Journal of Advanced Concrete Technology Vol. 9, No.

2, 127-132, June 2011 / Copyright © 2011 Japan Concrete Institute 127

Scientific paper

Effect of the Methylene Blue Value of Manufactured Sand on

Performances of Concrete
Li Beixing1, Zhou Mingkai2 and Wang Jiliang3

Received 21 August 2010, accepted 2 March 2011

Abstract
The methylene blue value (MBV) is an important index that reflects the quality of manufactured sand (MS). The relation
between MBV of MS and its limestone fines content, clay content and clay characteristics was investigated and the effects
of MBV ranging from 0.35 to 2.5 on the performance of MS concrete were tested. Results showed that MBV of MS is
affected not by the limestone fines content, but by the clay content and the liquid limit index of clay. With an increase in
MBV, the workability, flexural strength and 7d compressive strength of the MS concrete decreased, while the 28d com-
pressive strength was not affected. Moreover, the increase of MBV promoted plastic shrinkage and drying shrinkage
cracking of the concrete, and remarkably accelerated freeze-thaw damage and abrasion loss. It was concluded that the
critical MBV was 1.4, a value below which MS concrete performances are not significantly diminished.

1. Introduction contain clay minerals (AASHTO TP57 2000; BS EN 933

The use of manufactured sand (MS) in concrete has
significantly increased especially in areas where natural
sand is scarce. MS is the product of rock crushing and
sieving. The crushing process tends to produce a certain
amount of stone fines, which may be intermingled with
clay minerals due to the failure to clear off mountain soil
in mining or the inclusion of soil in the rock strata. Ow-
ing to its fine grain size, large porosity and surface ac-
tivity, clay can increase the water requirement in concrete
to achieve the same workability, and thus decrease the
strength, durability and volume stability of concrete
(Yool et al. 1998; Norvell et al. 2007). However, research
has shown that stone fines with 10% in MS, which has
the same grain size as clay (less than 75 μm), has no
harmful effect on the performance of most concrete
mixtures (Koehler and Fowler 2008; Celik and Marar
1996; Li Beixing et al. 2006; Quiroga et al. 2006; Wang
Jiliang et al. 2008). Thus, it is necessary to determine
whether the fine particles with a size smaller than 75 μm
in MS are stone fines or clay fines. This may be carried
out using the methylene blue (MB) absorption method,
which has been incorporated in United States and Euro-
pean standards to determine whether aggregate fines
1 and 28 days, respectively. First grade, class F fly ash was
Professor, Key Laboratory for Silicate Materials
Science and Engineering of Ministry of Education,
Wuhan University of Technology, Wuhan , China.
E-mail: libx0212@126.com
2
Research Associate, Key Laboratory for Silicate
Materials Science and Engineering of Ministry of
Education, Wuhan University of Technology, Wuhan,
China.
3
Engineer, Key Laboratory for Silicate Materials Science
and Engineering of Ministry of Education, Wuhan
University of Technology, Wuhan, China.
2000; ASTM C03 2003). However, the critical MBV has
not been identified in foreign standards. The current
Chinese National Standard (GB/T 14684-2001) intro-
duces the MB method, and specifies that the limit of
stone fines content in MS is 3%, 5% and 7% when MBV
< 1.4, and 1%, 3% and 5% when MBV ≥ 1.4, respec-
tively, based on the used concrete strength grade such as
higher than 60 MPa, between 60 and 30 MPa and lower
than 30 MPa. However, the critical MB value is not
explained in GB/T 14684-2001. Although some re-
searchers have observed correlations between MBV and
workability and drying shrinkage of MS concrete
(Stewart et al. 2007; Hosking and Pike 1985), the rela-
tionship between MBV and concrete performance still
requires further study to predict concrete properties
based on MBV. In order to provide some suggestions for
controlling MBV of MS, this paper investigated the
effect of MBV of MS, which was adjusted by the addi-
tion of clays, on the workability, mechanical properties,
shrinkage, cracking and durability of concrete.
2. Experimental procedure
2.1 Materials
A 42.5 grade ordinary Portland cement was used, with
27.4 MPa and 52.6 MPa compressive strength at 3 days
used as a supplementary cementitious material. The
coarse aggregate was crushed limestone with 5 to 25 mm
continuous gradation. The fine aggregate was limestone
MS with a fineness modulus of 3.1, with original stone
fines content of 4.3%. The limestone fines smaller than
the 75 μm were obtained by grinding the limestone MS,
with Blaine specific surface area of 346.4 m2/kg. Three
clays, A, B and C, were employed, and clay fines were
manufactured by drying at 105°C for 24h and grinding to
passing a 75 μm mesh before use. Their physical and
128 B. Li, M. Zhou and J. Wang / Journal of Advanced Concrete Technology Vol. 9, No. 2, 127-132, 2011

