Construction and Building Materials 112 (2016) 790–799

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Construction and Building Materials

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

Utilization of sludge from ready-mixed concrete plants as a substitute

for limestone fillers
Mariane Audo, Pierre-Yves Mahieux ⇑, Philippe Turcry
Laboratoire des Sciences de l’Ingénieur pour l’Environnement, Université de La Rochelle, Avenue Michel Crépeau, 17000 La Rochelle, France

h i g h l i g h t s

Environmental impacts of sludge coming from ready-mixed concrete plants.

Substitution of limestone fillers by sludge coming-from ready-mixed concrete plants in mortars formulation.

Mechanical characterization of mortars made with sludge coming from ready-mixed concrete plants.

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

Article history: This study deals with the incorporation of sludge coming from ready-mixed concrete plants into mortars.
Received 12 May 2015 Preliminary environmental investigations, made through leaching tests, showed the importance of
Received in revised form 12 January 2016 managing those waste as they can be potentially pollutant regarding to their arsenic and chromium con-
Accepted 16 February 2016
tents. Thus, management of the sludge can be environmentally and economically difficult.
Reincorporation of those sludge into a closed loop concrete production is of particular interest. Also, it
represents an interesting way to save raw materials (water, sand and limestone fillers). Yet, two main dis-
Keywords:
advantages were observed when using those sludge as limestone fillers substitute:
Ready-mixed concrete plant sludge
Waste management
– a decrease in the workability of the fresh state mortar, calling for a higher superplasticizer content;
Environmental impact – a variability in the compressive strength of the hardened state mortars, between 30% and +17%
Mortar design when comparing to a reference mortar.
Physical characterization Ó 2016 Elsevier Ltd. All rights reserved.
Mechanical characterization

1. Introduction
European ready-mixed concrete production has notably
increased over the last decades. Since 2010, around 370 million
cubic meters of ready-mixed concrete are produced each year in
Europe, of which around 10% come from the French production
[1]. From this high production results a high level of by-products.
Indeed, it has been estimated that a 9-m3 truck contains daily
around 300 kg of returned concrete [2]. Generally, this leftover
concrete is discharged in large containers. The hardened concrete
can be then crushed and easily used as recycled aggregates for road
construction. After the leftover being discharged, the truck is
washed out with huge amounts of water, up to 1300 L per truck,
and the suspended matter is allowed to settle in large sedimenta-
tion basins. Wash-waters from mixers are also directed to those
basins. Several studies have been focused on the reuse of the clar-
ified water of those basins, which presents a high up to 12 pH. This
water can be partially reused for trucks washing or in concrete pro-
⇑ Corresponding author.
E-mail address: pierre-yves.mahieux@univ-lr.fr (P.-Y. Mahieux).
duction [3,4,5]. Su et al. showed that, according to the total sus-
pended solids content, shorter setting times and a lower
flowability are obtained [3]. On the opposite, Chatveera et al. high-
lighted a time lag when using sludge water and no additives nor
admixtures, but reported a flowability decrease as well [5]. In
another study, the use of the wet sludge as partial cement or sand
substitute leads to a decrease in the compressive strength [6].
Recently, a study was led on the use of the sludge as a new raw
material for Portland clinker production [7]. The variability in the
chemical composition of the sludge leads to an impossibility in
their reuse for Portland clinker production, due to their high chem-
ical variations, as well as their high alkali, SO3 and MgO contents.
Yet, not many studies have dealt with the utilization of the set-
tled sludge, made of the fines particles (cement, mineral additions,
etc.) as well as sand and aggregates. Though, it represents a large
available quantity of raw material. As around 1 m3 of wet sludge
is created by the production of 90 m3 of concrete, around 4 millions
of cubic meters are produced every year in France [8]. Wet sludge
is collected several times a year at the bottom of the basins and
stored on the ready-mixed concrete plant area so that the water
content decreases. When the water content is low enough, the

