Construction and Building Materials 249 (2020) 118224

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Construction and Building Materials

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

External sulfate attack on concrete under combined effects of flexural

fatigue loading and drying-wetting cycles
Fang Liu a,b,⇑, Zhanping You c, Aboelkasim Diab d, Zhuangzhuang Liu b, Chao Zhang f, Shuaicheng Guo e,f,⇑
a
Faculty of Transportation Engineering, Huaiyin Institute of Technology, Huai’an, Jiangsu 223003, China
b
School of Highway, Chang’an University, South Erhuan Middle Section, Xi’an, Shaanxi 710064, China
c
Department of Civil and Environmental Engineering, Michigan Technological University, 1400 Townsend Drive, Houghton, MI 49931, USA
d
Department of Civil Engineering, Aswan University, 81542, Egypt
e
Key Laboratory for Green & Advanced Civil Engineering Materials and Application Technology of Hunan Province, College of Civil Engineering, Hunan University,
Changsha 410082, China
f
Key Laboratory of Building Safety and Energy Efficiency of the Ministry of Education, Hunan University, Changsha 410082, China

h i g h l i g h t s

Sulfate attack on concrete under flexural fatigue loading and drying-wetting cycles simultaneously was investigated.

Flexural fatigue loading incorporated with drying-wetting cycles can accelerate the sulfate corrosion of concrete.

The stress level of flexural fatigue loading acts an important role in combined actions.

The phase composition of corrosion products was analyzed using XRD.

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

Article history: The concrete transportation infrastructures will undergo both fatigue traffic loading and environmental
Received 19 July 2019 impacts during the whole service life, including rigid pavements, bridges decks, airfield runways, railway
Received in revised form 17 December 2019 bridges, even high-speed railways and concrete structures in the ocean. This study aims to investigate the
Accepted 18 January 2020
effects of external sulfate attack on concrete under flexural fatigue loading and drying-wetting cycles.
The changes of mass loss rate and relative dynamic elastic modulus were measured to indicate the influ-
ence of the coupled effects on the integrity and mechanical performance of concrete, also the sulfate con-
Keywords:
tent inside concrete was determined to indicate the permeability of sulfate ion under different
Sulfate attack
Flexural fatigue loading
experimental conditions. Moreover, the phase composition of samples was analyzed using X-ray diffrac-
Drying-wetting cycles tion (XRD). In addition, the effect of fly ash on sulfate attack was duly studied. Fatigue loading causes
Relative dynamic elastic modulus cracking in the interfaces of various phases and forms cracks in the concrete. Within the influence depth
Mass loss rate of drying-wetting cycles, concrete is subjected to both water convection due to capillary action and dif-
fusion due to concentration gradients. The results indicate the fatigue loading and drying-wetting cycles
can accelerate the transportation of sulfate ion inside concrete and the deterioration degree of concrete
subjected to sulfate. The findings in this study can help to understand the influence of fatigue loading and
drying-wetting cycles on the development of sulfate attack.
Ó 2020 Published by Elsevier Ltd.

1. Introduction

Sulfate attack is one of the most severe threats to the long-term

⇑ Corresponding authors at: Faculty of Transportation Engineering, Huaiyin
Institute of Technology, Huai’an, Jiangsu 223003, China (F. Liu), Key Laboratory
for Green & Advanced Civil Engineering Materials and Application Technology of
Hunan Province, College of Civil Engineering, Hunan University, Changsha 410082,
China (S. Guo).
E-mail addresses: cherry1226@yeah.net (F. Liu), scguo@hnu.edu.cn (S. Guo).
performance of the concrete infrastructure [1]. The previous study
has well understood the material damage mechanism [2–4], dam-
age characterization [5–7], phase formation [8,9], damage evalua-
tion [10–12], expansion mechanism of sulfate erosion, and
chemo-mechanical modeling [13–15]. However, the knowledge
gap on the development of sulfate attack under field conditions
still exit. The former studies indicated that, besides the traffic