Table 1 Physical and chemical properties of clay samples.

Blaine specific sur- Liquid limit Plastic limit Plastic index
No. Mineral compositions
face area (m2/kg) index WL (%) index WP (%) IP (%)
Kaolinite 13%, quartz 25%, feldspar 30%,
A 598.2 28 18 10
hornblende 12%, mica and vermiculite 20%
Kaolinite 40%, quartz 41%, feldspar 11%,
B 634.5 42 23 19
illite and montmorillonite 6%, mica 2%
Kaolinite 65%, quartz 19%, mica and ver-
C 658.7 55 34 21
miculite 10%, feldspar 3%, illite 3%

chemical properties are listed in Table 1. A polycarbox-
ylic-acid type superplasticizer commercially branded as
JK-180 was used in concrete mixtures. The solid content,
pH, and specific gravity of the superplasticizer were 35%,
6.7, and 1.05 g/cm3, respectively.
2.2 Concrete mixture
The reference mixture proportion of concrete used in this
study consisted of 430 kg/m3 cement, 70 kg/m3 fly ash,
760 kg/m3 MS with a fixed amount of particles finer than
75 μm of 7% (namely the sum of limestone fines and
clay fines), 1110 kg/m3 crushed stone, and 2.25 kg/m3
superplasticizer. MBV was adjusted by changing the
ratio of the mass of clay to limestone fines in MS.
2.3 Experimental methods
MBV of MS with limestone or clay fine particles (< 75
μm) replacements was determined by the methylene blue
value test for fine aggregate according to Chinese Stan-
dard for Test Method of Aggregate for Highway Engi-
neering (JTG E 42-2005). Clay materials replaced 1% to
6% of MS by weight, and limestone fines replaced 5% to
20% of the sand by weight. This test is a measure of the
capacity of fine aggregate to adsorb methylene blue dye
and can be used to indicate the presence or absence of
clay in a fine aggregate sample.
To test the effects of MBV on concrete or mortar
properties, the MBV was adjusted from 0.35 to 2.5, by
changing the weight ratio of clay B to limestone fines
when the sum of limestone and clay fines content in MS
is fixed to 7% by weight.
Fresh concrete properties were tested according to the
Chinese Standard for Test Method of Performance on
Ordinary Fresh Concrete (GB/T50080-2002). Compres-
sive strength, flexural strength and elastic modulus were
determined by testing 150 mm × 150 mm × 150 mm
cubes, 100 mm × 100 mm × 400 mm prisms and 150 mm
× 150 mm × 300 mm prisms, respectively, according to
the Chinese Standard for Test Method of Mechanical
Properties on Ordinary Fresh Concrete (GB/
T50081-2002).
Plastic shrinkage crack tests were conducted accord-
ing to Chinese Standard for Guide of Design and Con-
struction to Durability of Concrete Structure (CCES