http://dx.doi.org/10.1016/j.conbuildmat.2016.02.044
0950-0618/Ó 2016 Elsevier Ltd. All rights reserved.
 M. Audo et al. / Construction and Building Materials 112 (2016) 790–799
material can disposed of at controlled landfills for inert wastes,
regarding to the French decree on passive wastes [9]. Up to now,
not many characterizations of this sludge have been led in the lit-
erature. However, their hazardous behavior has already been high-
lighted, due to their high alkalinity and their high heavy metals
and metalloid elements content [10]. All these factors lead to a
high whole total disposal cost of the sludge. That is why new envi-
ronmental friendly strategies must be found for sludge managing.
We herein propose a new original way to valorize sludge as
limestone fillers substitutes in a closed loop concrete production,
avoiding any environmental and economical impacts. Neverthe-
less, for now, the European standard does not allow the utilization
of non-standard mineral addition in concrete [11]. Thus, the objec-
tive of this study is to prove the feasibility of incorporating sludge
into concrete. To reach that aim, the sludge coming from four
French ready-mixed concrete plants were firstly characterized
from a chemical and physical point of view. The activity index of
the dry sludge, as well as their chemical activities were deter-
mined. Giving those results, utilization of the studied sludge into
mortars compositions was studied using the concrete equivalent
mortar concept [12]. Compressive strength and porosity were
studied at various due dates, and relationship between mortars
composition and compressive strength was stated.
2. Experimental program
2.1. Raw materials
The studied sludge were sampled at four ready-mixed concrete plants (C1, C2,
C3, C4) located in the Poitou-Charentes area, France (Fig. 1). Those four plants pro-
duce basically the same main concrete, whose formulation will be given later. The
samples had a high water content, between around 50 and 120%, depending on the
weather conditions and the storage duration. The moisture contents are presented
in Table 1.
The raw materials were then split in two fractions: one finer than 100 lm (frac-
tion A) and one coarser than 100 lm (fraction B).
Limestone filler (designed as LF), CEM II/A 42.5 and CEM I 52.5 cements were
provided by Carmeuse (Saint Porchaire, France), Calcia (Airvault, France) and
Lafarge (Saint Pierre La Cour, France) companies, respectively. Their properties
are given in Table 2. 0/4 mm sand from Sablimaris Pallice (La Rochelle, France)
was used in the studied mortars. For the determination of activity index, a standard
sand from the SNL Company (Leucate, France) was used. Chrysofluid Optima 220
superplasticizer was used for the fabrication of mortars.
2.2. Characterization of raw materials
2.2.1. Leaching tests
Leaching tests were performed following the French standard dedicated to
sludge characterization [13]. Basically, a test portion of sludge containing 90 g of
dry matter is poured into a 1L HDPE flask. Deionized water is added so that the total
water content is 900 mL. The whole mixture is kept under continuous mechanical
Fig. 1. Picture of the raw materials coming from the C4 ready-mixed concrete plant.
791
Table 1
Water contents of the sludge
C1 C2 C3 C4
Water content (%) 47.1 99.5 120.3 155.2
stirring for 24 ± 0.5 h (Fig. 2). The mixtures are then filtered over a 2 lm filter with
a Büchner apparatus and the filtrate is recovered for further analysis. Right before
the analysis, samples were filtered on 0.45 lm syringe filter.
All the leachates are diluted tenth and hundredth in a 5% HNO3 solution (77 mL
of HNO3 – FisherScientific, Trace Metal Analysis quality – completed to 1 L with
milli-Q water). Ba, Cr, Cu, Mo, Ni, Pb and Zn were analyzed with a Varian Vista
Pro ICPOES and As, Cd and Se with a ThermoFischerScientific Xseries2 ICPMS. The
quantification limits (lg L1 solution) were 2 (As), 2 (Se), 0.1 (Cd), 50 (Ba), 10(Cr),
10 (Mo), 10 (Ni), 10 (Pb) and 50 (Zn). To check the analytical data precision, all sam-
ples were analyzed in duplicate.
Ionic chromatography was also performed on the leachates. A Metrohm appa-
