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Construction and Building Materials 40 (2013) 10211028

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Construction and Building Materials


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

A visual investigation on chloride ingress into ceramic waste aggregate


mortars having different water to cement ratios
Hiroshi Higashiyama a,, Kiyoshi Yamauchi a, Manote Sappakittipakorn b, Masanori Sano c,
Osamu Takahashi c
a
b
c

Department of Civil and Environmental Engineering, Kinki University, 3-4-1, Kowakae, Higashiosaka, Osaka 577-8502, Japan
Department of Civil Engineering, King Mongkuts University of Technology North Bangkok, 1518, Pracharat 1 Rd., Bangsue, Bangkok 10800, Thailand
The Kanden L&A Company, Ltd., 1-3-12, Shinmachi, Nishi-ku, Osaka 550-0013, Japan

h i g h l i g h t s
" The compressive strength of the CWA mortars was similar to that of the RS mortars.
" The chloride concentration of the CWA mortars was lower than that of the RS mortars.
" The CWA mortars had lower apparent chloride diffusion than the RS mortars.

a r t i c l e

i n f o

Article history:
Received 16 August 2012
Received in revised form 11 October 2012
Accepted 21 November 2012
Available online 28 December 2012
Keywords:
Porcelain insulator waste
Mortar
Chloride ingress
W/C
EPMA

a b s t r a c t
In reinforced concrete structures, chloride ingress causes deleterious consequences due to corrosion of
steel reinforcement. With no protective means, the service life of the structures is shortened proportionately to the rate of chloride ingress designated as a coefcient of chloride diffusion. Previous experimental study using the rapid chloride migration test has indicated that the use of ceramic waste aggregate
(CWA) is effective in lowering the chloride diffusion coefcient of the 0.5 water to cement (W/C) ratio
mortars and thus making mortars more durable.
In this study, further experiments were conducted to seek visual evidences of the inhibiting of chloride
ingress in the CWA mortars using a silver nitrate (AgNO3) solution spray method and an electron probe
microanalysis (EPMA) after 24 weeks submersion in 5.0 wt.% sodium chloride solution. The CWAs tested
at this time were electrical porcelain insulator wastes from an electric power company, which were
crushed and ground in a recycle plant. In particular, the test program was extended to investigate the
CWA mortars at a wider range of W/C ratios, i.e. 0.4, 0.5, and 0.6. All the CWA mortars were also compared with their counterpart mortars made of typical river sand (RS). It is visually found that, at the
W/C ratio of 0.4, 0.5, and 0.6, the CWA mortar is more effective in resisting chloride ingress (having lower
coefcient of apparent chloride diffusion) than the RS mortar. Moreover, the compression test was carried
out. It is worth noting that the CWA has no adverse effect on the compressive strength of mortars in relation to river sand.
2012 Elsevier Ltd. All rights reserved.

1. Introduction
The innite use of resources to meet consumer demand results
in the continual increase of industrial wastes, which is one of the
major environmental problems worldwide. To dispose industrial
wastes [1,2], a recycling process is preferably an attractive solution
because the availability of landlls is limited [3]. Many researchers

Corresponding author. Tel.: +81 66 721 2332; fax: +81 72 995 5192.
E-mail address: h-hirosi@civileng.kindai.ac.jp (H. Higashiyama).
0950-0618/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2012.11.078

in the world have investigated the recyclability and utilization of


ceramic wastes, such as blocks, bricks, roof tiles, sanitary ware or
electrical insulators, as aggregates and/or pozzolanic admixtures
in mortar and concrete [420].
The authors have also investigated on the recyclability and utilization of electrical porcelain insulator wastes as aggregates
(abbreviated to CWAs) in cement-based materials [21,22]. The porcelain insulator wastes shown in Fig. 1 (a suspension insulator) are
discarded not only from electric power companies but also from
ceramic industries. Porcelain insulator wastes are chemically stable, dense and hard. From a material sustainability point of view,
a recycling of the porcelain insulator wastes as aggregates in
cement-based materials has been noted a remarkable method.