https://doi.org/10.1016/j.conbuildmat.2020.118224
0950-0618/Ó 2020 Published by Elsevier Ltd.
2 F. Liu et al. / Construction and Building Materials 249 (2020) 118224
loading, the environmental factors can also deteriorate the trans-
portation structure [16,17]. Brown and Taylor [18] pointed out that
field-like conditions should be considered in the experimental
work and be related to field observations.
In recent years, sulfate attack with existing environmental and
mechanical factors have attracted the attention of scholars, such as
sulfate attack under drying-wetting and heating–cooling environ-
ments [19,20], frost action [21–23], static flexural loading
[24,25], flexural fatigue loading [26], static flexural loading and
drying-wetting cycles [27–30], static flexural loading and freeze–
thaw cycles [31]. Specifically, the study by Steindl et al. [32] build
a novel powder protocol to examine the sulfate resistance of eco-
concrete. These studies manifest that environmental and mechan-
ical factors have different degrees of effects on sulfate attack. Some
concrete structures in service, such as structures under earthquake,
pavement slabs, bridges decks, airfield runways, railway bridges,
even high-speed railways and concrete structures in the ocean
have to undergo fatigue loading [33] and environmental impacts
simultaneously. Recently, some studies on fatigue loading and
environmental factors are reported [26,34,35]. Currently the chem-
ical sequences of sulfate attack in concrete has been widely studied
and its reaction mechanism has been thoroughly understood [36].
Meanwhile, the current understanding on the correlation between
external loading and sulfate attack is still under investigation,
especially the fatigue loading. Specifically, the study by Yan et al.
[37] indicated compressive fatigue loading at the stress level larger
than 0.7 could promote the entrance of sulfate ions into the con-
crete. Besides that, the study by You et al. [38] Zhang et al. [39]
and Long et al. [40] focused on the combined effects of loading
and sulfate attack on the expanded polystyrene concrete, magne-
sium sulfate cement and fly-ash based geopolymer concrete,
respectively. At present the understanding on the coupling effects
between flexural fatigue loading and sulfate attack is still quite
limited. This study aims to partially fill the knowledge gap by
in-situ examining the concrete material with the combined actions
of fatigue loading, drying-wetting cycles and sulfate attack
simultaneously.
Also to enhance the sulfate resistance of concrete, supplemen-
tary cementitious materials has been added into concrete to
improve its durability performance. The study by Ghafoori et al.
[41] indicated that, compared to the nanoscale silica, the micro-
scale silica is more efficient to improve the sulfate resistance of
mortar samples. Also the sulfate resistance of the nanoscale silica
modified concrete highly depend on the dispersion effect [42].
The study by Jin et al. [43] indicated the added fly ash can help
to prohibit the entrance of sulfate ions into concrete and then
enhance its resistance to sulfate attack. Similar results were also
reported in the study of Ghafoori et al [44]. The application of class
F fly ash has been proved to be an efficient and cost-effective
method to enhance the sulfate resistance of concrete [45].
To in-situ study the combined effects of sulfate attack and dry-
ing–wetting cycles, various protocols have been proposed in for-
mer studies. Yuan et al. [19] adopted a drying-wetting cycle
regime consisted of 8 h drying with 70 ℃ in the oven and keeping
2 h cooling, next soaking in the sulfate solution for 16 h, to inves-
tigating the failure process of concrete under the coupled actions
between sulfate attack and drying-wetting cycles by using X-ray
CT. Gao et al. [27] adopted a similar regime consisted of drying
at a temperature of 60℃ for 45 h and cooling down in the air at
a room temperature for 3 h, then immersing in the sulfate solution
at room temperature for 21 h, following by 3 h drying in air. Previ-