ratus with a Metrosep A Supp 5 100/4.0 column and an automatic sample changer
was used. A Na2CO3 3.2 mM/NaHCO3 1.0 mM (1:1, v/v) eluent was used, with a
0.7 mL/min flow. F, Cl and SO2 4 were so quantified. Sodium salts from Sigma-
Aldrich company were used as standards. The quantification limits were 0.5 mg L1
for F, Cl and SO24 .
2.2.2. Physical and mineralogical characterization
Water content of sludge (defined as mass ratio of water over dry matter) was
determined by drying at 80 °C until constant weight. Specific surfaces of the dry
raw materials were determined with a Blaine apparatus, allowing the measurement
of the resistance of the air passing through a porous bed of powder [14]. The den-
sities were determined using a water pyknometer according to the European Stan-
dard NF EN 1097-7 [15].
The particle-size distribution of the dry sludge was determined by sieving 500 g
of powder at 4, 2, 1.25, 0.5, 0.25, 0.125 and 0.100 mm. The 100 lm passing fraction
was characterized by dynamic light scattering with a CILAS 1190 apparatus, used in
dry mode. Calculations were performed using the Mie theory [16].
Powder X-Ray Diffraction (XRD) was carried out with a Brücker diffraction
instrument, with Cu Ka1 radiation. Measurement range was from 5 to 70° 2b, with
a 0.02° step. Identification of the peaks was performed by comparison to a database
references.
Thermogravimetric analysis (TGA) was performed on a Setaram Setsys Evolu-
tion 16/18 apparatus. Around 100 mg of samples were heated from 20 °C to
1000 °C at a 10 °C/min heating rate, under neutral argon atmosphere. To get more
accurate results, data were analyzed through the differential thermogravimetric
curves.
ICP-AES analysis were performed sludge materials after their drying at 80 °C
and after being grinded to 80 lm. Basically, around 100 mg of dry materials was
digested using 4 mL of a 67–70% HNO3 – 34–37% HCl 2:2 (v/v) solution (FisherSci-
entific, Trace Metal Analysis quality). Acidic digestion of the samples was carried
out overnight at room temperature. Each sample was completed to 50 mL with
milliQ water. Al, Ca, Fe, S and Si were analyzed with a Varian Vista Pro ICPOES.
The quantification limits (lg g1 dry weight) were 500 (Ca), 100 (Al), 50 (Si), 10
(S) and 5 (Fe).
2.2.3. Determination of sludge activity
The potential activity of sludge was evaluated through compressive tests on
standard mortars. We focused on the sludge fraction lower than 100 lm which
should contain the most reactive elements. For this purpose, an activity index
was determined according to the French standard dedicated to limestone additions
[17]. A mortar made of CEM I cement, deionized water and standard sand was made
and used as reference. A second mortar was made by substituting 25% of the cement
mass by the 100 lm passing fraction of the sludge. Mortars compositions, as well as
the water-to-cement ratio (W/C) are given in Table 3. Compressive strengths were
determined on 28-day old mortars kept in water. The activity index (denoted i) of
the sludge was defined as the ratio between the compressive strength of the mortar
with sludge and the one of the reference mortar.
The activity of sludge was also investigated through ionic conductivity mea-
surement. This test is based on the measurement of time-evolution of the ionic con-
centrations during the cement hydration in aqueous suspension. As done in the case
of activity index, only the 100 lm passing fraction of sludge was used. The ionic
conductivity time-evolution of the cement and blends (‘‘limestone filler + cement”
and ‘‘dry sludge + cement”) were obtained by measurements in dilute medium. In
the blends, the ratios between cement and dry sludge or limestone filler were the
same as the ones used for the CEM mortars. The same cement as the one used in
the concrete formulation was used. The composition of the blends is given in
Table 4.
Briefly, 300 mL of deionized water are poured into a cell equipped with a con-
ductivity probe. The whole system is kept at 25 °C and under perpetual mechanical
stirring. A 1–5 solid-to-liquid ratio is applied, which allows a good sensitivity, as
792 M. Audo et al. / Construction and Building Materials 112 (2016) 790–799