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H. Higashiyama et al. / Construction and Building Materials 40 (2013) 10211028

Connect pin

Porcelain insulator
Metal socket
Fig. 1. Suspension insulator.

2. Experimental program
2.1. Ceramic waste aggregate
A recycled porcelain insulators as shown in Fig. 1 was rst received from an
electric power company in Japan. It was subsequently transformed to ne aggregate
namely ceramic waste aggregate (CWA) at a recycle plant (The Kanden L&A Company, Ltd.) via the processes developed primarily by Sano et al. [26] as follows.
Firstly, it was broken by using a hammer and a jaw crusher to small pieces ranging

Fig. 2. Ceramic waste ne aggregates.

100
80

Passing (%)

From the literature review, mechanical and permeation properties of the porcelain insulator wastes as aggregates in cementbased materials have been investigated by Hata et al. [5], Senthamarai et al. [7,16], Jacintho et al. [15], Takeda et al. [18], and Sekar
et al. [19]. When ne aggregates in concrete were partially replaced with CWA powder, Hata et al. [5] found that the compressive strength of concrete was increased. They stated that it was
because of the micro-ller effect. In the case of crushing porcelain
insulator wastes as coarse aggregate, Senthamarai et al. [7,16]
found no different on mechanical and permeation properties between conventional concrete and CWA concrete. Jacintho et al.
[15] investigated a performance related to the compressive
strength and absorption index of mortars made of crushed CWA
as ne aggregate. Takeda et al. [18] used CWA as coarse aggregate
in porous concrete. Sekar et al. [19] performed mechanical tests on
CWA concrete. The authors [21,22] also examined the mortars containing CWA recycled from porcelain insulator wastes on their
compressive strength and their resistance to chloride penetration.
We found that the replacement of entire ne aggregates with the
CWA in mortar increases the compressive strength and reduces
the chloride penetration depth and the cumulative pore volume
in mortar when compared with the river sand (RS) mortar. The
CWA in mortar not only increases the tortuous pathways in the
matrix but also reduces the transportation of chloride ion through
itself. The CWA in mortar thus has a dilution effect on the chloride
penetration.
In the present study, the inuence on chloride ingress into CWA
mortars with different water to cement (W/C) ratios was investigated by comparing with RS mortars. Unlike the previous studies
[21,22], the CWAs were crushed and ground at a recycle plant in
The Kanden L&A Company, Ltd. and were used as received. Their
performances in mortar on the chloride ingress were visually
investigated by using a silver nitrate (AgNO3) solution spray method [23] and an electron probe microanalysis (EPMA) [24,25]. Furthermore, the apparent chloride diffusion coefcients of mortars
made of the CWA and the RS, which were calculated from chloride
concentration proles obtained by EPMA, were compared. The
chloride concentration prole obtained by EPMA is useful for the
estimation of the apparent chloride diffusion coefcient [25].

60
40
20

CWA
RS

0
0.075 0.15

0.3

0.6

1.2

2.5

3 4 5 6
Sieve size (mm)

5.0

10.0

Fig. 3. Grain size distributions.

from 50 to 100 mm size. Next, by using a cone crusher, these pieces were crushed to
small grains at a particle size of 30 mm or smaller. These particles have very sharp
edges like a knife edge at this stage, which are still dangerous to supply as aggregate
for mortar and concrete. Therefore, the CWA with the safety shape of particle edge
was subsequently achieved by a grinding machine. Finally, the particle size ranging
from 0.075 to 5.0 mm by sieving (see Fig. 2) was used in this study. The grain size
distribution of the CWA after going through the above process and the RS used here
is presented in Fig. 3 along with the grading requirements (dashed lines) of JIS A
5005 [27]. The grain size distribution of the CWA is within the grading requirements only except for one particle size of 2.5 mm. As reported in Table 2, the neness modulus of the CWA and the RS is 3.20 and 2.39, respectively.

