfate attack was dominating.
The XRD samples were nely ground while still in a moist state and
immediately scanned from 5 2H to 90 2H at a scan rate of 0.02
per second using a Bruker D8 Advance spectrometer.
3. Results
Only the results from the control bars (100% cement), 25% Type
F y ash bars, and y ash and silica fume ternary bars in Na2SO4
solution are reported here to facilitate comparison of the different
C3A levels. Also, for ease of comparing the limestone contents
among different C3A contents, only GU-Mod, GUL-15-Mod,
GU-High, and GUL-High are reported here.
3.1. 23 C Na2SO4 solution

2. Material and methods
2.1. Cementitious materials
Two different clinker types were used for this study: a moder-
ate-C3A clinker (89% C3A), and a high-C3A clinker (1112% C3A).
The rst clinker was interground with two different limestone con-
tents (4% and 15% limestone by mass). Throughout the remainder
of the paper, these cements will be referred to as GU-Mod and
GUL-15-Mod. The high C3A clinker was interground with 4% and
10% by mass limestone, referred to as GU-High and GUL-High. Each
of the cements studied was blended with varying levels of supple-
mentary cementitious materials. See Table 2 for the chemical com-
positions of the cementitious materials, and Table 3 for mixture
proportions and exposure conditions.
2.2. Mortar testing
Mortar bars were cast with each of the cements (mixed and pro-
portioned according to CSA A3004-C1 and C2 except that the
water-to-cementitious-materials ratio (w/cm) was kept constant
Fig. 1 shows the expansion results for all four cements (both
high and moderate-C3A, GU and GUL cements) in combination
with y ash or ternary blends. The expansion up to 30 months
(130 weeks) in 23 C Na2SO4 is reported. Note: GUL-High + 5%
SF + 20% F ash was broken after 18 months in solution; therefore
further measurements were not possible. As per CSA A3004-C8
procedure A, all control samples failed and all SCM blends passed
the sulfate test dened as: 60.10% (Type MSb) or 60.05% (Type
HSb) expansion after 6 months or 60.10% (HSb) after 12 months,
see Table 1 above. Results were generally unaffected by C3A con-
tent or limestone content within the CSA A3004-C8 time frame.
3.2. 5 C Na2SO4 solution
Fig. 2 shows the expansion data up to 30 months (130 weeks)
for all four cements with y ash and ternary blend mortar bars
in 5 C Na2SO4.
The control mortar bars, cast with both moderate- and high-C3A
cements, with both limestone contents exceeded the maximum
expansion (60.10% after 18 months) permitted by CSA A3004-C8
procedure B for Portland limestone cements.

Table 1
Requirements for sulfate-resisting cements in Canada (CSA A3001-13).

Cement type Types Requirements

permitted
Portland cement (PC) MS or HS  Limits on C3A content
 14-Day expansion limit for mortar bars containing gypsum (7% SO4 by mass of cement)
Blended Portland cement containing MSb or  6-Monthb expansion limit (0.10% for MSb and 0.05% for HSb) for mortar bars in 5% Na2SO4 at 23 C
SCMa HSb
Portland limestone cement (PLC) PLC is not permitted in sulfate exposure classes unless it is used in combination with sufcient levels of SCM to meet the
requirements shown below
Blended Portland limestone cement MSLb or  6-Monthb expansion limit (0.10% for MSLb and 0.05% for HSLb) for mortar bars in 5% Na2SO4 at 23 C
containing SCMa HSLb  18-Month expansion limitc (0.10% for MSLb and HSLb) for mortar bars in 5% Na2SO4 at 5 C
 Minimum SCM replacement levels of 25% Type F y ash, 40% slag or 15% metakaolin, or of combinations of 5%
silica fume with 20% Type F y ash or 5% silica fume with 25% slag
a
SCM can be combined with either PC or PLC of the concrete mixture provided it is demonstrated that such combinations meet the requirements for blended PC or blended
PLC.
b
Mortar bars that exceed the 6-month expansion limit of 0.05% for Types HSb and HSLb, cements are still deemed to pass provided that the 12-month expansion does not
exceed 0.10%.
c
If the expansion between 12 months and 18 months exceeds 0.03%, the test must be continued until 24 months, and the 24-month expansion is not permitted to exceed
0.10%.
 A.M. Hossack, M.D.A. Thomas / Cement & Concrete Composites 56 (2015) 115120 117

Table 2
Chemical compositions of the cementitious materials (%).