Table 2
Properties of cements and limestone filler.

Physical properties Clinker composition (%) Carbonates content

(%)
Density (g/cm3) Blaine (cm2/g) Clinker (%) CaO SiO2 Al2O3 Fe2O3 SO3 CaCO3 MgCO3
CEM I 52.5 3.15 3650 98 64.5 20.1 5.0 3.1 3.3 – –
CEM II/A 42.5 3.12 3800 92 63.0 18.7 4.5 3.2 2.7 6.0 –
LF 2.70 3530 – – – – – – 95.0 3.7

designed with sludge. Firstly, it was chosen to use dry sludge, even if from an indus-
trial point of view, using wet sludge would avoid any costly drying process. At a lab-
oratory scale, using dry sludge allowed us a better mastering of the water content in
the mortars. Secondly, the mix proportions were derived from the CEM mortar. Dry
sludge was used as a substitute of all the limestone filler and of part of the sand con-
tained in the CEM mortar. The mass ratios between the dry sludge and the sand in
the sludge-made mortars were determined by setting the particle-size distribution
of those mortars identical as much as possible to the one of the CEM mortar. To
determine the masses of dry sand and dry sludge, a second condition was applied
to close the equations system: the volume (i.e. sand + mineral addition + cement
+ water) of both mortars was fixed equal. The dry sludge-made mortars composi-
tions (denoted C1-CEM, C2-CEM, C3-EM and C4-CEM) are given in Table 6.
Mortars were also designed with wet sludge to monitor the influence of the
water content of the sludge on the properties of the mortars (Table 7). Tap water
contents were adjusted following the sludge water contents.
The sludge was mixed with cement and sand for 30 s at low speed [11]. Tap
water was then added and the blend was mixed for additional 30 s at low speed.
After scraping, another 30 s mix were applied at high speed [11]. Some superplas-
ticizer (Chrysofluid Optima 220) was added so that the slump at the Abrams mini-
Fig. 2. Picture of the mechanical stirring system. cone test was the same as the CEM mortar one. A vibration table was used to fill the
4  4  16 cm molds with the mortar. After removal from the moulds (24 hours
after their manufacturing), all the mortars were kept into water at 20 °C until their
later characterization.
Table 3
Compositions of mortars used to determine activity index.
2.3.2. Mortars characterization
Standard mortar Standard mortar
Fresh mortars were characterized by slump measurement with a cylinder
(reference) with sludge
(H = 100 mm, d = 50 mm).
Standard sand (g) 1350.0 1350.0 Heat releases determination were performed following a protocol adapted from
CEM I 52.5 cement (g) 450.0 337.5 the semi-adiabatic Langavant method [19]. This method consists in the introduc-
Dry sludge (<100 lm) (g) – 112.5 tion of a reference fresh mortar (denoted CEM’, Table 6) and the studied fresh
Deionized water (g) 225.0 225.0 sludge-based mortar into two separates 800 cm3-Dewar flasks and the measure-
W/C 0.50 0.66 ment of the difference of temperature in the core of the mortars at any time. In
the reference CEM’ formulation, no limestone filler was used. Indeed, it had been
substituted by the quantity of CEM II cement having the same hydraulic activity.
It has to be noted that the mortars were made without any superplasticizer addi-
tion. Indeed, it is known that chemical admixtures can modify hydration kinetics
well as a short reaction time. At the zero time, 75 g of cement, cement and filler or
[20] and we herein want to monitor the inherent influence of sludge on hydration.
cement and dry sludge are added and the conductivity is measured every 5 s during
Compressive strength was determined at the ages of 2, 7 and 28 days using the
the first 30 min and every two minutes during the last 7h30 [18].
4  4  16 cm prisms, with a Zwick press (loading rate = 2200 N/s and pre-
load = 3000 N). 4 measurements were performed on each mortar formulation.
Experimental variability will be indicated as error bars on graphs. Porosity was
2.3. Study of mortars made with sludge
measured at the age of 28 days by water soaking following the recommended
method [21].
2.3.1. Mortars mix proportioning
Mortars were designed using the concrete equivalent mortar concept [12]. The
latter is based on the substitution of the coarse aggregates of concrete by a certain
3. Results and discussion
quantity of sand in the mortars, which develops the same area as the coarse aggre-
gates do. This method was firstly developed in order to easily detect compatibility
troubles between cements and superplasticizers. It is also a convenient method for 3.1. Sludge characterization
comparison studies in laboratory.
The mortars compositions were obtained from a reference concrete mixture 3.1.1. Leaching behavior
given in Table 5. The latter corresponds to a ‘‘XC1 C20/25” concrete according to
European standard [11], with W/C = 0.6. It is usually produced by the four ready-
The results of the chemical analysis led on the leachates are pre-
mixed concrete plants where the studied sludge come from. The equivalent mortar sented in Table 8. Concerning the anions contents, fluorides, chlo-
derived from the reference concrete is denoted CEM in Table 6. Mortars were also rides and sulfates contents comply with the limit values of the

Table 5
Table 4 Compositions of reference concrete (kg per m3).
Composition of the blends for ionic conductivity measurements.
Weight (kg/m3)
CEM II/A (g) Sludge (fraction A) (g)
Gravel 10/20 823
Cement 75.00 – Gravel 6/10 352
Limestone filler 67.53 7.47 Sand 0/4 775
C1 67.99 7.01 Cement CEM II/A 253
C2 67.74 7.26 Limestone filler 28
C3 69.15 5.85 Water 169
C4 69.74 5.26 Superplasticizer (%) 0.6
 M. Audo et al. / Construction and Building Materials 112 (2016) 790–799 793

Table 6
Compositions of the studied mixtures with dry sludge (kg per m3).