Table 1
Chemical composition.
Chemical compositions (wt.%)

Cement

CWA

SiO2
Al2O3
Fe2O3
CaO
MgO
SO3
Na2O
K2O
TiO2
P2O5
MnO
SrO
S
Cl

20.68
5.28
2.91
64.25
1.40
2.10
0.28
0.40
0.28
0.25
0.09
0.06

0.015

70.90
21.10
0.81
0.76
0.24

1.47
3.57
0.33






Loss on ignition

1.80

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H. Higashiyama et al. / Construction and Building Materials 40 (2013) 10211028


Table 2
Physical properties of ne aggregates.
Physical properties

CWA

River sand

Maximum size (mm)


Specic gravity
Water absorption (wt.%)
Fineness modulus

5.0
2.40
0.70
3.20

5.0
2.59
1.73
2.39

5 % NaCl solution

Fig. 7. Instrument used for EPMA.

Compressive strength (N/mm2)

Fig. 4. Immersion of mortar in a 5.0 wt.% NaCl solution.

80

60

40

20

CWA mortar
RS mortar

0
0.3

0.4

0.5

0.6

0.7

W/C ratio
25 mm

Fig. 5. Example of a fresh split surface showing white silver chloride precipitation
after sprayed a 0.1 N silver nitrate solution.

Fig. 8. Compressive strength and water to cement (W/C) ratio.

Chloride penetration depth (mm)

25 mm

25
CWA mortar

20

RS mortar

15
10
5
0
0.4

0.5

0.6

W/C ratio
Fig. 9. Chloride penetration depths for all mixtures measured.

2.2. Materials and mixture proportions

Fig. 6. Preparation of specimen for EPMA.

The CWA used as ne aggregate was compared with the RS in mortar mixes. The
chemical composition of the CWA and the cement is presented in Table 1. The
chemical composition of the CWA used is similar to that of sanitary ceramic wastes
[13,20]. The physical properties of both CWA and RS are shown in Table 2. In addition, the cement used here was an ordinary Portland cement (OPC) with the specic
gravity of 3.15 and the specic surface area of 3360 cm2/g. The cement used was
equivalent to ASTM Type I as shown in Table 1.

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H. Higashiyama et al. / Construction and Building Materials 40 (2013) 10211028

In this study, the W/C ratio of the mortars was varied with three different values, i.e. 0.4, 0.5, and 0.6 by weight. The sand to cement (S/C) ratio was kept constant
to 2.0 by weight. Hence, there were six mortar mixtures in total. Preliminarily, the
CWA was dried out in an oven for 24 h. After that, the CWA was kept in an uncontrolled laboratory (R.H.: 4050%) until mortar making. The CWA was mixed in an
air-dry condition due to its low water absorption while the RS was mixed in a saturated surface-dry condition.

2.3. Specimens and test methods


For all mixtures, the mortars were prepared in a Hobart mixer of 5 L capacity.
The mixing process started with the blending of the OPC and ne aggregate for
1 min and was followed with the addition of water and further mixing for 3 min.
Each of the mortar mixtures was cast in three 50 mm dia.  100 mm cylindrical
specimens for a compression test and, at the same time, two 100 mm

dia.  200 mm cylindrical specimens for the test of chloride ingress. After casting,
all specimens were covered with a plastic waterproof sheet for 24 h. Subsequently,
they were demoulded and cured in a water tank at 20 2 C.
At the age of 28 days, the 50 mm dia.  100 mm cylindrical specimens were
tested in compression using a 500 kN capacity universal testing machine. The loading speed was constant at 0.2 N/mm2/s according to JSCE-G 505 [28].
At the age of 7 days, the 100 mm dia.  200 mm cylindrical specimens were
prepared for the one dimensional ingress of chloride as follows. They were cut into
150 mm height with the 50 mm top end discarded to eliminate the inuence of segregation. After they were allowed to dry in a room condition at 20 2 C and R.H.
65 5% for 24 h, they were epoxy coated leaving only one sawn surface free of coating and were proceeded to dry the epoxy resin for additional 24 h. Then, they were
fully immersed in a 5.0 wt.% NaCl solution in hermetic tanks at 20 2 C as shown
in Fig. 4 for 24 weeks. After the immersion was completed, one of the two 100 mm
dia. (200 mm cylindrical specimens was examined with a silver nitrate spray method whereas another was followed with the EPMA method.

