Construction and Building Materials 41 (2013) 239–245

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Construction and Building Materials

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Application of the colorimetric method to chloride diffusion evaluation

in concrete structures
Myung-Yu Kim a, Eun-Ik Yang a,⇑, Seong-Tae Yi b
a
Department of Civil Engineering, Gangneung-Wonju National University, 7, Jukheon-gil, Gangneung-si, Gangwon-do 210-702, South Korea
b
Department of Civil and Environmental Engineering, Inha Technical College, 100, Inha-road, Nam-gu, Incheon-si 402-752, South Korea

h i g h l i g h t s

" The colorimetric method can be an easy and practical alternative means to estimate the penetration depth of chloride ion.
" To use a silver nitrate concentration exceeding 0.05 N is recommended if the penetration depth of chloride ion is measured.
" The measurement of penetration depth by the colorimetric method is not practical if the pH of concrete is below 10.

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

Article history: The purpose of the present study are to properly estimate diffusion coefficient and determine the concen-
Received 12 June 2012 tration of sprayed silver nitrate (AgNO3) that corresponds with the critical chloride amount. We also pro-
Received in revised form 14 November 2012 pose a suitable guide for application of the colorimetric method through indoor and field tests.
Accepted 16 November 2012
According to the results, the colorimetric method using AgNO3 showed distinguished change to white
Available online 10 January 2013
reaction (AgCl) from brown reaction (AgOH). Any concentration (more than 0.05 N) of AgNO3 is useful in
evaluation of the diffusion coefficient and is available regardless of age. The model equation for the rela-
Keywords:
tionship between Da (the concentration profile according to distance from the surface) and Dc (the pen-
Colorimetric method
AgNO3
etration depth of the colorimetric method) is also proposed. When AgNO3 of 0.1 N is sprayed, free
Critical chloride content chloride amount (0.045%/1.08 kg/m3) of the color-change border is similar to the critical chloride content
Diffusion coefficient where corrosion is observed. Measurement of penetration depth by the colorimetric method is not appro-
priate when the pH of concrete is below 11.
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction
The chloride diffusion coefficient in concrete is important in
estimating limits on the life time of structures due to corrosion
as well as for expressing the penetration velocity of chloride.
Accordingly, numerous estimation methods have been introduced
to obtain the chloride diffusion coefficient of concrete [1–9]. The
representative method is estimation of the diffusion coefficient
using a general solution of Fick’s second law [2]. This method is
completed by measuring the chloride ion amount according to
the distance from the concrete surface. This method, however, en-
tails a complicated procedure and prolonged test time for measur-
ing chloride.
To mitigate these problems, acceleration tests (rapid chloride
penetration test (RCPT), chloride migration test (CMT)) have been
proposed and revised [3,4]. However, these acceleration
approaches cannot address real diffusion problems, because the
⇑ Corresponding author.
E-mail address: eiyang@gwnu.ac.kr (E.-I. Yang).
electrical field is artificially used and the applied high voltage leads
to an increase in temperature. Namely, this method cannot be
applied to real structures. Recently, a new method has been intro-
duced to determine the depth of chloride penetration wherein
0.1 N silver nitrate (AgNO3) aqueous solution is sprayed on a
cross-section of split concrete [5]. This test method is often called
the colorimetric method, because the spraying of 0.1 N AgNO3 solu-
tion on a cross-section of split concrete subjected to penetration of
chloride leads to the formation of white and brown regions with
well-distinguished boundaries [5,10]. The colorimetric method is
used extensively in many areas such as RCPT and CMT. Because test
process is simple and quick, this method has been used to widely
evaluate the penetration characteristics of chloride (Da).
However, the colorimetric method has been used without
sufficient investigation into the reaction mechanism and use scope
followed in condition of corresponding structures. Namely, W/C,
age, concentration of AgNO3, and the chloride amount of the col-
or-change border and so on also should be defined [10]. These fac-
tors can be regarded as restrictions to the application of the
colorimetric method under various environmental conditions.

0950-0618/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2012.11.084
240 M.-Y. Kim et al. / Construction and Building Materials 41 (2013) 239–245

The objectives of this research are to properly estimate the dif- Table 1
fusion coefficient and determine the concentration of sprayed Physical properties of aggregates.

