Construction and Building Materials 47 (2013) 10011009

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Construction and Building Materials

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Granitic quarry sludge waste in mortar: Effect on strength and durability

Telma Ramos a,, Ana Mafalda Matos a, Bruno Schmidt c, Joo Rio a, Joana Sousa-Coutinho a,b
a

LABEST-FEUP Department of Civil Engineering, Faculty of Engineering University of Porto, Portugal

FEUP Department of Civil Engineering, Faculty of Engineering, University of Porto, Portugal
c
Department of Civil Construction, Federal University of Paran, Curitiba, Brazil
b

h i g h l i g h t s
 An abundant waste was analyzed as cement replacement for strength and durability testing (ASR and Chlorides).
 Marginal workability and strength loss are observed for up to 10% cement replacement levels.
 Improvement of up to 38% reduction in ASR expansion was observed and up to 70% improvement into chloride resistance.
 SEM after ASR attack showed deeper surface grooving and thicker gel layers corresponding to higher measured expansion.
 SEM on mortar after chloride ingress showed that aluminates led to formation of chloroaluminates explaining good results.

a r t i c l e

i n f o

Article history:
Received 18 January 2013
Received in revised form 13 May 2013
Accepted 20 May 2013
Available online 22 June 2013
Keywords:
Waste
Quarry sludge
Granite
Sustainability
Concrete

a b s t r a c t
Granitic quarry sludge is an abundant waste from granite rock processing, causing serious environmental
concern. The use of this waste could become a valuable resource if properly engineered into a successful
solution as a partial cement replacement in concrete.
The effect of granitic sludge from a quarry in northern Portugal was analyzed as a partial cement
replacement in mortar in terms of strength and durability, so as to envisage its use in concrete.
The experimental program included chemical analyses, laser particle size distribution and scanning
electron microscopy of granitic quarry sludge, as well as mechanical strength, expansion due to alkali silica reaction and chloride penetration resistance on mortars containing different dosages of cement
replacement with granitic quarry sludge waste ground to different neness levels.
Results showed that granitic quarry sludge waste, if ground to sufcient neness, produces a denser
matrix promoting up to 38% reduction in expansion due to ASR and almost 70% improvement in resistance to chlorides, without compromising workability and strength. This surprising improvement in
terms of chloride resistance seems to derive from captivation of chlorides by aluminates present in the
waste with formation of chloroaluminates.
Finally, a properly engineered use of granitic waste in cement-based composites, leading to enhanced
durability can turn granitic quarry sludge, an abundant waste, into a valuable resource and therefore contribute to sustainable construction.
2013 Elsevier Ltd. All rights reserved.

1. Introduction
Concrete is the worlds most widely used building material.
Global production of concrete is about 12 billion tons a year [1]
corresponding to almost 1 m3 per person per year. Yearly cement
production levels are about 3 billion tons [1].
Adjustments and improvements to the present concrete making
methods are essential in order to address environmental and
economic issues. This has encouraged researchers in the area of

Corresponding author. Address: Rua do Dr. Roberto Frias, s/n, 4200-465 Porto,
Portugal. Tel.: +351 225081936; fax: +351 225081441.
E-mail address: telmajr@fe.up.pt (T. Ramos).
0950-0618/$ - see front matter 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2013.05.098

concrete engineering and technology to investigate and identify

supplementary by-product materials that can be used as substitutes for constituent materials in concrete production [2].
Cement industries contribute to about 7% of the total global CO2
emissions. This is due to the calcination of raw materials for the
production of cement and burning fuels needed to maintain high
temperatures in a kiln. In recent times, one of the most important
goals of the global environmental agenda is the reduction of emissions to protect the Earths climate pattern [1].
In fact an effective way to reduce CO2 emissions from the cement manufacturing process is the use of blended cement by
reducing clinker/cement ratio.
Production of cements with several main constituents like granulated blast furnace slag, y ash from coal power plants and natu-

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T. Ramos et al. / Construction and Building Materials 47 (2013) 10011009

Table 1
Particle size distribution of cement, PG and PGS.