(a)

(d)

(b)

(e)

(c)

(f)

Fig. 10. Area analysis of the chloride concentration distribution by EPMA, (a) CWA mortar (W/C = 0.4); (b) CWA mortar (W/C = 0.5); (c) CWA mortar (W/C = 0.6); (d) RS
mortar (W/C = 0.4); (e) RS mortar (W/C = 0.5); and (f) RS mortar (W/C = 0.6).

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H. Higashiyama et al. / Construction and Building Materials 40 (2013) 10211028

3.2. Chloride penetration depth and concentration


One example of the freshly split surface showing the white silver chloride precipitation after sprayed with a 0.1 N silver nitrate
solution is presented in Fig. 5. In this gure, the bottom side of
specimen is the exposed surface. The chloride penetration depths
measured for all mixtures are shown in Fig. 9. The chloride penetration depth is an averaged of the depths measured at three points
shown in Fig. 5. From the results in Fig. 9, at all W/C ratios, the
chloride penetration depth of the CWA mortar is less than that of
the RS mortar. The more effectiveness of the CWA mortar is observed especially when the W/C ratio is lower.
By using the EPMA method, the 25  60 mm cross sectional
area of the EPMA specimens was analyzed. The EPMA analysis resulted in the distribution of chloride concentration as shown in
Fig. 10af. In these gures, the upper side of specimen is the exposed surface. It is clearly seen that the higher the W/C ratio is
the deeper the chloride ingress. This is due to the more open and
coarse pore structure at the higher W/C ratio [30]. From the colorimetric image of EPMA, the chloride concentration in the CWA
mortar along the depth shows lower than that in the RS mortar.
In the CWA mortars with W/C ratio of 0.5 and 0.6 presented in
Fig. 10b and c, a part of higher chloride concentration found in
the vicinity of 10 mm depth from the exposed surface. Unfortunately, this is due to the existence of hardened cement paste. The

3.3. Apparent chloride diffusion coefcient


In order to draw a chloride concentration prole from the EPMA
results, the chloride concentration was averaged along the same
penetration depth at 0.2 mm intervals in the direction of chloride
ingress. However, to avoid the effect of ne aggregates, the chloride concentration was employed only in the paste part. The chloride concentration proles of the CWA and RS mortars are shown
in Fig. 11a and b, respectively. These proles quantitatively verify
that, in the mortars, the chloride ingress is deeper when the W/C
ratio is higher. In the RS mortars, it is common to nd that the
higher W/C ratio mixes had higher chloride concentration at all

(a)

35
W/C = 0.4

Corresponding to the W/C ratios, the compressive strength results of both CWA and RS mortars are plotted in Fig. 8. It is observed that the compressive strength was linearly decreased with
the W/C ratio. Besides, at all W/C ratios, the compressive strengths
of CWA and RS mortars were fairly similar. That is contrast to our
previous ndings [21,22] in which, at a constant W/C ratio of 0.5, a
10% greater compressive strength was found in a CWA mortar corresponding to a RS mortar. In that case, the grain size distribution
of the CWA was adjusted manually to match that of the RS in the
laboratory. In this study, however, the modication of the grain
size distribution was omitted. But, the CWA as received from the
recycle plant was used instead. The CWA obtained was much coarser than the RS (neness modulus of 3.20 compared with 2.39).
Thus, the compressive strength is possibly dependent on the grain
size distribution of the CWA.
Jacintho et al. [15] presented that the compressive strength of
mortar with the above 50% substitution of CWA was increased in
proportion to the amount of the CWA. They explained that the pozzolanic reaction and the lower permeability due to the ne crushed
porcelain possibly cause the strength gain. In this study, at the age
of 28 days, the pozzolanic reaction of the CWA was not observed.
When compared with the compressive strength of the CWA mortar
at W/C ratio of 0.47 by Jacintho et al. [15], the compressive
strength of the CWA mortar shown in Fig. 8 is close to their result.