AgNO3 that corresponds with the critical chloride amount. In this Item Specific gravity Absorption (%) FM
study, through indoor and field tests, a guideline is proposed for Type
application of the colorimetric method. Studies on the reaction Sand 2.59 1.01 2.65
principle and the factors affecting the colorimetric method, as well Gravel 2.78 0.62 6.80
as on the characteristics of the color-change border by carbonation
and concrete properties are conducted. In order to ensure the reli-
ability of the colorimetric method, the chloride diffusion coeffi-
Table 2
cient (Da) by the colorimetric method is compared with that (Dc) Mixture proportions of concrete.
by Fick’s law [2]. On the basis of an indoor experiment, a field test
was executed to estimate the field applicability of the colorimetric W/C (%) S/a (%) Unit weight (kg/m3)

method. W C S G
40 43 170 425 721 1022
2. Mechanism of colorimetric method 50 45 172.5 345 782 1021
60 46 175 292 816 1024

Penetration depth measurement of chloride ion using silver ni-

trate colorimetric method is firstly introduced by Otsuki et al. [11]
(Fig. 1). This method used the principle of which a white deposit is
formed through reaction between silver ion (Ag+) and chloride ion
(Cl). If colorimetric method is applied to concrete structures ex-
posed to chloride ion, additional precipitation reaction beside
white-precipitation reaction happens. That is, after creating of cal-
cium hydroxide [Ca(OH)2] resulting from the hydration of cement,
hydroxide ions at voids make brown-precipitation through reac-
tion with silver ions.
3. Experiment and measurement
3.1. Materials
In this test, chemical agents [NaCl (58.44 g), NaOH (45.00 g), and AgNO3
(168.97 g)] were used to examine the reaction principle and factors. These agents
were mixed in an aqueous solution state and distilled water was used as a solvent
to minimize the effects of other ions.
The cement used in the experiments was ordinary Portland cement (ASTM Type
I), and river sand was used as a fine aggregate. Crushed granite gravel passed
through a 25 mm sieve was used as a coarse aggregate. Physical properties of the
aggregates are given in Table 1.
3.2. Specimens and mixture design
the amount of chloride ion at the color-change border. Using silver nitrate solution
with varying concentrations, chloride ion penetration depths were measured for
concrete specimens immersed in seawater. The chloride diffusion coefficient was
determined with measured penetration depth. To confirm the results of indoor
experiments, field tests were performed to estimate the field applicability of the
colorimetric method for marine structures and pavement structures exposed in
deicing salts.
3.4. Test procedures
3.4.1. Influence factors
After melting a fixed amount of calcium chloride in sodium hydroxide solution
of pH 10–13, color-change of the blended solution was observed by adding silver
nitrate of fixed quantity into the solution. Fig. 2 presents a photograph taken during
the experiment showing the color-change reaction.
From these results, it was investigated whether the value of pH affected the
reaction. Generally, the reaction rate constant is defined as the time that some ions
take to react with other ions. This constant is measured through a quantitative
change of reaction outgrowth by time. However, in the case of a color-change reac-
tion, as a precipitation reaction, reaction velocity is faster than a general chemical
reaction. Because a comparison of fast reaction velocity is generally difficult, the rel-
ative reaction velocity among Cl, OH, and Ag ions was measured in this study. The
following equation was used in the calculation.
d½AgCl 
v1 ¼ ¼ k1 ½Agþ ½Cl  ð1Þ
dt

d½AgOH
In this test, the cylindrical concrete specimens of 100 mm diameter and v2 ¼ ¼ k2 ½Agþ ½OH  ð2Þ
100 mm height were used to examine the diffusion coefficient and concentration dt
of the color-change border with mixture proportions of the concrete. Mixture pro-
  K
portions of concrete are given in Table 2. After removal of the mold, specimens were ½Cl 0  ½AgCl ½OH 0  ½AgOH
 ¼  ) Y ¼ XK ð3Þ
stored for 7 days in saturated limewater at a temperature of 20 ± 3 °C. ½Cl 0 ½OH 0

Considering the maximum solubility of Cl, OH, and Ag, the mole ratio given in
3.3. Test variables
Table 4 was used to obtain the factors affecting color-change.