01-2004). In order to initiate cracks in the concrete, a
steel mold of 600 mm × 600 mm × 63 mm with 14 bolts,
10mm in diameter, mounted regularly at each at each of
the four sides of the rigid frame, was used to restrict
possible drying shrinkage of concrete. Concrete was
placed in the steel form and cured with a cover of acrylic
board for 2 hours under a constant temperature of 30°C
and relative humidity of 60%. Subsequently, it was ex-
posed to an air flow with a velocity of 8 m/s under a
constant temperature of 30°C and relative humidity of
60%. Then, the age of crack initiation, number of cracks,
crack length and crack width were measured up to the
age of 24 hours. Parameters representing crack propaga-
tion characteristics at the age of 24 hours may be the
average crack area, number of cracks per unit area and
total crack area per unit area. The test apparatus used and
the details of crack parameter calculation and evaluation
methods are shown in the Chinese standard (CCES
01-2004).
Drying shrinkage was tested according to Chinese
Standard for Test Methods of Cement and Concrete for
Highway Engineering (JTG E30-2005). The dimensions
of concrete specimens are 100 mm × 100 mm × 515 mm.
After 1 day of wet curing, the demolded specimens were
stored at constant temperature (20±2°C) and constant
relative humidity (60±5%). A micrometer was applied to
monitor the drying shrinkage of specimens at 1, 3, 7, 14,
28, 60, 90, and 180 d.
Abrasion loss of mortar specimens (150 mm × 150
mm × 50 mm) was tested in accordance with JTG
E30-2005, with the ratio of cement, MS and water as 1:
2.5: 0.44. Chloride ion permeability was measured using
100 mm × 100 mm × 50 mm concrete specimens by the
NEL method based on the Nernst-Einstein equation ac-
cording to CCES 01-2004. The freeze-thaw resistance of
concrete prisms (100 mm × 100 mm × 400 mm) was
conducted in accordance with JTG E30-2005.
3. Results and discussion
3.1 Relation between MBV and limestone fines
content and clays content in MS
Figure 1 illustrates effect of limestone fines content on
MBV. For every 5% increase of limestone fines content
in MS, MBV increased no more than 0.05 g/kg. The
effect of the three kinds of clays, A, B and C, on MBV
was shown in Fig. 2. With an increase in clay content in
MS, MBV of the MS increased rapidly in a linear manner.
Clay C and Clay B replacement results in much higher
MBVs than Clay A, and the MBVs are significantly
 B. Li, M. Zhou and J. Wang / Journal of Advanced Concrete Technology Vol. 9, No. 2, 127-132, 2011 129