CEM mortar C1-CEM mortar C2-CEM mortar C3-CEM mortar C4-CEM mortar CEM’ mortar
Sand 0/4 1476 1290 1391 1335 1427 1476
Cement CEM II/A 424 424 424 424 424 436
Limestone filler 47 0 0 0 0 0
Dry sludge 0 185 109 149 79 0
Water 283 283 283 283 283 283
Superplasticizer (%) 0.2 0.6 0.5 0.8 0.9 0

Table 7
Compositions of the studied mixtures with wet sludge (kg per m3).

CEM mortar C1-CEM mortar C2-CEM mortar C3-CEM mortar C4-CEM mortar
Sand 0/4 1476 1290 1391 1335 –
Cement CEM II/A 424 424 424 424 –
Limestone filler 47 0 0 0 –
Wet sludge 0 272 218 328 –
Water 283 144 174 104 –
Superplasticizer (%) 0.2 1.6 2.0 1.2 –

European decision concerning the acceptance of waste at landfills.
Concerning the heavy metals and metalloids content, special atten-
tion must be paid to the arsenic and chromium elements, as the
detected values are sometimes slightly higher than the limit values
for inert waste [22]. Consequently, the sludge cannot be surely sta-
ted inert materials. This point is of particular importance from an
environmental and economical point of view. Indeed, the price
concerning the waste storage is directly depending on the category
they belong to: 8 €/t for inert waste over 40 €/t for non-dangerous
waste [23]. Nevertheless, the measured suspicious concentrations
are right above the inert waste acceptability limit. Thus those
results need to be completed by analyzing new sludge.
Regarding to those results, finding a way to avoid storage of
sludge becomes of particular interest. Thus, incorporation into
cement matrix could be a promising, innovative and easy way to
valorize them.
3.1.2. Physical and mineralogical properties
The particle-size distributions analysis of the four dry sludge
showed a continuous material containing between 20 to 40% of
particles finer than 100 lm (Fig. 3, sieving). Nevertheless, the
particle-size distribution of the fractions finer than 100 lm
remains almost the same for all the sludge (Fig. 4, dynamic light
scattering). Moreover, this distribution is very closed to the one
of limestone filler. Indeed, two of the four modes of the filler are
observed on the sludge. The dmax of all sludge being less than
8 mm, it makes them a priori convenient for a use as sand and min-
eral addition substitute.
Measurements of density were led on those two fractions
(Table 9). The results showed that both fractions have a lower den-
sity (around 2.2) than the limestone fillers (2.7). Compared to frac-
tion B, the fraction A slightly lower density can be explained by a
higher cementitious materials content and a lower sand content.
Concerning the specific surface, the one measured on the fraction
A is up to 5 times higher than the one of the limestone fillers,
which could be explained by a higher open porosity or different
morphology.
XRD patterns were also acquired on each fraction (Fig. 5). Basi-
cally, the same peaks were observed for all samples, but with var-
ious proportions. The coarsest material is mainly made by
aggregates. Indeed, quartz (SiO2) and limestone (CaCO3) were
observed, as well as aggregates formed by portlandite (Ca(OH)2)
and/or C–S–H conglomeration. The composition of the finest frac-
tion is more complex. Quartz, limestone and portlandite were
identified as main constituents, but gypsum (CaSO42H2O), as well
as anhydrous (2CaOSiO2; 3CaOSiO2) and hydrated calcium sili-
cates were also observed. The presence of anhydrous calcium sili-
cates show a potential residual hydraulic activity. While no
ettringite (6CaOAl2O33SO332H2O) was identified, some hydrated
calcium carboaluminates (3CaOAl2O3CaCO311H2O) have been
detected. In literature, it has already been shown that this kind
of compounds can be formed during the hydration of cement

Table 8
Sludge leachates composition (g/kg of dry matter) and criteria of acceptance of waste at landfills [22] (in bold: inert waste value exceeded). Up: Heavy metals and metalloid
elements contents; Down: Anions contents.