Cements SiO2 Al2O3 Fe2O3 CaO MgO Na2O K2O SO3 LOI
GU-Mod 19.9 4.88 3.13 63.2 1.85 0.23 0.90 3.50
GUL-15-Mod 18.1 3.82 2.23 61.5 1.86 0.21 0.91 3.48
GU-High 19.6 5.33 2.12 61.8 2.36 0.21 1.22 4.17 2.68
GUL-High 18.3 5.00 2.04 59.8 2.25 0.20 1.10 3.99 6.69
Series 1 Supplementary cementitious materials
Type F y ash 57.8 18.0 9.37 2.96 1.99 1.32 2.03 1.12
Silica fume 96.7 0.30 0.10 0.40 0.30 0.10 0.70 0.09
Series 2 Supplementary cementitious materials
Type F y ash 48.5 19.0 13.6 5.24 2.26 2.52 1.87 2.45 3.22
Silica fume 93.2 1.41 0.20 0.44 0.59 0.20 1.13 0.15 2.35

The ternary bars with 10% limestone and high-C3A cement

Table 3
Mortar bar mixture proportions and exposure conditions.
GU-Mod
100% Cement 5% Na2SO4 at 23 C & 5 C
25% Type F y ash
20% F y ash +5% silica fume
GU-High
100% Cement 5% Na2SO4 at 23 C & 5 C
25% Type F y ash
15% F y ash +5% silica fume
All of the bars cast with high-C3A cement (GU-High, GUL-High)
and 25% y ash failed the requirement of expansion 60.10% after
18 months whereas the moderate-C3A, 25% y ash bars (GU-
Mod + 25% F ash) did not. The moderate-C3A bars (4% limestone)
failed the additional requirement of expansion 60.10% after
24 months if expansion is P0.03% between 12 and 18 months.
The moderate-C3A, 15% limestone bars (GUL-15-Mod + 25% F ash)
narrowly passed the test; expansion between 12 and 18 months
was 0.01%, therefore avoiding the requirement for expansion
60.10% after 24 months. See Table 1 for maximum expansion val-
ues permitted in CSA.
(GUL-High + 5% SF + 15% F ash) failed the requirement of expansion
60.10% after 18 months; all of the other ternary bars passed the
GUL-15-Mod requirements of the CSA A3004-C8 procedure B test.
4. Discussion
GUL-High
4.1. Performance at 23 C
The results indicate that, of the control samples (without SCM),
only GU-mod (GU control in Fig. 1 above) was able to resist sulfate
attack in the harsh 5% Na2SO4 solution and meet the expansion
requirements for a Type MSb cement. The GU-mod mortar bars
failed (0.194% expansion) at the next measurement (9 month) fol-
lowing the 6-month measurement required for classication as
Type MSb.
Expansion due to sulfate attack was extensive in all control
mortar bars, regardless of limestone or C3A content. However, at
23 C the mortar bars with the addition of y ash (GU + 25% F
ash, GUL + 25% F ash, GUL 15 + 25% F ash) or the ternary y ash
and silica fume blends (GU + 5% SF + 15% F ash, GUL + 5% SF + 15%
F ash, GU + 20% F ash + 5% SF, GUL 15 + 20% F ash + 5% SF) resisted
sulfate attack well; all bars achieved sulfate resistance equivalent

23C GU-High 23C GU-Mod

0.10 GU control 0.10 GU Control
GU + 25%Fash GU + 25% F ash
Expansion (%)

Expansion (%)

0.08 0.08
GU+5% SF+15% F ash GU+20% F ash+5% SF
0.06 0.06

0.04 0.04

0.02 0.02

0.00 0.00
0 6 12 18 24 30 0 6 12 18 24 30
Age (months) Age (months)

23C GUL-High 23C GUL-15-Mod

0.10 GUL Control 0.10 GUL 15 Control
GUL + 25% F ash GUL 15 + 25% F ash
Expansion (%)

Expansion (%)

0.08 0.08
GUL+5% SF+15% F ash GUL 15+20% F ash+5% SF
0.06 0.06

0.04 0.04

0.02 0.02

0.00 0.00
0 6 12 18 24 30 0 6 12 18 24 30
Age (months) Age (months)

Fig. 1. 30-Month expansion results, all cements, 23 C.