1.4 5
1.2
4 Clay C y = 0.6964x + 0.3464
1 R2 = 0.9998
Clay B

MBV (g/kg)
MBV (g/kg)

0.8 3 y = 0.3589x + 0.3589

Clay A
R2 = 0.9996
0.6 2
y = 0.1089x + 0.3375
0.4 R2 = 0.996
y = 0.012x + 0.269 1
0.2 R2 = 0.9736
0
0
0 1 2 3 4 5 6
0 5 10 15 20
Clay content (％)
Limestone fines content ( ％)
Fig. 2 Effect of clay content in MS on MBV of MS.
Fig. 1 Effect of limestone fines content in MS on MBV of
MS.

5
clay 1% clay 2% clay 3% 10

4 clay 4% clay 5% clay 6% Clay content requirment (%)

when MBV=1.4g/kg 8
MBV (g/kg)

3
6

2
4

1 y = 101251x -2.7824
2
R2 = 0.9968
0 0
25 35 45 55 25 35 45 55
W L (%) W L (%)

Fig. 3 Effect of liquid limit index (W L) of clay on MBV of Fig. 4 Clay content required with liquid limit index (W L)
MS. when MBV is up to 1.4 g/kg.

larger than that of the MS with limestone fines. This
indicates much higher absorption of methylene blue by
clays than by limestone fines. From Fig. 3 and Fig. 4, it
can be found by further analysis that when the clay
content in MS is fixed, the MBV of MS is proportional to
the liquid limit index (WL) of clay, and when the clay in
MS has a high WL, a small amount of clay can cause
MBV of over 1.4.
It can be perceived that MBV of MS is affected not by
limestone fines content but by the content and character
of clay fines. Increasing WL of clay and the percentage of
clay in the MS increases the MBV, as expected. MS
containing distinctive clays differs in MBV, which is due
to the differences of the mineral characteristics, surface
area and number of cation exchange sites among clays,
which also influence concrete performances. Thus, the
MBV can more exactly reflect the effect of clays on
concrete performances than clay content.
3.2 Effect of MBV of MS on the workability and
mechanical properties of concrete
Table 2 shows the effect of MBV of MS on the worka-
bility and mechanical properties of concrete. For the
concrete mixtures with a constant water-binder ratio,
with the increase of MBV, the slump and slump flow of
fresh concrete marked a slight reduction when the MBV
was less than 1.1, but the workability decreased dra-
matically when the MBV surpassed 1.45, as expected.
The mechanisms for clay decreasing workability of
concrete are: (1) clay particles are very small, resulting in
high specific surface areas and potentially increasing
water demand, clay minerals absorb additional water into
a layered structure, increasing water demand further. (2)
the cations in the clay can be exchanged with the organic
compounds comprising the superplasticizer (Sakai et al.
2006). This results in adsorption of the water-reducing
admixture into the clay structure, leaving less available
for the cement paste. Thus it is clear that the workability
of concrete with clay will decrease when the amount of
water and dosage of superplasticizer are both held con-
stant.
With an increase in MBV of MS, the 7d compressive
strength and 28d flexural strength were lower, but 28d
compressive strength was not affected, as shown in Ta-
130 B. Li, M. Zhou and J. Wang / Journal of Advanced Concrete Technology Vol. 9, No. 2, 127-132, 2011

Table 2 Effect of MBV of MS on workability and mechanical properties of concrete.

MBV Slump Slump flow Compressive strength (MPa) 28 d flexural 28 d elasticity

No.
(g/kg) (mm) (mm) 7d 28d strength (MPa) modulus (GPa)
1 0.35 220 550 63.3 73.2 9.12 47.6
2 0.70 220 550 64.1 74.3 9.18 47.8
3 1.10 200 520 63.2 75.6 8.91 48.1
4 1.45 190 430 60.5 72.1 8.80 47.2
5 1.80 140 — 59.3 73.9 8.63 47.9
6 2.15 80 — 58.6 74.5 8.02 46.1
7 2.50 10 — 54.3 72.8 7.78 45.3

80 crack initiation gradually shortened with the increase of

MBV, and especially with MBV > 1.45, it shortened
suddenly. Cracking of concrete was not seriously af-
Compressive strength (MPa)