ous studies have shown that the erosive product ettringite will
become unstable and the erosion mechanism will change when
the heating temperature exceeds 70 °C, therefore, in this study,
the drying temperature with 60 °C is taken. Chaube et al. [46]
pointed out that the evaporation process of water in concrete sig-
nificantly lagged behind the moisture process during the drying-
wetting cycles, the ‘‘ink-bottle effect” is the main cause of this phe-
nomenon. In order to speed up the test process, the drying time
should be longer than the soaking time, at the same time, a buffer-
ing period is set between the immersion and the drying to prevent
the temperature stress caused by subcooling and overheating. Cur-
rently, it is still difficult for the existing instrument to adequately
in-situ analyze the combined effects of fatigue loading, drying-
wetting cycles and sulfate attack on concrete materials.
Motivated by current status, this research aims to evaluate the
effects of flexural fatigue loading and drying-wetting cycles on the
mortar specimens that are exposed to an external sulfate solution.
In this study, an experimental system was improved based on
existing instrument [47] to simulate the impact of flexural fatigue
loading and environmental factors on the sulfate erosion of con-
crete. At regular time intervals, the mass loss rate, relative dynamic
elastic modulus, and sulfate ion content in layer sample were mea-
sured. In addition, the corrosion products of interior concrete are
examined using XRD. This research is beneficial to providing a ref-
erence to the durability evaluation of concrete structures in service
suffering from sulfate attack and durability design of concrete
structures to be built.
2. Materials, methods, and calculations
2.1. Materials
Ordinary Portland cement with the strength grade 42.5 was
used in this study, which was produced by Ji-dong Cement Com-
pany in Shaanxi Province, China. Class F fly ash produced by San-
menxia Thermal Power Plant was utilized, which is selected
based on the recommendation in reference [43]. The contents of
main oxides in cement and fly ash are given in Table 1. The lime-
stone with an apparent density of 2.714 g/cm3 was selected as
coarse aggregate (size range is 5–25 mm). River sand with 2.74
fineness modulus was used in this study (apparent density is
2.630 g/cm3). The polycarboxylic acid water-reducing agent was
used as the concrete admixture produced by a building scientific
research institute. The above materials were all mixed with tap
water and the mix proportion of concrete is shown in Table 2.
The prismy specimens of 100 mm  100 mm  400 mm were pre-
pared for the test.
2.2. Method and calculations
2.2.1. Flexural fatigue loading
There has no existing equipment to consider the combined
impacts of flexural fatigue loading and environmental factors with
the presence of the sulfate attack on concrete. Therefore, an exper-
imental system was improved based on existing instrument in this
research. The experimental system of sulfate attack under flexural
fatigue loading and drying-wetting cycles is shown in Fig. 1. The
device uses brackets, beams, motors, pressure heads, force value
sensors, etc. to form stress loading components. The maximum
and minimum values of the alternating load and the frequency of
the alternating load are controlled by electronically controlling
the meter and the frequency converter. The simulation parts of
drying-wetting cycles and sulfate attack are composed of environ-
mental chambers, heaters, temperature sensors, etc., and the tem-
perature of the heating is controlled by a temperature control
apparatus. The specimens are stacked one to another in the exper-
imental box. According to the basic mechanical properties of con-
crete, concrete subjected to bending stress, when the
corresponding stress is about 60% of its ultimate strength, it is in
an unstable state. In this study, three maximum stress levels were
 F. Liu et al. / Construction and Building Materials 249 (2020) 118224 3