118 A.M. Hossack, M.D.A. Thomas / Cement & Concrete Composites 56 (2015) 115120

5C GU-High GU Control 5C GU-Mod GU Control

GU + 25% F ash GU + 25% F

0.10 0.10 ash
Expansion (%)

Expansion (%)
GU+5% SF+15% F 0.08 GU+20% F
0.08
ash ash+5% SF
0.06
0.06
0.04
0.04
0.02
0.02 0.00
0.00 -0.02
0 6 12 18 24 30 0 6 12 18 24 30
Age (months) Age (months)

5C GUL-High GUL Control 5C GUL-15-Mod GUL 15

Control
GUL + 25% F ash 0.10 GUL 15 + 25%
0.10
F ash
0.08
Expansion (%)

Expansion (%)
GUL+5% SF+15%
0.08 GUL 15 + 20%
F ash 0.06 F ash+5% SF
0.06
0.04
0.04 0.02
0.02 0.00
0.00 -0.02
0 6 12 18 24 30 0 6 12 18 24 30
Age (months) Age (months)

Fig. 2. 30-Month expansion results, all cements 5 C.

to a Type HSb (high-sulfate resisting blended Portland cement)
regardless of C3A or limestone content.
4.2. Performance at 5 C
At 5 C, 5% Na2SO4 solution, all of the control bars failed within
49 months in solution. Of the 25% Type F y ash bars, the high-
C3A bars (GU + 25% F ash, GUL + 25% F ash) failed in 46 months;
the moderate-C3A bars (GU + 25% F ash, GUL 15 + 25% F ash)
exceeded 0.10% expansion after 2 years in solution. Due to the
requirement that the expansion from 12 to 18 months must exceed
0.03% to warrant extending the test to 24 months the moderate-
C3A 15% limestone bars with 25% y ash (GUL 15 + 25% y ash)
would pass the requirements of CSA A3004-C8 for HSLb cement;
the extension of the test to 24 months would not be required.
The ternary y ashsilica fume mortar bars all survived at least
1 year in the 5 C 5% Na2SO4 solution. After 1 year, the GUL
High-C3A ternary mortar bars (GUL + 5% SF + 15% F ash) failed; all
of the other ternary mortar bars are intact.
4.3. Effect of temperature
In the present study the mortar bars cast with PCSCM blends
and PLCSCM blends both failed much sooner in 5 C than their
companion bars in 23 C solution. Several possible explanations
exist including: the propensity of thaumasite to form more rapidly
at lower temperatures [11]; or the reduced maturity of the SCM
blends at the time they are submerged in Na2SO4. The rapid forma-
tion of thaumasite at low temperatures does not appear to fully
explain the differences in the rates of degradation. Fig. 3 shows
XRD traces of three different cements revealing that after 100 days
in 23 C Na2SO4 solution and 70 days in 5 C Na2SO4 solution,
thaumasite was present in all three cements at both temperatures
regardless of limestone content (4%, 9%, and 15% interground
limestone). The 4% and 15% limestone cements are GU-High and
GUL-High discussed previously; the 9% limestone cement is com-
posed of the same clinker as the other cements, interground with
9% limestone. This leads to the question of the maturity of the
PCSCM blends and the PLCSCM blends.
Fly ash reacts much more slowly than Portland cement, and the
reaction may begin much later than Portland cement [15,16]. The
pozzolanic reaction relies on the calcium hydroxide produced by
Portland cement hydration. Therefore, the mortar cubes may reach
20 MPa before the y ash has begun to react or with minimal con-
tribution from the y ash. Once the mortar cubes have reached
20 MPa, the mortar bars are submerged in sodium sulfate solution.
The present CSA standards may require revision to account for the
delayed contribution of SCMs to Portland cement hydration.
In addition to the reliance on calcium hydroxide production, y
ash reaction is also strongly inuenced by temperature. The hydra-
tion of y ash is signicantly accelerated at elevated temperatures
and severely retarded at cold temperatures [17]. Therefore, if the
mortar bars are submerged in 5 C Na2SO4 after only one or two
days of curing, the y ash will not have an opportunity to contrib-
ute to the properties of the mortar; whereas, the bars submerged in
23 C solution will continue to hydrate. This would undoubtedly
lead to a more porous, permeable pore structure in the y ash