As Ba Cd Cr Cu Mo Ni Pb Se Zn
C1-sludge 0.54 12.53 <0.001 0.37 0.23 <0.11 <0.11 <0.11 <0.02 <0.56
C2-sludge 0.15 17.70 <0.001 0.31 0.32 <0.11 <0.11 <0.11 <0.02 <0.56
C3-sludge <0.02 13.41 <0.001 0.64 <0.11 <0.11 <0.11 <0.11 <0.02 0.71
C4-sludge <0.02 14.16 <0.001 0.12 0.31 <0.11 <0.11 <0.11 <0.02 <0.56
Inert waste 0.5 20 0.04 0.5 2 0.5 0.4 0.5 0.1 4
Non-dangerous waste 2 100 1 10 50 10 10 10 0.5 50
F Cl SO2
4

C1-sludge <8.37 39.91 5.65

C2-sludge <4.61 49.91 13.27
C3-sludge <8.77 182.81 5.07
C4-sludge <8.76 39.47 3.84
Inert waste 10 800 1000
Non-dangerous waste 150 15,000 20,000
794 M. Audo et al. / Construction and Building Materials 112 (2016) 790–799
Fig. 3. Particle-size distribution of the dry sludge.
containing limestone (such as CEM II type cement), from the time-
conversion of hemicarboaluminates [24]. As the studied ready-
mixed concrete plants mainly use a CEM II/A cement with lime-
stone addition, the presence of hydrated calcium carboaluminates
in the sludge was expected.
Limestone and portlandite contents were both determined with
TGA. After differentiation, the typical curve showed four main
peaks (Fig. 6). The first two ones, observed between 25 °C and
250 °C result from the free water evaporation, as well as the water
loss coming from the dehydration of the C–S–H and calcium car-
boaluminates. Around 460 °C is observed the signal due to the
dehydroxylation of portlandite. The last peak is due to the CO2 loss,
corresponding to the decarbonation of the limestone. The integra-
tion of those peaks allowed us to determine the mass losses and
consequently, the calcium carbonate and portlandite contents
(Table 9). The weak peaks near 300 °C and 400 °C may be attribu-
ted to polymeric additives decomposition. The latter peak may also
be attributed to the quartz dehydroxylation.
Fractions A present high content of CaCO3, regarding to the total
limestone content of the sludge, which is likely due to the lime-
stone filler and cement being the main CaCO3 inputs. On average,
the total limestone content of the sludge is around 11.2%. This
mass percentage in the mixture can be explained by considering
the limestone coming from a usual concrete formulation (reference
concrete, Table 6) produced in the ready-mixed concrete plant.
Indeed, considering no gravels in the sludge, a 12.6% content of cal-
cite in the dry sludge (coming from the cement, the limestone fil-
lers and the sand) was expected, which is closed to the content
Fig. 4. DLS particle-size distribution of the 100 lm passing of the dry sludge and comparison with a limestone filler (left: non-cumulative passing; right: cumulative passing).
determined by TGA. Regarding to the total portlandite content,
fractions A present lower contents, which can be explained by
the conglomeration of portlandite, which forms particles coarser
than 100 lm.
Global chemical compositions of the sludge are given in
Table 10. Weak variability is observed between the four sludge
(standard deviation below 20%). Those results can be explained
by the homogeneity of the concrete produced in the four studies
ready-mixed concrete plants. Indeed, they mainly produced the
same concrete (formulation in Table 6). Those compositions are
consistent with literature data on sludge chemical composition
[4,5,6,7].
3.1.3. Reactivity
As can be seen in the Table 11 and the Fig. 7, the substitution of
25% of the cement by a mineral addition causes a decrease of the
mechanical strength of the standard mortar. Indeed, a compressive
strength of 37.52 MPa was obtained on the reference mortar, the
compressive strength of mortars with mineral addition were
included between 29.20 and 34.73 MPa. However, the French stan-
dard [17] stipulates that the activity index of a limestone fillers
must be higher than 71%. The activity index of the used filler is
around 92%, which is in compliance to the standard. The activity
index of the C1, C3 and the C4 sludge (fractions A) are slightly
lower than the one of the limestone filler. Nevertheless, they
remains higher than the required 71%. The activity index of the
C2-sludge (fraction A) reaches a value of 94%, which is even slightly
higher than the value obtained with the limestone fillers. Overall,
few dispersion is observed when comparing the activity index of
the finer fraction of the sludge, which can be explained by a very
close mineralogical and chemical composition. The differences
may be attributed to a variation in the particle-size distributions,
so to a variation in the packing densities.
In order to get more accurate results on the chemical activity of
the sludge, conductimetric tests were performed on blends
between cement and the fraction A of the sludge. The composition
of the blends is given in the experimental section.
The results highlighted a classical behavior of cementitious
materials [18]. During the first minutes, an exponential rising of
the conductivity is observed, due to the high dissolution rate of
the compounds of the clinker and gypsum. This period is known
as the mixing period (I). Then, the dormant period (II) begins.
The C–S–H and ettringite precipitation begins, while the conduc-
tivity remains rising. Gradually, the solution becomes richer in
Ca2+ and HO ions, up to the point where the critical concentra-
tions are reached and the portlandite precipitation begins. At that
 M. Audo et al. / Construction and Building Materials 112 (2016) 790–799 795