Table 1
Contents of main oxides in cement/fly ash based on XRF analysis (% by mass).

Main oxide CaO SiO2 Al2O3 Fe2O3 MgO Na2O K2O SO3
Cement (%) 60.28 21.7 5.66 3.12 1.52 0.37 0.55 2.1
Fly ash (%) 3.93 53.25 28.75 4.94 1.59 0.54 1.92 1.7

Table 2
Mix proportion of concrete.

Water-binder ratio Cement Fly ash Water Sand Coarse aggregate Water reducing agent 28d Flexural strength
kgm3 kgm3 kgm3 kgm3 kgm3 kgm3 (MPa)
0.4 440 0 176 642 1192 1.54 5.91
308 132 176 642 1192 0.88 4.28

Fig. 1. Experimental system of sulfate attack under flexural fatigue loading and drying-wetting cycles: (a) loading diagram (b) loading scheme (c) field test device.

selected as 20%, 35%, and 50%; the minimum stress level was one-
tenth of the corresponding maximum stress level. During the stress
loading procedure, the loading and unloading remained 1.5 min,
and that was 3 min per one cycle and 480 cycles every day. In this
study, the loading and unloading cycles were set as 86,400 during
180 d, which could reflect the field fatigues of pavement slabs,
bridge decks, airfield runways, railway sleepers and bridges whose
service life fatigue cycle number was believed between 103 and 107
[48].
2.2.2. Drying-wetting cycle regime
At present, there is no uniform regulation for the drying-
wetting cycle regime. With regard to anti-sulfate attack test in
Standard GB/T 50082–2009 [49], heating temperature of
4 F. Liu et al. / Construction and Building Materials 249 (2020) 118224