Test variables are given in Table 3. The objectives of this study are to review the
mechanism of the colorimetric method, investigate the influencing factors, and con-
firm the applicability in situ. For influencing factors, reaction velocity, Cl:OH ratio,
and carbonation in the color-change border were investigated. Also, it was neces-
sary to determine the most suitable sprayed concentration of silver nitrate and
3.4.2. Chloride penetration test and estimation of diffusion coefficient
Penetration of chloride was performed by an immersion test using NordTest
method of NT Build 443 [12]. Seawater was used in the immersion solution. The dif-
fusion coefficient was calculated each from the immersed specimen by measuring

Fig. 1. Diagram of colorimetric method.

 M.-Y. Kim et al. / Construction and Building Materials 41 (2013) 239–245 241

Table 3
Test variables.

Item Content Details

Reaction of colorimetric method (mechanism, effect factors) pH 10, 11, 12, 13
NaCl concentration(kg/m3) 0.1–1.0
Ag+: Cl: OH 1:1:0.05, 1, 10, 50, 100
Optimum AgNO3 concentration determination Test AgNO3 concentration 0.03 N, 0.04 N, 0.05 N, and 0.1 N
Concrete applicability estimation test Indoor test Cl concentration of colored zone
Field test Chloride diffusion coefficient Influence of carbonation

both the concentration profile according to distance from the surface (Dc) and the
penetration depth of the colorimetric method (Da). Equation to calculate the diffu-
sion coefficient is as follows:
 
Cðx; tÞ x
¼ 1  erf pffiffiffiffiffiffi ð4Þ
C0 4 Dt

!2
xd
Da ¼ pffiffiffiffiffi ð5Þ
yd 4t

 
1 Cd  Ci
yd ¼ erfc ð6Þ
C0  Ci

3.4.3. Measurement of chloride ion and carbonation

The samples cut at 5 mm thickness from the specimen to obtain the concentra-
tion profile with depth. After pulverized the sample, powder passed through a No.
40 sieve was only used. Chloride ion from concrete powder was extracted according
to ASTM C 114 [13] and measured using a selective ion electrode. Carbonation
depth in the field test was measured using a phenolphthalein solution of 1%
concentration.

3.4.4. Application to the field test

On the basis of the indoor experiment, field tests (Table 5) were performed to
estimate the field applicability of the colorimetric method for marine structures
and pavement structures.
Marine structures exposed to various conditions such as air, coast, and splash
zones were selected for the field tests. In the case of pavement structures, national
roads (37L, 43L, 45L, and 46L) of South Korea exposed to chloride attack due to deic-
ing salt were selected.

Fig. 2. Color-change reaction test. 4. Test results and discussion

4.1. Reaction of colorimetric method

Table 4
Mole ratio of ions used in reaction velocity test.
The colorimetric method is based on distinguishing two reac-
Mole ratio Ag+ Cl OH tions on the basis of color, i.e., brown and white. The white region
1:1:0.05 1 1 0.05 has been attributed to the precipitation of AgCl in a number of
1:1:1 1 1 1 studies [5,10,14,15]. However, the reaction principle for the brown
1:1:10 1 1 10
region, which is regarded as the ‘no chloride zone’, has not yet been
1:1:50 1 1 50
1:1:100 1 1 100 elucidated. In this study, the existence of a black region due to the
precipitation of AgOH was demonstrated. Eqs. (7) and (8) are the
reaction equations. Strictly speaking, precipitation of AgOH is clo-
ser to brown than black color. It is also known that the reactions of
Table 5
three ions influence the color-change process. This study examined
Details of field tests. the reaction velocity constant of these ions by comparing with the
relative velocity by fast precipitation reaction.
Structure name Service life Distance from Exposure
(year) coast (m) condition