CEM I 42.5 R
PG
PGS

d10 (lm)

d50 (lm)

d90 (lm)

0.69
1.55
0.84

8.09
13.05
3.48

30.81
55.46
13.34

ral pozzolans offer additional benets in cement performance [3],

especially in terms of durability properties.
In recent years there has been an increase in the consumption of
mineral additions by the cement and concrete industries. The use
of adequate industrial or agricultural by-products for partial cement replacement is an environmental friendly method of disposal
of large quantities of materials that would otherwise pollute land,
water and air [4].

The granite cutting industry produces large amounts of wastes,

solids (generated during extraction) and sludge (produced during
transformation processes) [5].
Granite nes are often referred to as quarry or rock dust, and
this residue generally represents less than 1% of aggregate production [6] or between 1% and 2% by mass of the total aggregate
crushed in quarries, according to Abukerh and Faireld [7].
Managing large amounts of sludge can be rather problematic for
its producers, which must nd appropriate places for storage and
deposition. Dumping into rivers and lagoons is obviously not an
environmentally safe solution and landlling has serious drawbacks. Transporting and dumping of waste in landlls involves
substantial costs; therefore, incorporating waste into other industrial processes could lead to a reduction of management costs and
open up new business opportunities. Some previous studies have
shown that granite sludge has a high potential as a raw material
for the ceramic industry and it is amenable to use as ller in dry

Table 2
Chemical composition of cement, PG and PGS.
Composition (% mass)

CEM I 45.2 R

PG/PGS

Requirements in ASTM 618 [15] (class N)

LOI
Insoluble residue
SiO2
Al2O3
Fe2O3
SiO2 + Al2O3 + Fe2O3
CaO
MgO
Na2O
K2O
SO3
Free lime
Pozzolanicity

2.61
1.33
20.36
5.1
3.12

2.04

610

62.72
1.81

3.44
1.62

63.22
15.66
4.47
83.35
3.26
1.82
2.68
5.02
0.00
Negative

Fig. 1. SEM photos of cement, silica fume, PG and PGS.

P70

64

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T. Ramos et al. / Construction and Building Materials 47 (2013) 10011009

Table 3
Mixture proportions and workability of mortars.
Mixture proportions

Control

Partial cement replacement of

5% PG

10% PG

5% PGS

10% PGS

SF

CEM I 42.5 R (g)

PG (g)
PGS (g)
SF (g)
Sand (g)
Water (ml)
sp/c (%)
w/c
Sp/Blinder
Workability (mm)

450

1350
225

0.5

427.5
22.5

1350
225

0.5

405
45

1350
225

0.5

427.5

22.5

1350
225

0.5

405

45

1350
225

0.5

200

201

199

199

198

405

45
1350
225
0.37
0.5
0.0035
198

Fig. 2. Flexural and compressive strength results at 28 days.

mortars [5]. In fact Mrmol et al. [5] studied granite sludge waste
for incorporation as alternative to ordinary limestone ller into cement-based mortar formulations. In this study ndings revealed
that the composition of this waste, the main components of which
are SiO2, Al2O3, CaO and Fe2O3 based compounds, together with the
small particle size, warrant its use by the mortar industry. It was
also concluded that 10% cement can be replaced with granite
sludge waste without loss of 28 d compressive strength. These results support the use of granite sludge waste in mortar by virtue of
their appropriate particle size distribution and potential pozzolanic
activity.

Albukersh and Faireld referred that concrete mixes containing

30% recycled red granite dust showed good fresh properties, better
than expected mechanical properties and excellent surface nish.
This concrete demonstrated better early age strength than similar
y ash based concrete [7].
Results of Felixkala and Ilangovana et al. also clearly show that
granite powder as a partial sand replacement has benecial effects
of the mechanical properties of high performance concrete [8,9].
According to Ho et al. [6] in normal concrete, the introduction of
quarry dust to mixes must be limited due to its high neness. Its
addition to fresh concrete would increase the water demand and
consequently the cement content for given workability and
strength requirements. In fact Ho et al. demonstrated that granite
nes, as supplied, could be used successfully in the production of
SCC. Compared to the use of limestone powder, both paste and
concrete studies conrmed that the incorporation of granite nes
required a higher dosage of superplasticizer for similar yield stresses and other rheological properties. However, it is important to
point out that as a waste material, the properties of granite nes
are expected to vary over time. Furthermore, the neness of granite nes could promote durability problems, such as alkali-silica
reactions. These two issues would need to be addressed if the
material is to be used with condence [6].
The present study aims at analyzing the effect of using granitic
quarry sludge as partial cement replacement on strength and durability of mortar in terms of not only alkali silica reaction but also
chloride ion ingress.