(80 ± 5) °C was designed in drying phase. In order to speed up the
test process, the drying time should be longer than the soaking
time, at the same time, a buffering period is set between the
immersion and the drying to prevent the temperature stress
caused by subcooling and overheating. In this research, the
drying-wetting alternate system was adopted and the procedure
was as following: firstly, the standard curing specimens for 28 d
were baked at 60 °C for 24 h in the oven then cooled to room tem-
perature. The dried specimens were immersed in sulfate solution
for 10 h followed by drying for 1 h at room temperature then were
baked at 60 °C for 36 h in the environmental box and finally cooled
for 1 h in the air. The newly prepared corrosion solution replaced
the original solution every 20 d to ensure that a little change in
concentration under the corrosion environment of the concrete
specimens.
2.2.3. Testing scheme
In order to show the deterioration of concrete under different
exposure conditions subjected to sulfate, in this study, sulfate
attack under continuous soaking was considered to compare with
the combined effects of sulfate attack and drying-wetting cycles;
also sulfate attack under flexural fatigue loading and drying-
wetting cycles was investigated. The studied conditions of sulfate
attack under different factors are shown in Table 3.
2.2.4. Mass loss rate
Specimens with the size of 100 mm  100 mm  400 mm were
used and three replicates were made to verify reproducibility of
results in this experiment. The mass loss rate of the concrete spec-
imen was calculated using equation (1), as following:
W0  Wt
DW t ¼  100%
W0
where DW t : mass loss rate of concrete specimens at corrosion
age t;
(which calculated as the average of the three specimens, %);
W 0 : mass of concrete specimens before corrosion, g; and
W t : mass of concrete specimens at corrosion age t, g.
2.2.5. Relative dynamic elastic modulus
The dynamic elastic modulus can be used to characterize the
degree of damage for concrete specimen under different expo-
sure conditions subjected to sulfate, and to assess the durability
of concrete. In this study, DT-16 concrete dynamic elastic
modulus tester was used to measure the concrete samples
(100 mm  100 mm  400 mm) at regular time intervals. Relative
dynamic elastic modulus is calculated using equation (2), as
following:
Edt
Erd ¼
Ed0
whereErd : relative dynamic elastic modulus;
Edt : dynamic elastic modulus of concrete specimens at corrosion
age t; and
Ed0 : dynamic elastic modulus of concrete specimens before
corrosion
2.2.6. Sulfate ion content
Concrete specimens at specific corrosion age were obtained by
drilling cores firstly then cores were cut into layers at certain thick-
nesses. The thicknesses of each slice were 2 mm (first layer), 3 mm
(second layer), and 5 mm (third layer and the subsequent). The
naturally dry slices were put into the agate mortar, broken and
repeated grinded then sieved through 0.08 mm size sieve. Sulfate
ion content of powder samples will be measured via barium sulfate
gravimetric method according to JTJ270-98 [50], and sulfate ion
content of concrete is calculated using equation (3), as following:
1:2  0:343  ðm2  m1 Þ
W SO2 ¼  100% ð3Þ
4 m
where W SO2 : sulfate ion content of concrete (accurate to
4
0.01%);
m1 : mass of porcelain crucible;
m2 : total mass of sediment and porcelain crucible; and
m: mass of concrete powder samples;
where 0.343 and 1.2 represent the converted coefficient from
BaSO4 to SO3 and the converted coefficient from SO3 to SO24 - ,
respectively.
Fig. 2 shows the measurement process of sulfate ion content in
ð1Þ concrete. Here, the initial sulfate-ion contents of two kinds of con-
crete, listed in Table 2, are 0.859%, 0.801%, respectively. That is, the
final value obtained from barium sulfate gravimetric method
should be subtracted with 0.859% or 0.801%.
3. Results and discussion
3.1. Mass loss rate
The variation of the mass loss rate of concrete specimens with
erosion time, to a certain extent, reflects the deterioration rule of
concrete due to erosion. The changes in mass loss rate under differ-
ent exposure conditions subjected to sulfate are depicted in Fig. 3
and Fig. 4.
From Fig. 3, negative growth in the mass loss rate of the speci-
mens L10, G10, and G5 was noticed, among which, the mass gain of
specimen L10 was the slowest while the specimen G10 had the
maximum gain. The mass loss rate of the specimen G10F30 has
negative growth firstly, then turns positive. The specimens L10
ð2Þ
were continuously soaked in sulfate sodium solutions, mass gain

Table 3
Experimental conditions of sulfate attack under different factors.