Table 9
Density, specific surface and CaCO3 and Ca(OH)2 contents of the fraction A and B – Fractions A and B mass content in sludge.

LF C1 (A) C1 (B) C2 (A) C2 (B) C3 (A) C3 (B) C4 (A) C4 (B)

3
Density (g/cm ) 2.7 2.2 2.2 2.2 2.2 2.1 2.3 2.2 2.3
Specific surface (m2/kg) 350 1100 – 1300 – 1800 – 1350 –
Ca(OH)2 content (%) – 8.8 10.8 7.5 13.9 6.0 10.8 4.6 14.7
CaCO3 content (%) 98.0 17.5 13.0 18.7 23.5 22.2 13.4 19.6 9.0
C1 C2 C3 C4
Fraction A (%) 20.9 40.0 26.9 38.6
Fraction B (%) 79.1 60.0 73.1 61.4

point, the conductivity starts to decrease: this is the acceleration
period (III). The curve obtained on the CEM II/A cement is shown
on Fig. 8 for example.
The limestone filler, as well as fractions A of the dry sludge, does
not show any hydraulic behavior. Indeed, when placed in an aque-
ous media, the conductivity increases during the first seconds and
then remains stable until the end of the experiment (Table 12). But
a large difference in the chemical behavior of the sludge and the fil-
lers can be observed, as the maximal conductivity is at least ten
times higher when sludge are used over fillers. Nevertheless, when
mixed with cement, all studied materials modify the hydration
kinetic of the cement. Especially, when the limestone filler delays
the portlandite precipitation (30 min for a reference time of
210 min), the fraction A of the sludge speed up the portlandite pre-
cipitation (between 10 and 60 min). Those time gaps were higher
to the accuracy of the method (estimated to be 4 min). Ten, those
results highlight a chemical activity of the sludge within the
cementitious matrix, which is likely due to a high dissolution rate
in water. Indeed, the higher is the maximum conductivity in pres-
ence of sludge, the quicker is the cement hydration. In concrete,
limestone fillers are known to speed up the hydration kinetics
[25]. This effect cannot be observed here, as the dilute medium
does not allow to highlight the physical behavior of filler additions.
3.2. Mortars made with sludge
3.2.1. Mortars composition
In Figs. 9 and 10 are presented the volume proportions of the
reference concrete, the reference CEM, and the dry sludge-CEM
and wet sludge-CEM. It can be noted that, depending on the
particle-size distribution of the sludge, between 4.5 and 11% of
the sand of the CEM mortar can be substituted by the sand brought
by the sludge. Moreover, the mass of dry sludge with particle size
lower than 100 lm in the sludge-based mortar is almost equal to

Fig. 5. XRD patterns of the fractions A and B of the C1- (up, left), C2-sludge (up, right), C3-sludge (down, left) and C4-sludge (down, right) (C: Calcite; CC: Hydrated calcium
carbonates; CS: Calcium silicates; CSH: Hydrated calcium silicates; G: Gypsum; P: Portlandite; Q: Quartz).
796 M. Audo et al. / Construction and Building Materials 112 (2016) 790–799

Fig. 6. Typical DTG curve (example on the fraction A of the C3 sludge).

Fig. 8. Conductimetric curve obtained with the CEM II/A cement.