blended mortar bars in 5 C solution rather than 23 C solution.
The increased porosity could explain why the SCM-blend mortar
fails failed much sooner in 5 C solution than their companion bars
in 23 C solution. Further research is required in this area; PCSCM
and PLCSCM blends should be cured for a longer period of time,
allowing the y ash to react, before being submerged in cold tem-
perature sulfate solution.
4.4. Effects of C3A and limestone (CaCO3) contents
In the present study, the limestone content does not appear to
have had an effect on the rate of deterioration of the mortar bars.
In 5 C Na2SO4 solution, the GUL-High mortar bars failed in a
shorter time period than the GU-High mortar bars; however, it is
important to consider that this mix composition would not be per-
mitted in a sulfate environment due to the high-C3A content of the
 A.M. Hossack, M.D.A. Thomas / Cement & Concrete Composites 56 (2015) 115120
Fig. 3. XRD traces of control (no SCM) cements.
cement. All other mortars bars show little if any difference in the
performance of the GUL mortars compared to the GU mortars.
The effect of C3A content on the rate of expansion is much more
pronounced than the effect of limestone content. In 23 C sulfate
solution, the C3A content does not affect the age at failure of the
mortar bars. However, in 5 C sulfate solution, the high-C3A mortar
bars failed much sooner than the moderate-C3A mortar bars; on
average, the high-C3A bars failed in half the time of their moder-
ate-C3A companion mortar bars. This observation lends support
to the theory that ettringite formation is required prior to thaum-
asite formation and thaumasite forms from ettringite [6]. More
ettringite is formed in cements with higher alumina contents;
therefore, according to the theories suggesting that ettringite for-
mation is necessary for thaumasite formation, more thaumasite
can be expected with higher alumina contents also.
Thaumasite has a crystal structure very similar to that of
ettringite [18]. Other researchers [19,20] have theorized that
thaumasite uses ettringite as a basis for nucleation of thaumasite
crystals because of their very similar crystal structures. Thaumasite
then continues to form in the cement matrix. The observations in
119
the present study support this theory; ettringite formation is a nec-
essary precursor to thaumasite formation.
5. Conclusions
(1) The partial replacement of Portland cement with Type F y
ash improved the mortars resistance to external sulfate
attack at both 23 C and 5 C.
(2) The ternary blend of Portland cement, Type F y ash, and sil-
ica fume (GU + 5% SF + 15% F ash, GUL + 5% SF + 15% F ash,
GU + 20% F ash + 5% SF, GUL 15 + 20% F ash + 5% SF) further
improved resistance to external sulfate attack. The improve-
ment in sulfate resistance (with the addition of silica fume)
was very evident at 5 C, the silica fume had little effect at
23 C. The difference in the effect of silica fume at 23 C ver-
sus 5 C may be attributed to the ability of silica fume to
react rapidly in the short curing period prior to 5 C submer-
sion in sulfate solution.
(3) Particularly at 5 C, the moderate-C3A Portland cement mor-
tar bars (GU-Mod, GUL-15-Mod) exhibited much greater
120 A.M. Hossack, M.D.A. Thomas / Cement & Concrete Composites 56 (2015) 115120
resistance to sulfate attack than the high-C3A mortar bars
(GU-High, GUL-High). No difference in performance was
observed in 23 C solution.
(4) No notable relationship was observed between the inter-
ground limestone content and the age at failure of the mor-
tar bars at either temperature.
Acknowledgements
The authors would like to thank the Natural Sciences and
Engineering Research Council of Canada (NSERC), the Portland
Cement Association (PCA) (Research Fellowship F11-02), as well
as the Cement Association of Canada (CAC) for their nancial sup-
port throughout this study.
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