Specimen Days of continuous Times of drying-wetting Stress level of flexural fatigue Concentration of sodium sulfate Content of fly ash (mass
code soaking cycles loading (mass fraction) ratio)
L10 180 0 0 10% 0
G10 0 90 0 10% 0
G5 0 90 0 5% 0
G10F30 0 90 0 10% 30%
G10DS20 0 90 20% 10% 0
G10DS35 0 90 35% 10% 0
G10DS50 0 90 50% 10% 0

Note: L-full immersion, G-drying-wetting cycle, F-fly ash DS-stress level of flexural fatigue loading. The numbers after G, L stand for the sulfate concentration, the number
after F stands for the content of fly ash, and the numbers after DS stand for the stress level.
 F. Liu et al. / Construction and Building Materials 249 (2020) 118224 5

Fig. 2. Measurement process for sulfate ion content in concrete:(a) drilling core (b) core samples (c)slicing (d) slicing samples (e) grinding (f) weighing before titration (g)
dissolving (h) filtering (i) adding 10% BaCl2 solution (j) static setting (k) filtering and washing (l) weighing empty crucible (m) ashing (n) burning in high temperature furnace
(o) weighing precipitate + crucible.

depends on two reasons: one is on account of water absorption and
further hydration, the other is that expansive erosion products fill
micro pores and cracks in matrix. The study by Ikumi et al. [10] indi-
cated the deterioration at microscale level can be generated by both
external chemical attack [51] and external loadings. In comparison
with drying-wetting cycles, the mass gain of specimen L10 is less
than that of specimen G10. Drying and wetting cycles accelerate
sulfate diffusion to concrete through humidity gradient of cycles
and aggravate the deterioration of concrete. The mass loss rate of
the specimens L10, G10 for 180 d was 1.313% and 2.078%,
respectively. The specimen G5 in the mass loss rate exhibited a
similar trend to the specimen G10, while the degree of change is
different. After 180 d, the mass loss rate of the specimen G5 was
1.273%. Under high-concentration Na2 SO4 solution (mass frac-
tion), the speed of generating expansive products is faster; the
mass gain is also faster, so the absolute value of mass loss rate is
higher. The mass loss rate of the specimen G10F30 for 180 d was
0.619%, negative growth at first, then the forming surface of
6 F. Liu et al. / Construction and Building Materials 249 (2020) 118224
Fig. 3. Changes of mass loss rate for concrete under drying-wetting cycles and
sulfate.
Fig. 4. Changes of mass loss rate for concrete exposed to sulfate attack under
drying-wetting cycles and flexural fatigue loading.
concrete specimen emerging peeling, the mass gain was not
enough to resist the mass loss due to forming surface peeling, so
the mass loss rate was from negative to positive.
From Fig. 4, the mass loss rate of the specimens G10DS20 and
G10DS35 both have negative growth firstly, then mass gain
become smaller after reaching the extreme value, the magnitude
of mass gain is greater than that of G10. A lot of specimens
G10DS50 were broken and the longest time that the specimen
can bear for the experiment was 70 d, the mass gain of the speci-
men G10DS50 was the largest. After 180 d, the mass loss rate of the
specimens G10DS35 and G10DS20 were 0.458%, 1.345%,
respectively. Compared with that of the specimen G10, the speci-
mens G10DS35 and G10DS20 firstly showed a negative maximum,
then increased, and the negative maximum of the specimen
G10DS35 is earlier than the specimen G10DS20.
The fatigue loading generates cracks and accelerates the dam-
age process of concrete under drying-wetting cycles and sulfate
attack, so the negative growth rate of the mass loss for the speci-
mens was sooner than that of G10.
3.2. Relative dynamic elastic modulus
The changes in relative dynamic elastic modulus with different
experimental conditions are shown in Figs. 5 and 6. Dynamic elas-
tic modulus of concrete specimens will change under sulfate envi-
ronment. In this study, relative dynamic elastic modulus was used
to characterize the damage inside the concrete.
From Fig. 5, relative dynamic elastic modulus of the concrete
specimens L10 first has a significant increasing then rises slowly.
After 180 d, relative dynamic elastic modulus of specimens L10
was 1.058, thus it could be seen that the damage process of con-
crete caused by continuous soaking in 10%Na2 SO4 solution is very
slow. Relative dynamic elastic modulus of the specimens G10
was 0.797 after 180 d. The reduction is caused by the sulfate accu-
mulated during drying-wetting cycles and the generated crystal-
lized expansion [52]. The crystallization of sulfate salt will lead
to crystallization pressure [53,54] and thus accelerated the damage
process obviously with the number of cycles [55]. Relative dynamic
elastic modulus of the specimens G5 was 0.854 after 180 d of
drying-wetting cycles. There is a similar trend in relative dynamic
elastic modulus between the specimens G10 and G5, increases
firstly then decreases, however, the degree of loss is different.
The rise and fall of the specimen G10 are larger than G5. Under
high-quality fraction ofNa2 SO4 solution, the speed of generating
expansive products is faster, so the expansion stress is also larger,
crack propagation is faster, and the degree of degradation is more
obvious. Relative dynamic elastic modulus of the specimens
G10F30 was 0.943 after 180 d of drying-wetting cycles and the
decreasing degree is smaller than that of the specimen G10. It
was clear that the fly ash concrete has the better performance in
terms of the resistance of concrete to sulfate attack. This is proba-
bly due to the reduction of pore sizes, filling and the pozzolanic
effect, which results in an improvement in the resistance to sulfate
attack of concrete, to some extent [56–58].
From Fig. 6, relative dynamic elastic modulus of the specimens
G10DS50 declined at the beginning after 70 d and the value of rel-
ative dynamic elastic modulus was 0.919. A lot of specimens
G10DS50 were broken, thus the longest time that the specimen
can bear for the experiment was 70 d. Among these broken con-
crete specimens, it was found that its relative elastic modulus
declines sharply before the brittle fracture. This also proves that
relative dynamic elastic modulus could characterize the damage
inside the concrete. The mechanical damage caused by high stress
Fig. 5. Changes of relative dynamic elastic modulus for concrete under drying-
wetting cycles and sulfate.
 F. Liu et al. / Construction and Building Materials 249 (2020) 118224 7