Marine GOS 32 300 Air Agþ þ Cl ) AgClðsÞ ð7Þ
structures SOS 7 50 Coast
YD 18 3 Splash zone
WY 5 72 Air
Agþ þ OH ) AgOHðsÞ ð8Þ
SCN 7 12 Coast
HH 6 5 Splash zone Fig. 3 displays regression analysis results of a reaction velocity
KJ 40 450 Air constant as average values obtained through repetition of the same
Pavement 37L 18 – Deicing salt experiment 5 times. According to the results, the reaction velocity
structures 43L 14 constant, K is 3240. In other words, when silver nitrate (AgNO3)
45L 15
46L 15
solution was sprayed on a cross-section of split concrete, the reac-
tion of chloride ions is 3240 times faster than that of hydrated ions.
242 M.-Y. Kim et al. / Construction and Building Materials 41 (2013) 239–245

0.10
Concentration of AgNO 3 Color-change of concrete

0.08
Reaction velocity of AgCl

0.03N
0.06

0.04

0.02 0.04N

0.00

0.988 0.990 0.992 0.994 0.996 0.998 1.000

0.05N
Reaction velocity of AgOH

Fig. 3. Reaction velocity constant.

4.2. Application of colorimetric method through indoor tests

0.1N
4.2.1. Optimal concentration decision of sprayed AgNO3
A preliminary test was executed for determining a suitable
AgNO3 concentration that can indicate the critical chloride content,
when chloride permeation depth was measured by the colorimet- Fig. 4. Color-change of concrete with concentration of AgNO3.
ric method. Table 6 shows the color-change results with the con-
method, the effect of concrete age was not addressed. In this test,
centration of AgNO3 in an aqueous solution of pH 12. Color-
estimation of diffusion coefficient was performed in accordance
change in the aqueous solution was more clearly observed in
with concentration of AgNO3 and concrete age. Fig. 5 shows the dif-
0.03 N AgNO3 or more.
fusion coefficient (Da) with concentration of AgNO3 and W/C. Even
On the basis of the results, four AgNO3 samples were applied to
when the concentration of sprayed silver nitrate (AgNO3) is chan-
concrete specimens that were exposed to chloride attack for
ged, the diffusion coefficient (Da) that corresponds with the 0.05 N
3 months. Fig. 4 shows the color-change of concrete with the con-
AgNO3 is almost similar that of 0.1 N AgNO3 regardless of W/C. This
centration of AgNO3.
is because the permeation depth and chlorine ion concentration of
According to the results, as the concentration of AgNO3 in-
the color-change border vary in accordance with the employed
creases, an apparent change of color could be observed. Since the
concentration of AgNO3.
color-change is not clearly observed in low-concentration, includ-
Fig. 6 shows the diffusion coefficient (Da) with age. The results
ing 0.03 and 0.04 N, the possibility of errors is higher at these con-
show that the diffusion coefficient evaluated in concrete speci-
centrations (0.03 and 0.04 N). Therefore, when the penetration
mens of the same W/C does not change with age. Therefore, suit-
depth of chloride ions is measured, it is recommended that silver
able concentrations (above 0.05 N) of silver nitrate (AgNO3) are
nitrate concentration of more than 0.05 N should be used.
useful in evaluating the diffusion coefficient and are available
regardless of age.
4.2.2. Diffusion coefficient by the colorimetric method
In the case of measuring chloride penetration depth, the color-
imetric method is widely used, typically at a silver nitrate solution 4.2.3. Relationship between diffusion coefficients
concentration of 0.1 N. However, evaluation of a chloride diffusion Fig. 7 shows diffusion coefficients (Da, Dc) of specimens
coefficient that can be used to apply silver nitrate solutions of immersed for 6 months. According to the results, the diffusion
other concentrations has not been reported. Also, when the
chloride diffusion coefficient was evaluated by the colorimetric 10
0.05N AgNO3
Diffusion coefficient (10 m /s)

8 0.1N AgNO3
2

Table 6
-12

Color-change with concentration of AgNO3 and chloride.

6

0
0.35 0.40 0.45 0.50 0.55 0.60 0.65
W/C

Fig. 5. Diffusion coefficient (Da) with concentration of AgNO3 and W/C.