Chloride concentration (kg/m )

3.1. Compressive strength

30

W/C = 0.5

25

W/C = 0.6

20
15
10
5
0
0

Depth from exposed surface (cm)

(b)

35
W/C = 0.4

3. Results and discussion

hardened cement paste was generally used as an adhesive between


a porcelain insulator and a metal socket as shown in Fig. 1 when a
suspension insulator was assembled. In the crushing process making the CWAs mentioned above, porcelain insulators having the
metal socket are thrown into a jaw crusher. Consequently, the
hardened cement paste mingles with the CWAs. This hardened cement paste should be removed as an impurity.
Thus, when the chloride concentration proles for the CWA
mortars with the W/C ratio of 0.5 and 0.6 were made, rectangular
area surrounding the part of higher chloride concentration was
eliminated. In the comparison with the chloride concentration of
the RS mortars, it can be seen that the CWA in mortars have inuence on the chloride ingress as well as the results of the colorimetric tests. Since the CWA is chemically stable, dense and hard, it not
only increases the tortuosity of the matrix but also reduces the
chloride transportation through itself [21,22]. Further studies,
however, are needed for a better understanding of the mechanism
on the chloride resistance of the CWA mortar.

Chloride concentration (kg/m )

According to the silver nitrate spray method, the freshly split surface of mortars
was sprayed with a 0.1 N silver nitrate solution. To determine the chloride penetration depth, the white silver chloride precipitation appeared on the sprayed surface
was measured. By using a caliper, the measurement was made at three points along
the penetration front, i.e. one was at the middle and the other two points were on
the left and right at 25 mm apart from the middle, as shown in Fig. 5.
For the EPMA method, the test specimens were cut into 25 mm width and
60 mm length as shown in Fig. 6. The JEOL JXA-8200 instrument presented in
Fig. 7 was used to obtain chloride content and chloride concentration prole. Then,
the apparent chloride diffusion coefcient was calculated. The measurement conditions consisted in accelerating voltage of 15 kV, beam current of 2  107 A, a pixel
size of 200 lm, a probe diameter of 150 lm, and the number of mapping points of
400  400 pixels referring to JSCE-G 574 [29].

30

W/C = 0.5
W/C = 0.6

25
20
15
10
5
0
0

Depth from exposed surface (cm)


Fig. 11. Chloride concentration proles, (a) CWA mortars and (b) RS mortars.

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H. Higashiyama et al. / Construction and Building Materials 40 (2013) 10211028

points along the penetration depth. Yet, in the CWA mortars, such
correlation was reverse within the range of 9 mm depth from the
exposed surface. Regarding that, further studies are needed for a
better understanding.
The apparent chloride diffusion coefcient and the surface chloride concentration were determined by tting the chloride concentration results to the following Ficks second law.



x
Cx; t C 0 1  erf p
2 Da  t

where, C(x, t) is the chloride concentration (kg/m3) at depth x (cm)


and exposure time t (year), C0 is the surface chloride concentration
(kg/m3), Da is the apparent chloride diffusion coefcient (cm2/year),
and erf is the error function.
In the analysis of the chloride concentration prole, a value of Da
was found by the curve tting and C0 used the test result. The calcu-

(d)

35

Chloride concentration (kg/m3)

Chloride concentration (kg/m3)

(a)

lation result of the chloride concentration prole for all mortar


mixes is presented with a solid line as shown in Fig. 12af. The
apparent chloride diffusion coefcients are also given in Table 3.
The apparent chloride diffusion coefcient of both CWA and RS mortars is increased when the W/C ratio is increased. Since the pore
structure becomes ner in mortar with the lower W/C ratio, chloride
transportation is delayed. The same trend was also reported by
Gjrv and Vennesland [31] and Song et al. [32] due to cement hydration development. As reported further by Song et al. [32] and Park
et al. [33], the apparent chloride diffusion coefcient and the surface
chloride concentration are inuenced by the time dependence of
chloride transportation. Hence, in order to determine the time
dependence of those two variables for the CWA mortar, the chloride
ingress tests will be continued up to 96 weeks of exposure.
The apparent chloride diffusion coefcient of the CWA mortar is
lower than that of the RS mortar at all of the W/C ratios. At the W/C

Exp.