Fig. 6. Changes of relative dynamic elastic modulus for concrete exposed to sulfate Fig. 7. SO2
4 Concentration depends on the depth for concrete under drying-wetting

attack under drying-wetting cycles and flexural fatigue loading. cycles and sulfate.

level of fatigue loading (50%) was the main factor leading to the
deterioration of the concrete. Relative dynamic elastic modulus
of the specimens G10DS35 was 0.732 after 180 d and the variation
curve with time was going down all the time. Relative dynamic
elastic modulus of the specimens G10DS20 increased with corro-
sion time in the early state, decreased afterwards, and relative
dynamic elastic modulus was 0.773 after 180 d. Relative dynamic
elastic modulus of the specimens G10DS20 and G10DS35 was
smaller than that of the specimen G10. The higher the stress level
of flexural fatigue loading, the faster the decrease in relative
dynamic elastic modulus will be. The flexural fatigue loading accel-
erates the propagation of micro-cracks within the concrete,
thereby expanding the diffusion of sulfate into the interior of the
concrete. The generation of micro-cracks together with the sulfate
attack and drying-wetting cycle action made concrete deteriorate
rather quickly.

3.3. SO2
4 concentration depending on depth

Figs. 7 and 8 depict the changes in SO24 concentration with the
depth for the specimens after 180 d. The transport of sulfate ions
from the erosion solution to the interior of the concrete is a gradual
transfer process.
From Fig. 7, with the increase of erosion depth, the content of
sulfate ions reduced significantly. With the growth of erosion
age, sulfate ion from the erosion solution into the shallow layer
of concrete increases, which would produce a chemical reaction
with cement hydration products in concrete, thus generating gyp-
sum, ettringite, and other erosion products [59–61]. Due to the fill-
ing and compaction effects of erosion products, hindering the
further transport of sulfate ions into the interior of the concrete,
there had a certain enrichment of the surface sulfate ion distribu-
tion; concrete with larger depth was relatively lagged by the sul-
fate ion attack, so that the content of sulfate ions reduced
significantly with the increase of erosion depth.
Fig. 7 also shows that each specimen has different erosion
depth; the maximum erosion depth of the specimen L10 was
7.5 mm, and the content of sulfate ion in the first three layers of
L10 concrete was 3.524%, 1.695%, and 1.254%, respectively. The
maximum erosion depth of the specimen G10 was 12.5 mm, and
the content of sulfate ion in the first four layers of G10 was
4.282%, 4.558%, 1.988%, and 0.558%, respectively. Under drying-
wetting cycles, the transmission of sulfate ions in concrete can
Fig. 8. SO2
4 Concentration depends on the depth for concrete exposed to sulfate
attack under drying-wetting cycles and flexural fatigue loading.
be regarded as the coupling of convection caused by capillary
action and the diffusion caused by concentration gradient, while
under continuous soaking, the transmission of sulfate ions in con-
crete is dominated by diffusion. The maximum erosion depth of the
specimen G5 was also 12.5 mm while the amount of sulfate ions
per erosion depth was less than that of G10. The maximum erosion
depth of G10F30 was 7.5 mm, and its sulfate ions content
decreased the fastest with erosion depth. Compared with G10, it
was also confirmed that the addition of admixtures can improve
the ability of sulfate resistance of concrete when it is subjected
to drying-wetting cycles.
The effect of compressive stress on the sulfate ion transport
properties is not significant as it is basically the same as the non-
stress state. Compared with the acceleration effect of tensile stress
in tensile zone on the ion transmission, the compressive stress of
the compression zone has a smaller effect on the ion transport,
so in this research, only the distribution of sulfate ion in the ten-
sion zone is analyzed.
As the stress level of fatigue loading was relatively high, the
fracture of the specimen G10DS50 was earlier than that of the
8 F. Liu et al. / Construction and Building Materials 249 (2020) 118224
experimental design, thus there has no curve of sulfate ion evolu-
tion for the specimen G10DS50 in Fig. 8. The maximum erosion
depth of the specimen G10DS20 was 12.5 mm and the content of
sulfate ion in the first four layers of G10DS20 concrete was
5.289%, 4.743%, 2.257%, and 0.837%, respectively. The maximum
erosion depth of the specimen G10DS35 was also 12.5 mm and
the content of sulfate ion in the first four layers of G10DS35 con-
crete was 5.809%, 5.078%, 3.056%, and 1.469%, respectively.
The erosion depth is also shown in Fig. 8. The content of sulfate
ions in Fig. 8 can be arranged as G10DS35 > G10DS20 > G10. With-
out flexural fatigue loading, the sulfate ion contents of the speci-
men G10 were much lower than those of specimens G10DS35
and G10DS20. The stress level had a positive effect on sulfate ion
in layers. The greater the stress level, the higher the sulfate ion
content will be. More discrete small cracks generated under fatigue
loading at first. With the increase in the number of cycles, gener-
ated new cracks and initiated the expansion of the original crack,
which provided a channel for the entry of sulfate ions into the inte-
rior of the concrete. On the same time, drying and wetting cycles
accelerated sulfate ion diffusion into concrete through humidity
gradient of cycles, so more sulfate ions reacted with hydration
products of cement and generated expansive erosion products.
When the internal stress of expansion exceeded the tensile
strength of concrete, cracks generated. The fatigue stress acceler-
ated the corrosion, and the corrosion exacerbated the fatigue dam-
age of the material.
3.4. The corrosion products of interior concrete
X-ray diffraction analysis of ground powder samples at different
depth was carried out using a D8 ADVANCE X-ray diffractometer
manufactured by Bruker AXS Co., Ltd. The XRD pattern obtained
from the experiment was compared with the standard diffraction
pattern in the database to determine the phase of the crystal in