Fig. 3. ASR expansion versus time.

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T. Ramos et al. / Construction and Building Materials 47 (2013) 10011009

Fig. 4. ASR nal expansion after 14 days.

In fact, the rate of chloride ion ingress into concrete is of great

importance for the performance of reinforced concrete structures
exposed to chloride-contaminated environments. It is widely
known that diffusion of chloride ions in concrete is an important
aspect related to corrosion of reinforcement [10]. Corrosion of steel
in concrete occurs only if certain species are efciently transported
to the vicinity of the reinforcement. The presence of aggressive
agents such as chlorides can cause depassivation of the reinforcing
steel. This can happen in concrete even when the surrounding pH
is as high as 12.5 [11]. The property of diffusion of chloride ions in
concrete appears to be the dominant factor in this type of corrosion. Again, this property depends to a large extent on the pore size
distribution in the concrete matrix and whether the pore system is
continuous [12,13].
The experimental program carried out consisted of characterizing granite powder obtained from the dried and ground granitic
sludge waste taken from a quarry in northern Portugal. These tests
included chemical analyses, scanning electron microscopy (SEM)
and laser particle size distribution. Then mechanical and durability
properties were determined on mortar produced with different cement replacement dosages as well as for different neness levels of
the granite powder. Alkalisilica reaction (ASR) of mortar containing this waste was thoroughly analyzed and observations under
scanning electron microscopy (SEM) were carried out after ASR
testing for full understanding of the effect of granitic sludge.
Chloride ion penetration testing was also undergone on mortar
specimens with cement replacement by granitic powder and SEM
observations detailed and completed this study.
Results of this program show that granitic sludge waste, if
ground to sufcient neness and used up to 10% cement replacement in mortar does not compromise workability or strength and
greatly enhances durability in terms of resistance to ASR and
chloride ion penetration. These results may lead to the successful
use of this abundant waste in concrete.

2. Research programme and results

2.1. Materials and methods
Type I 42.5 R Portland cement (specic gravity 3.16 g/cm3) was used. Commercially available silica fume (SF) (specic gravity 2.20 g/cm3) was used as a reference
cement replacement material.
Granitic quarry sludge was dried at 105 5 C for 24 h and ground to two different levels of neness. The dried sludge was ground in a ball mill for 30 min
and is henceforward referred to as PG (Powder from quarry Granitic sludge). A ner

material, referred to as PGS (superne powder from granitic sludge) was obtained
from PG submitted to further grinding in a planetary mill RETCSH PM 100 using zirconia balls of 1 mm diameter, for 10 min at constant 450 rpm.
Particle size distribution and chemical composition for PG and PGS are shown in
Tables 1 and 2 respectively.
Chemical composition, which can be seen in Table 2, was carried out on granite
powder following NP EN 196:2 [14].
Pozzolanic activity was assessed by comparing the concentration of calcium ion,
expressed as calcium oxide, present in the aqueous solution containing the binder,
in this case 90% cement and 10% PG, after 15 days, with the quantity of calcium ion
capable of saturating a solution of the same alkalinity, as described in NP EN 196-5
[15]. The binder tests positive for pozzolanicity if the concentration of calcium ion
in the solution is lower than the saturation concentration. Results obtained were a
CaO concentration of about 13.6 mmol/l and a OH-concentration of 48 mmol/l,
leading to a negative result, as expected.
Fig. 1 shows scanning electron microscopy (SEM) carried out on cement, silica
fume and PG/PGS samples. Commercially available silica fume with over 99% SiO2
was used for comparison. As can be observed PG particles are coarser than cement
particles and PGS particles are ner in accordance with the particle size distribution
curves. PG and PGS particles seem more angular and more prismatically shaped
compared to cement particles which look rounder. Silica fume spherical particles
are far smaller than the PG and PGS and cement, as expected.
Six mortar types were prepared following the procedure described in NP EN
196-1 [17]: a control mix with 100% cement (CTL), two mixes with 5% (PG 5%
and PGS 5%) cement replacement with granitic powder (PG) and superne granitic
powder (PGS), respectively, two mixes with 10% (PG 10% and PGS 10%) cement
replacement with PG and PGS, respectively and a last mix with 10% (SF) cement
replacement with silica-fume.
Mortar workability was maintained at the same level and measured according
to ASTM C 109 [18] and ASTM C 230 [19], and the results are given in Table 3.
Superplasticizer (Sikament) was only needed for silica fume mortar.