70
60
7d
50
28d
40
30
0 0.5
Fig.5 Effect of MBV of MS on compressive strength of
concrete.
ble 2 and Fig. 5. When the MBV increased to 2.5, the 7d
compressive strength and 28d flexural strength of con-
crete were respectively reduced by 14% and 15%, com-
pared with those when MBV was 0.35. For MBV ≤ 1.8,
the elastic modulus of concrete was hardly changed,
while it began to decrease when MBV exceeded 1.8.
In general, the presence of clays in aggregates is con-
sidered harmful to concrete. The extremely fine particu-
late nature of clay minerals and their surface activity
generally increase the mix-water required to provide a
concrete of given workability, as well as restrain the
hydration of cement, and hinder the interfacial bonding
between cement and aggregate (Zhao Shangchuan et al.
2007). This has implications for the strength of the
hardened concrete. However, the 28 d compressive
strength results shown in Fig. 5 were widely divergent
with the usual views. The main reason may be that clay B
used in these tests mainly consists of kaolinite and quartz
and contains a small amount of montmorillonite. Seleem
and El-Hefnawy (2003) also observed that when w/c is
held constant, kaolinite and illite had no effect on com-
pressive strength, and only montmorillonite clay
significantly decreased compressive strength.
3.3 Effect of MBV of MS on the plastic shrinkage
crack and dry shrinkage of concrete
It can be seen from the results in Table 3 that the age of
fected by the MBV with less than 1.10, when MBV was ≥
1.45, the crack width, the average crack area and the total
crack area per square meter increased rapidly. Compared
with concrete with MBV of 0.35, increases of 88% and
133% were obtained in the total cracking area per square
meter for concretes with MBV of 1.8 and 2.5, respec-
tively.
Plastic shrinkage cracks occur when the surface
moisture loss of concrete exceeds the transport of inter-
1 1.5 2 2.5 3 nal moisture to the surface, leading to negative capillary
MBV (g/kg) pressures and plastic shrinkage in paste. Owing to the
high moisture absorption of porous clays, the moisture
retention of fresh concrete containing clays is improved
and the transport of internal moisture to the surface is
reduced, causing an increase in the plastic shrinkage of
concrete surface and the occurrence of plastic cracks.
The effect of MBV of MS on the drying shrinkage of
concrete is shown in Fig. 6. With increasing MBV, es-
pecially when MBV exceeds 1.45, the drying shrinkage
of concrete increased. This result has been observed
previously (Seleem and El-Hefnawy 2003). There are
two primary reasons for the increasing degree of drying
shrinkage. One reason is that the clay particles them-
selves have a loose and porous layer structure. When
they are scattered in concrete, the clay particles can ad-
sorb mixing water and then swell. Once the concrete is in
a dry environment, the loss of surface moisture of con-
crete causes the adsorbed water in the layers of the clay
particles to be released by diffusion and migrate to the
concrete surface, resulting in a decrease of the internal
humidity of concrete. The other reason is that clays with
high specific surface area in MS also increase the volume
of paste.
3.4 Effect of MBV of MS on durability of con-
crete
Abrasion resistance is one of the important performances
of pavement concrete. Figure 7 shows the effect of MBV
on the abrasion resistance of cement mortar. Abrasion
mass loss of mortar increased with the increase of MBV.
Especially when MBV was larger than 0.7, the abrasion
resistance of mortar decreased noticeably. This is be-
cause that clay is weaker, and the incorporation of clay
 B. Li, M. Zhou and J. Wang / Journal of Advanced Concrete Technology Vol. 9, No. 2, 127-132, 2011 131

Table 3 Effect of MBV of MS on plastic shrinkage crack propagation of fresh concrete at the age of 24 hours.

Age of crack Number Average Number of Total crack area Crack

MBV Crack fea-
No. initiation of cracks crack area cracks per unit per unit area evaluation
(g/kg) ture
(min) (N) (mm2/N) area (N/m2) (mm2/m2) grade
1 0.35 410 63 very fine 3.82 175 668.3 medium
2 0.70 405 59 very fine 3.89 164 637.5 medium
3 1.10 385 61 very fine 3.85 169 653.1 medium
4 1.45 340 65 fine 4.80 181 866.4 inferior
5 1.80 265 66 fine 6.86 183 1257.2 inferior
6 2.15 245 62 wide 8.05 172 1387.2 inferior
7 2.50 210 61 wide 9.18 169 1554.7 inferior

550 4.5

Abrasion mass loss per unit area

180d
4
Drying shrinkage (×10-4 )

450 90d
60d 3.5
350

(kg/m2 )
28d 3
14d
250 2.5
7d

150 3d 2
1d
1.5
50 0 0.35 0.7 1.05 1.4 1.75 2.1 2.45 2.8
0.35 0.7 1.05 1.4 1.75 2.1 2.45 2.8
MBV (g/kg)
MBV (g/kg)
Fig. 7 Effect of MBV of MS on abrasion resistance of ce-
Fig. 6 Effect of MBV of MS on dry shrinkage of concrete. ment mortar cured for 28 days.