 M.-Y. Kim et al. / Construction and Building Materials 41 (2013) 239–245 243

10 0.10
W/C=0.4 free chloride
Diffusion coefficient (10 m /s)

W/C=0.5

Chloride concentration (%)

total chloride
2

8 W/C=0.6 0.08
-12

6 0.06

4 0.04

2 0.02

0
0.00
8 12 16 20 24 28 32 36
0.03N 0.04N 0.05N 0.1N
Immersion age (weeks) AgNO3 concentration
Fig. 6. Diffusion coefficient (Da) with age.
Fig. 8. Chloride concentration with AgNO3 concentration at the color-change
coefficient (Da) evaluated for spraying AgNO3 of 0.1 N is less than border.

that (Dc) determined by the concentration profile. For analysis of

these results, a model equation of the relationship between Da
and Dc is proposed as follows: 0.10

Da
Dc ¼ ð9Þ
1:4  ðW=CÞ1:5
Chloride concentration (%)
0.08

4.3. Concentration of chloride in color-change border 0.06

In this study, concentration of the color-change border is exam-

0.04
ined with W/C and concentration of sprayed AgNO3. Figs. 8 and 9
show the chloride concentration with sprayed AgNO3 and with
W/C at the color-change border, respectively. 0.02 free chloride
Andrade et al. [14] found that the value of total chloride concen- total chloride
tration at which the change of color took place for concrete made
with different types of binder was 1.13 ± 1.4% by cement weight 0.00
or 0.18 ± 0.2% by concrete sample weight. Also, an earlier work car- 0.35 0.40 0.45 0.50 0.55 0.60 0.65
ried out at CSIRO by Sirivivatnanon and Khatri [15] on a limited W/C
number of concrete samples immersed in 3% NaCl solution and
then sprayed with 0.1 N AgNO3 revealed that the concentration Fig. 9. Chloride concentration with W/C at the color-change border.
of water-soluble chloride at the boundary varied from 0.84% to
chloride content at which corrosion is observed, when AgNO3 of
1.69% by weight of the binder.
0.1 N is sprayed. The average amount of free chloride measured at
According to the results of the present study, the total chloride
the color-change border was about 90 ppm. This value can be con-
amount at the color-change border is approximately twice that of
verted to 0.045% (1.08 kg/m3) chloride by concrete sample weight.
the free chloride amount [16]. The W/C does not influence the con-
Total chloride measured at the color-change border was 0.082%.
centration at the color-change border. Remarkably, the free chlo-
Therefore, in the case of using AgNO3 of 0.1 N, the depth of critical
ride amount at the color-change border is similar to the critical
chloride could be easily evaluated using the colorimetric method.
6
colorimetric method (Da) 4.4. Influence of carbonation on colorimetric method
Diffusion coefficient (10 m /s)

5 concentration method (Dc)

2

Fig. 10 shows the color-change with pH. According to Fig. 10,

-12

when the pH of concrete is below 10, measurement of the penetra-

4
tion depth by the colorimetric method is not practical. Thus, when
a concrete structure is exposed to chloride attack and carbonation
3 conditions, carbonation depth must be examined before measuring
the penetration depth of chloride. That is, when AgNO3 was sprayed,
2 if the depth of carbonation is deeper than the chloride penetration,
application of the colorimetric method is impossible since the car-
1 bonation depth seems same with penetration depth of chloride.

0 4.5. Field test of colorimetric method

0.3 0.4 0.5 0.6 0.7
W/C On the basis of the indoor test results, RC structures exposed to
chloride conditions were selected to confirm the applicability of
Fig. 7. Relationship between diffusion coefficients (Da, Dc). the colorimetric method.
244 M.-Y. Kim et al. / Construction and Building Materials 41 (2013) 239–245

Table 7
Field test results in marine structures.

Structure Chloride Carbonation Da Concentration at

name penetration depth (mm) (1012 m2/ the color-change
depth (mm) s) border (kg/m3)
HH 72.3 1.3 2.24 1.04
WY 19.3 20.0 0.27 0.85a
SCN 59.7 1.3 0.67 0.92
GOS 7.7 20.0 0.01 0.69a
SOS 59.0 20.3 1.43 1.08
KJ 49.3 45.0 0.30 0.74a
YD 76.7 6.3 0.84 1.15
a
(a) pH-10 It is not reliable because the carbonation depth is same or deeper than the
chloride penetration depth.