2.2. Strength
Flexural and compressive strength testing was undertaken at 28 days, on
40  40 mm  160 mm mortar specimens, following standard procedure in NP EN
196-1 [17]. Results of exural and compressive strength are presented in Fig. 2.

2.3. Alkali silica reaction (ASR)

In order to measure the ASR expansion for a given mix proportion, an
accelerated mortar bar test was carried out on three prism specimens of
25  25  250 mm in accordance with ASTM C 1567 [20].
After 24 h of production, mortar bar specimens were demoulded and stored in
distilled water at 80 C for another 24 h after which a zero reading was taken. The
bars were then transferred and immersed in 1 N NaOH (1 Normal Sodium Hydroxide solution) at 80 C.
Expansion of each mortar bar was measured within 15 5 s after being removed from the 80 C distilled water or alkali storage condition by using a length
gauge. Measurements were taken for 14 days.
Expansion with time and nal expansion of mortar type are shown in Figs. 3
and 4, respectively.

T. Ramos et al. / Construction and Building Materials 47 (2013) 10011009

1005

(a)

(b)

(c)
Fig. 5. SEM on PGS (a) and CTL specimens submitted to ASR (b) and reactive sand before attack (c).

Combinations of cement, pozzolanic materials and aggregate that expand more

than 0.1% (14 days in solution) are indicative of potentially deleterious expansion.
However, the occurrence of deleterious reaction should be conrmed by testing
the same combination of materials in concrete.
After testing for ASR, SEM with EDS spectrums were undertaken on PGS (Fig. 5a)
and CTL (Fig. 5b) mortar specimens (Figs. 57). SEM photos were also taken on reactive sand used, prior to ASR, and show in Fig. 5.

It is based on measuring the depth of color change of a silver nitrate solution

sprayed on specimens previously submitted to a migration test and application of
the following equation [22,23]:

p
RTL xd  a xd
ZFU
t

r


RTL
2C
e; e erf 1 1  d
C0
ZFU

Dns

a2
2.4. Chloride ion diffusion
The rapid chloride migration test (CTH) is a non-steady-state migration method
based on a theoretical relationship between diffusion and migration which enables
the calculation of the chloride diffusion coefcient from an accelerated test [21].

where Dns is the apparent diffusion coefcient obtained in a non-steady-state migration test (cm2/s); R the gas constant R = 8.314 J/(mol K); T the absolute temperature
(K); L the thickness of specimen (cm); Z the ion valence; F is Faraday constant; constant F = 9.648  104J (V mol); U the effective voltage applied (V); xd the depth of
chloride penetration measured by using a colorimetric method (cm); t the time of

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T. Ramos et al. / Construction and Building Materials 47 (2013) 10011009

Fig. 6. SEM and EDS on CTL mortar after ASR.

Fig. 7. SEM and EDS on PGS 10% mortar after ASR.

the test duration (s); a the laboratory constant; e = 0.0764 if external chloride concentration of 0.5 M; C = 0.0764 if external chloride concentration of 0.5 M; Cd the
concentration of free chloride at which the color changes when using the colorimetric method to measure the chloride penetration depth (kg/m3solition); and C0 is the
concentration of free chloride in the external solution.

The procedure for determining the apparent diffusion coefcient (Dns) consisted
of: after switching off the electrical eld the specimens were split in two halves and
the penetration of chlorides was measured by using the colorimetric method. This
method consists of spraying silver nitrate solution over the split faces, storing them
in a dark place for 1 h and then exposing them under a uorescent light for a few

T. Ramos et al. / Construction and Building Materials 47 (2013) 10011009

Fig. 8. Apparent diffusion coefcient Dns (cm2/s).

hours, after which the average front of the white zone in the central part of each
specimen is measured with a precision of 0.5 mm. Apparent diffusion coefcient
Dns results are shown in Fig. 8.
SEM was carried out on PGS 5% and PGS 10% mortar specimens after the accelerated chloride ion penetration test. Photos are show in Figs. 9 and 10.