the sample. XRD patterns at different depth for specimen
G10DS35 under the combined actions of sulfate attack, drying-
wetting cycles, and flexural fatigue loading simultaneously after
180 d are shown in Fig. 9.
As can be seen from Fig. 9, the diffraction peak of ettringite
appeared in the corrosion product of concrete surface layer under
the actions of 35% flexural fatigue load after erosion for 180 days. A
diffraction peak of ettringite and gypsum appeared in the corrosion
product of the second layer (1 cm), wherein the diffraction peak of
Fig. 9. XRD patterns at different depth for specimen G10DS35.
the gypsum was very low, which was related to the low gypsum
content in the corrosion product. There was no diffraction peak
of ettringite or gypsum in the corrosion product of the inner layer
(2 cm), indicating that sulfate ion did not erode to the inner layer.
3.5. Discussion
This research aims to study the durability performance of the
concrete transportation structures under the combined environ-
mental and mechanical loadings. During its service life, the trans-
portation structures will be impacted by the repeated dynamic
traffic loading, which will lead to fatigue damage of the concrete
infrastructure. Specifically, the flexural fatigue loading can crack
the concrete and also lead to the entrance of the sulfate ions into
concrete. But the study between the coupling effects of fatigue
loading and sulfate attack is still quite limited. The results in this
study support that the flexural fatigue loading can accelerate the
development of sulfate attack by enhancing the transportation of
the sulfate ion. Also the drying-wetting cycles are to simulate the
drying condition in the western China, where drying-wetting
cycles can also deteriorate concrete materials, especially the struc-
tures exposed to sulfate condition. The reduction effect of the fly-
ash used in this study can be generated by three mechanisms.
The reaction mechanism of the sulfate attack is now clear that
the sulfate ions entered into concrete will first react with the
Ca2+ to form gypsum. Then the gypsum will react with the C3A to
form the expansive ettringite material [36]. Hence, the mitigation
mechanism of the fly-ash can be explained in these aspects. Firstly
the fly-ash can consume the generated lime due to cement hydra-
tion through the pozzolanic reaction [62]. After the entrance of sul-
fate ions, the generation of gypsum in concrete can then be
prohibited due to reduced lime content. Secondly, the fly ash mate-
rial can lead to a denser internal structure and prohibited the
entrance of sulfate ions [63]. Finally, replacing Portland cement
with fly ash can reduce the amount of C3A [64] and then the reac-
tion between C3A and generated gypsum can be diminished. The
reduction mechanism for other Supplementary Cementitious
Materials (SCMs) is similar to that of the fly ash. The further studies
also indicated better sulfate resistance can be achieved by adding
silica fume [65].
The former studies indicate that the MgSO4 can lead to severer
threat to the durability performance of concrete compared to that
of Na2SO4 [66] used in this study. Besides the sulfate ion, the Mg2+
will also react the lime content and the magnesium hydroxide can be
generated during the process [67]. Besides that, the Mg2+ can also
lead to the destabilization of the C-S-H phase [68] by replacing the
contained calcium content. Hence the future study will try to study
the coupling effects between flexural fatigue loading and the
explosion to MgSO4 environment. Furthermore, the former study
the silica fume is more effective to enhance the resistance to
MgSO4 compared to that of other SCMs [65].
4. Conclusions
In this paper, external sulfate attack under flexural fatigue load-
ing and drying-wetting cycles was investigated. The mass loss rate,
relative dynamic elastic modulus, and sulfate ion content were
measured under sulfate attack incorporating with flexural fatigue
loading and drying-wetting cycles. Moreover, the phase composi-
tion of attached samples was analyzed using XRD. The conclusions
are summarized as following:
(1) The reduction on relative dynamic modulus is more obvious
for specimens under drying-wetting cycles and sulfate
attack compared to the specimens under sulfate attack.
 F. Liu et al. / Construction and Building Materials 249 (2020) 118224
Drying-wetting cycles accelerate the sulfate accumulation in
concrete and aggravate the damage degree of concrete subjected
to sulfate attack. However, it should be cautious to choose appro-
priate drying-wetting cycle regime.
(2) Concrete with the addition of 30% fly ash had the better per-
formance in terms of the resistance to sulfate attack and
drying-wetting cycles. The degree of concrete degradation
was more obvious under high-concentration sodium sulfate
solution (mass fraction) and drying-wetting cycles.
(3) The fatigue loading can accelerate the development of sul-
fate attack by increasing the cracks and transportation of
the sulfate ion, which then can lead larger amount of sulfate
ion in the pore solution and then higher expansion force. The
acceleration effect can be further examined with higher
stress level.
CRedit authorship contribution statement
Fang Liu: Conceptualization, Methodology, Software, Formal
analysis, Investigation, Resources, Data curation, Visualization.
Zhanping You: Conceptualization, Methodology, Resources, Super-
vision, Project administration, Funding acquisition. Aboelkasim
Diab: Software, Formal analysis, Investigation. Zhuangzhuang
Liu: Software, Validation, Formal analysis, Investigation, Resources,
Data curation. Chao Zhang: . Shuaicheng Guo: Conceptualization,
Methodology, Visualization, Supervision, Project administration,
Funding acquisition.
Acknowledgements
This study was sponsored by the Construction System Science
and Technology Project of Jiangsu Province (Grant Number:
2019ZD001229) and National Key R&D Program of China. Shuai-
cheng Guo acknowledges the financial support from the China
Scholarship Council under No. 201406370141.
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