30

Fit.
25
20
15
10
5
0

35

Exp.

30

Fit.
25
20
15
10
5
0

Depth from exposed surface (cm)

(e)

35

Chloride concentration (kg/m3)

Chloride concentration (kg/m3)

(b)

Exp.

30

Fit.
25
20
15
10
5

35

Exp.

30

Fit.
25
20
15
10
5

(f)
Chloride concentration (kg/m3)

35

Exp.

30

Fit.
25
20
15
10
5
1

Depth from exposed surface (cm)

35

Exp.

30

Fit.
25
20
15
10
5
0

0
0

Depth from exposed surface (cm)

Depth from exposed surface (cm)


Chloride concentration (kg/m3)

0
0

(c)

Depth from exposed surface (cm)

Depth from exposed surface (cm)

Fig. 12. Curve tting of chloride concentration proles, (a) CWA mortar (W/C = 0.4); (b) CWA mortar (W/C = 0.5); (c) CWA mortar (W/C = 0.6); (d) RS mortar (W/C = 0.4); (e)
RS mortar (W/C = 0.5); and (f) RS mortar (W/C = 0.6).

H. Higashiyama et al. / Construction and Building Materials 40 (2013) 10211028

enced by the cement hydration having the time dependence,


the chloride ingress tests presented herein are continuing up
to 96 weeks of exposure.

Table 3
Apparent chloride diffusion coefcient for all mixtures.
W/C ratio

Apparent diffusion coefficient (cm2/year)

0.4
0.5
0.6

Apparent diffusion coefcient (cm2/year)


CWA mortar

RS mortar

0.610
1.001
1.776

2.064
2.367
2.669

Acknowledgments
The authors wish to acknowledge the nancial support of Graduate School of Science and Engineering, Kinki University and The
Kanden L&A Company, Ltd. Furthermore, the authors are also
grateful to Mr. K. Nakayama and Mr. T. Kitanobo of Chuken Consults Co., Ltd. for their valuable comments on the chloride ingress
analysis.

CWA mortar
RS mortar
JSCE

1027

Concrete

References

0
0.3

0.4

0.5
W/C ratio

0.6

0.7

Fig. 13. Apparent chloride diffusion coefcient and W/C ratio.

ratio of 0.5, the CWA mortar is superior to the RS mortar by 42%


reduction on the apparent chloride diffusion coefcient. This result
is a similar trend with the result of the rapid chloride migration
test in the previous study [22]. In addition, the relationship between the apparent chloride diffusion coefcient and the W/C ratio
is shown in Fig. 13 compared with the JSCE predicting curve for
concrete using OPC [34]. The apparent chloride diffusion coefcients of the RS mortars exhibit higher values while those of the
CWA mortars with W/C ratios of 0.5 and 0.6 exhibit less than the
JSCE predicting curve.
4. Conclusions
In this study, the inuence on chloride ingress into CWA mortars with different W/C ratios was investigated. Regarding the
materials used and the range of parameters studied herein, the following conclusions can be drawn.
(1) The compressive strength of the CWA mortars in which the
CWA was used as received from the recycle plant was relatively similar to that of the corresponding RS mortars.
(2) In the mortars, the decrease of the W/C ratio reduced the
chloride penetration depth. Further reduction was observed
in the CWA mortars compared with the RS mortars. These
were veried from the results of both the colorimetric test
and the EPMA test.
(3) The EPMA method was successfully employed to determine
the chloride concentration, the chloride prole, and the
apparent chloride diffusion coefcient in the CWA mortars.
It quantitatively indicated that the CWA mortars had lower
apparent chloride diffusion coefcient than the RS mortars.
In comparison to the apparent chloride diffusion coefcient
of the JSCE predicting curve, the CWA mortar is more efcient when the W/C ratio is higher.
(4) At this point, it is concluded that the CWA in mortar has a
potential for reducing the chloride ingress. However, as the
chloride transportation in cement-based materials is inu-

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