3. Discussion
As can be seen in Table 2, quarry granite sludge is mainly
composed of silica and alumina, chemically similar to granite

1007

sludge wastes studied by Mrmol et al. [5] and Abukersh and Faireld [7]. Chemical properties are in accordance with requirements
stated in ASTM C 618 [16] regarding pozzolanic materials.
SEM observations, Fig. 1, indicate that quarry granite sludge
particles seem more angular, more elongated and more prismatically shaped compared to cement. This conrms ndings by Ho
et al. [6] who observed that the shape of granite nes is akier
and more elongated compared to limestone particles.
SEM and laser particle size distributions, Table 1, show that PG
particles are slightly coarser than cement. However PGS is ner
than cement and naturally, both are much larger than spherical silica fume particles.
According to Ho et al. [6] and as stated before, the introduction
of quarry dust to mixes is limited due to its high neness. Its addition to fresh concrete would increase the water demand and consequently the cement content for given workability and strength
requirements. However, as can be seen in Table 3, no superplasticizer was needed for mortar containing PG and PGS where similar
workability was obtained, comparing with control mortar. There
was no need of extra superplasticizer when using quarry powder
could, therefore, be an economic advantage for future use in concrete mix design.
Strength results for PG and PGS mortars at 28 days were lower
than control, where exural and compressive strength decreased
with increase of replacement dosage. Nevertheless strength loss
is marginal when using PGS. This conrms ndings by other
authors such as Abukersh and Faireld [7] for coarser granite dust

Fig. 9. SEM and EDS specimens on PGS5% specimens submitted to chloride testing.

Fig. 10. SEM and EDS specimens on PGS 10% specimens submitted to chloride testing.

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T. Ramos et al. / Construction and Building Materials 47 (2013) 10011009

for PGS mortar where the ner material seems to induce a denser
matrix leading to a better resistance to chloride compared to SF
mortar. In fact improvement of this resistance to chlorides was almost 70% compared to CTL and improved with dosage replacement
(67% reduction for PGS 5%, 70% for PGS 10% and 66% for SF).
Figs. 9 and 10 show SEM and EDS results on mortar specimens
after chloride ingress. As can be observed for PGS (5% and 10% cement replacement) chloroaluminates (Friedels salt) according to
[24,25] were frequently found, some of which shaped as hexagonal
plates in accordance with St. John et al. [26]. The presence of chloroaluminates suggests that alumna present in granite sludge may
react with chlorides and thus retard chloride ingress. This may help
explain lower apparent chloride diffusion coefcients for PGS,
however neness of granite sludge as a partial cement replacement
material plays an important role as this effect is only revealed for
sufcient neness.
Performance of mortar with granite powder is compared to CTL
in Fig. 11. SF mortar results are also presented for reference. PG
mortar showed worst performance but PGS mortar presented better results than CTL, close to SF results and even better in relation
to chlorides for PGS 10 mortar.

Fig. 11. Performance of mortars compared to CTL mortar.