Table 8
Field test results in pavement structures.

Road Chloride Carbonation Chloride Da Concentration

name penetration depth (mm) amount (1012 m2/ at the color-
depth (mm) of surface s) change border
(kg/m3) (kg/m3)
37L 22 3 4.26 2.24 1.26
43L 25 2 2.15 2.27 1.39
45L 23 2 3.28 1.87 1.30
46L 33 1 3.13 3.13 1.12

(b) pH-11 However, the chloride depth and carbonation depth were almost
identical in the case of WY and KJ. The carbonation depth was dee-
per than the chloride depth in GOS. In these cases (WY, KJ, and
GOS), it is not reliable to estimate the depth of the color-change
border. This means that, when carbonation depth is deeper than
that of chloride depth, we cannot recognize the true chloride depth
and, accordingly, it is impossible to apply the colorimetric method
related to the depth.
Therefore, when RC structures receive salt damage and carbon-
ation at the same time, measurement of carbonation depth is very
important before application of the colorimetric method. Accord-
ing to the concentration at the color-change border, the chloride
concentration (1.05 kg/m3) examined in the field was almost sim-
ilar to the free chloride concentration (1.08 kg/m3) determined via
a laboratory test.
(c) pH-12
4.5.2. Pavement structures exposed to deicing salt
Deicing salt is widely used to reduce traffic accidents due to
snowfall or icy conditions in winter. The use of deicing salt, how-
ever, can cause corrosion of bridge structures. This research exam-
ined salt damage using the colorimetric method. Four national
roads situated in the northern region of South Korea were selected
for the study (Table 8).
According to the results, while carbonation depth was mea-
sured to be less, chloride penetration due to the use of deicing salts
was measured as roughly 26 mm on the national roads. As carbon-
ation depth was less than the chloride penetration depth, estima-
tion of the penetration depth and diffusion coefficient is easily
accomplished using the colorimetric method. Concentration at
the color-change border was an average of 1.27 kg/m3 and was
(d) pH-13
similar to the results from lab experiments and marine structure
Fig. 10. Color-change with concentration of AgNO3 and chloride. evaluations.

4.5.1. Marine structures exposed to coastal environment
In the case of marine structures, the service life was 5–40 years,
and they are located at splash (2), coast (2), and air zones (3). Field
test results are shown in Table 7. According to the results, the
chloride in the splash zone penetrated deeper into the concrete.
5. Conclusions
The goals of this study are to properly estimate diffusion coeffi-
cient and determine the concentration of sprayed silver nitrate
(AgNO3) that corresponds with the critical chloride amount. We
also proposed a suitable guide for application of the colorimetric
 M.-Y. Kim et al. / Construction and Building Materials 41 (2013) 239–245
method through indoor and field tests. The following conclusions
have thereupon been obtained:
(1) The colorimetric method using AgNO3 is mainly comprised
of two reactions, which are distinguished as white (AgCl)
and brown reactions. (AgOH). When AgNO3 solution was
sprayed on a cross-section of split concrete, the reaction of
chloride ions is 3240 times faster than that of hydration ions.
(2) When the penetration depth of chloride ion is measured, it is
recommended that a silver nitrate concentration exceeding
0.05 N be used. Some concentration (above 0.05 N) of AgNO3
is useful in the evaluation of the diffusion coefficient and is
available regardless of age.
(3) The diffusion coefficient (Da) evaluated for spraying AgNO3
of 0.1 N is less than that (Dc) determined by the concentra-
tion profile. For analysis of these results, a model equation
of the relationship between Da and Dc was proposed.
(4) The W/C does not influence the concentration at the color-
change border. Remarkably, the free chloride amount
(0.045%/1.08 kg/m3) at the color-change border was similar
to the chloride threshold value at which corrosion is
observed, when AgNO3 of 0.1 N was sprayed.
(5) When the pH of concrete is below 10, the measurement of
penetration depth by the colorimetric method is not practical.
Thus, when a concrete structure is exposed to chloride attack
and carbonation conditions, carbonation depth must be
examined before measuring the chloride penetration depth.
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