increases the volume of paste as well as hinders the
bonding between the cement matrix and aggregates.
Table 4 shows the effect of MBV on the chloride ion
permeability and freeze-thaw resistance of concretes.
Only a slight increase in the chloride ion diffusion coef-
ficient (DNEL) was seen with the increase of MBV, which
indicates that the increase of MBV had no obvious
harmful influence on the impermeability of MS concrete.
Table 4 indicates that the influence of MBV on
freeze-thaw resistance is significant. The relative dy-
namic elastic modulus (RDM) for the two concrete
mixtures with MBV of 0.35 and 0.7 hardly decreased
when lasting 250 cycles in freeze-thaw testing. It is pre-
dicted that the freeze-thaw durability grade of the two
mixtures will exceeded F250. The RDM for the concrete
mixtures with MBV ≥ 1.45 was slightly reduced up to
150 cycles, but it dropped suddenly at 200 cycles. For the
two concrete mixtures with MBV of 2.15 and 2.5, the
RDM decreased to less than 60% at 200 cycles. These
results indicate that increasing MBV of MS aggravates
the deterioration of concrete exposed to the freeze-thaw
environment, and reduces freeze-thaw resistance. The
reason is that the high moisture absorption of porous clay
particles decreases the strength of the capillary pore wall
in the cement matrix dispersed with clays, causing the
destruction of capillary pores and a decrease of relative
dynamic elastic modulus of concrete when exposed to
the freeze-thaw environment.

Table 4 Effect of MBV of MS on chloride ion permeability and freeze-thaw resistance of concretes cured for 28 days.
Chloride diffusion Relative dynamic modulus after exposure to Freeze-thaw
MBV
No. coefficient DNEL freezing and thawing cycles (%) durability
(g/kg)
(×10-12 m2/s) 50 cycles 100 cycles 150 cycles 200 cycles 250 cycles grade
1 0.35 2.03 99.5 98.8 98.6 98.5 98.3 ≥F250
2 0.70 2.08 98.9 97.2 99.1 96.5 97.3 ≥F250
3 1.10 2.05 99.1 98.7 98.1 85.2 67.2 F250
4 1.45 2.19 96.8 97.5 96.0 76.9 53.4 F200
5 1.80 2.25 97.3 96.5 93.2 63.2 31.8 F200
6 2.15 2.41 96.6 97.0 91.1 48.7 — F150
7 2.50 2.40 97.3 95.2 73.2 32.1 — F150
132 B. Li, M. Zhou and J. Wang / Journal of Advanced Concrete Technology Vol. 9, No. 2, 127-132, 2011
4. Conclusions
1) With increases of MBV of MS, the workability, the
flexural strength and 7d compressive strength of
concrete decreased, but 28d compressive strength
was not obviously influenced. The elastic modulus
of concrete began to decrease only when the MBV
was more than 1.8.
2) The increase of MBV of MS promoted the early
plastic cracking of fresh concrete and increased the
drying shrinkage of hardened concrete. Especially
when MBV was greater than or equal to 1.45, the
resistance of concrete to shrinkage cracks became
even worse.
3) With the increase of MBV of MS, the resistance of
concrete to chloride ion permeability was slightly
decreased, while the resistance of concrete to
freeze-thaw cycles and abrasion were seriously af-
fected. Especially when MBV was greater than or
equal to 1.45, the freezing-thawing destruction of
concrete was accelerated.
It can be concluded from the above experimental re-
sults that the increment of clay content, as indicated by
the MBV test, decreased the workability, the resistance
to plastic shrinkage cracking, early strength as well as
resistances to the freeze-thaw and abrasion of the MS
concretes. Especially, the MS with MBV of greater than
or equal to 1.45 is not suitable for preparing
high-performance concrete. It is advisable that the MBV
index be applied to control the clay content of MS. There
is a critical MBV of about 1.4, below which the per-
formance of MS concrete does not appear to be affected.
Acknowledgements
The financial support under the Science and Technology
Item of Communication Construction for West China
(grant number 2009318811082) is gratefully acknowl-
edged.
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