(d50 < 38 lm), by Ho et al. [6] for granite sludge waste, also coarser
(d50 = 23.8 lm) and by Mrmol et al. [5] where granite sludge
waste was also coarser with 80% of particles with a diameter of
260 lm [5].
Coarser granite sludge, this is PG must have led to more voids in
the mix hardened structure compared to cement only structure.
This may explain lower mechanical strength of PG containing mortar as well as higher ASR expansion and higher apparent diffusion
coefcients (Dns).
Analyzing ASR results, for PG there was generally no improvement of resistance to ASR compared to CTL but for PGS, expansion
reduced with increase in replacement (19% reduction for PGS 5%
and 38% for PGS 10%). Nevertheless PGS was not as effective as
SF (reduction of 81%, compared to CTL).
Considering ASR SEM observations, a reactive sand particle is
shown in Fig. 5c at different magnications where the morphology
of the surface can be observed and compared to the grooved surfaces of a sand particle in mortar after attack by alkalis where
ASR gel can also be detected in Fig. 5a and b. Differences in PG
and CTL mortar can be observed in terms of the intensity of the
grooves resulting from the alkalis attack and also the thickness of
the gel resulting from the ASR attack on the surface of the reactive
sand particles. In Fig. 5a and b for 5000 times magnication,
grooves on the surface of a reactive particle in CTL mortar seem
ravenous canyons compared to the smoother and less marked surface of a reactive particle in PGS mortar. Comparing for example,
Fig. 5a and b for 1000 times magnication it can be seen that the
layer of ASR gel formed on the surface of the reactive aggregate
in CTL mortar is thicker than the layer formed in PGS mortar.
EDS was carried out and gel was found in the grooves of the surface of the aggregate or in the layers covering the aggregate. This
gel has considerable amount of sodium as can be seen in the spectrum, showing that this is ASR gel. Although PGS containing mortar, compared to CTL mortar, presented lower overall expansion
in the ASR test, ASR gel was still found in grooves and as layers
on the aggregate surface.
In terms of chloride ion ingress, for coarser waste material such
as PG, a resulting more permeable matrix reduced chloride resistance around 20% compared to CTL (22% increase of Dns for PG
5% and 15% for PG 10%). Surprisingly positive results were obtained

4. Conclusion
Quarry granitic sludge waste studied is mainly composed of silica and alumna and therefore in accordance with chemical requirements in ASTM 618 [16] regarding pozzolanic materials.
Particles observed in SEM showed to be more angular and elongated compared to cement but this did not seem to affect workability of mortar.
Mortars Strength at 28 days for coarser (PG) and ner (PGS) granitic sludge waste used at 10% cement replacement was lower than
control mortar but strength loss was marginal for PGS.
In terms of ASR there was generally no improvement of resistance to alkali reaction for PG mortar but for PGS, expansion reduced with increase in replacement dosage although not
attaining effectiveness of SF mortar.
SEM observations and EDS analysis on reactive aggregate particles prior to ASR attack and also after ASR testing led to the following conclusions:
 ASR testing leads to varying groove depth on the surface of the
attacked aggregate surface.
 ASR testing leads to the formation of a varying layer thickness of
the gel formed on the surface of the attacked aggregate surface.
 More deeply grooved surfaces of the attacked aggregate correspond to thicker gel layer formed.
 It seems that deeper grooved surfaces resembling ravinous canyons and thicker ASR gel layers were observed on CTL mortar,
corresponding to higher measured expansion results.
In terms of chloride ingress, the coarser waste material, PG reduced chloride resistance but for PGS, ner than cement, an
improvement of almost 70% was observed in the resistance to chlorides. SEM and EDS analysis on PGS specimens after chloride ingress revealed the presence of chloroaluminates, suggesting that
alumna present in granite sludge ground to sufcient neness, reacts with chlorides, thus retarding chloride penetration.
Therefore this work showed that granitic quarry sludge waste, if
ground to sufcient neness, produces a denser matrix promoting
up to 38% reduction in expansion due to ASR and almost 70%
improvement in resistance to chlorides (higher than SF mortar).
This surprising improvement for ne waste seems to derive from
captivation of chlorides by aluminates present in the waste with
formation of chloroaluminates.

T. Ramos et al. / Construction and Building Materials 47 (2013) 10011009

Finally, a properly engineered use of granitic waste in cementbased composites, leading to enhanced durability without compromising workability and strength as shown in this study, can turn
granitic quarry sludge, an abundant waste, into a valuable resource
and therefore contribute to sustainable construction.
Acknowledgments
The authors would like to thank DST-DOMINGOS DA SILVA
TEIXEIRA, S.A., the R&D unit LABEST, Laboratory for Concrete Technology and Structural Behaviour and to LEMC, Laboratory for Testing Construction Materials. This work was nanced by FEDER
funds under the Operational Program Factors of Competiveness
COMPETE and by National Funds under FCT Foundation for Science and Technology through Project PTDC/ECM/098117/2008:
Additions from waste materials for sustainable structural concrete.
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