Table 10
Chemical composition of sludge (%). Table 12
Conductimetric characterizations of the CEM II cement mixed with different mineral
Al2O3 Fe2O3 CaO SiO2 SO3
additions.
C1 1.70 1.45 31.79 57.04 0.59
C2 2.09 1.72 37.32 50.04 0.98
rmax (lS/cm) Slope reversal time (min)
C3 1.65 1.42 32.83 54.85 0.81 Cement 19.8 210
C4 1.97 1.62 34.85 53.50 0.71 Limestone filler 0.1 –
C1 dry sludge 5.5 –
C2 dry sludge 6.5 –
C3 dry sludge 1.7 –
Table 11
C4 dry sludge 1.1 –
Compressive strength of the standard mortars.
Cement + limestone filler 18.3 242
Reference Limestone filler C1 C2 C3 C4 Cement + C1 dry sludge 17.7 180
fc(28) (MPa) 37.52 34.73 33.38 35.13 29.20 30.21 Cement + C2 dry sludge 18.2 148
Cement + C3 dry sludge 18.1 188
Cement + C4 dry sludge 18.1 200

Fig. 7. Comparison of the activity of the limestone fillers and the fraction A of the Fig. 9. Volume proportions of the reference concrete, the CEM mortar and the C1-,
sludge. C2-, C3- and C4-CEM mortars made with dry sludge.

the mass of limestone filler in the CEM mortar. Also, using wet
sludge allows to substitute tap water, from 37% (C4-CEM) to 56%
(C3-CEM).
The particle-size distribution of the CEM mortar is presented in
Fig. 11(a). In Fig. 11(b) the relative differences between the
particle-size distribution of the CEM mortar and the ones of the
sludge-made mortars are presented. Those differences are calcu-
lated by:
Relative difference ¼ 100
CEM cum:passing  sludge made CEM cum:passing

CEM cum:passing
The largest differences between the particle-size distributions
of the CEM-mortar and the sludge-made mortars occur between
0 and 10 lm, but are negligible above 10 lm.
3.2.2. Slump
The measurement of the slump with the Abrams mini-cone
highlighted a special behavior of the sludge over the limestone fil-
lers. Indeed, when limestone fillers were used for mortar fabrica-
tion, a slump of 2 cm was measured. When the wet sludge was
used as limestone fillers substitute, a 0 cm slump was observed.
This difference could be explained by a water retention behavior.
Either the water of the sludge can be trapped into the porosity of
 M. Audo et al. / Construction and Building Materials 112 (2016) 790–799
Fig. 10. Volume proportions of the reference concrete, the CEM mortar and the C1-,
C2-, C3- and C4-CEM mortars made with wet sludge.
Fig. 11. Particle-size distribution of (a) the CEM mortar and (b) the relative
difference between the particle-size distribution of this mortar with the ones of the
sludge-made mortars.
the fraction A of the sludge, or the water can be adsorbed on the
surface of the particles. This difference can also be explained by a
modification of the packing density of the mortar. Thus, some
superplasticizer was needed to adjust the rheology when sludge
was used. The same slump class (S3) as the reference concrete in
ready-mixed concrete plants was targeted for all mortars. While
only 0.2% (based on cement weight) of superplasticizer was needed
for the reference mortar, a high percentage (from 0.5% to 1%) was
need when dry sludge was used. Unfortunately, those percentages
are hardly compatible with an industrial application.
797
3.2.3. Calorimetric characterization
On Fig. 12. are shown typical curve obtained by calorimetric
characterizations. Results obtained on several mortars are depicted
in Table 13. The incorporation of mineral additions allows to speed
up the hydration kinetics, which can be explained by the creation
of new nucleation sites for the hydrates precipitation [25] This
influence is very variable depending on the kind of addition. While
limestone filler, C2- and C4-sludge show only few influence on the
hydration kinetics, the influence of C1- and C3-sludge is more dis-
tinct. Variations in anhydrous cement content in sludge could
explain this phenomena. Also, it can be observed that the heat
released is higher when sludge are used (from 29.2 to 38.0 J/g of
cement). This could be due to the higher exothermic ions dissolu-
tion observed by conductimetric measurements, to the presence of
anhydrous cement or also to a filler effect as described previously
in the literature [25].
3.2.4. Harden state
3.2.4.1. Dry sludge. After 7 and 28 days of curing in water, the com-
pressive strengths of the mortars were measured. The Fig. 13
allows to compare the compressive strengths between the CEM
and the dry sludge-made mortars. All mortars present the same
hardening kinetic, but different compressive strength. At 7-days
old, the C1-, C2- and C3-sludge made mortars present a lower com-
pressive strength compared to the reference CEM (-28%, -21% and -
11% respectively). The C4-sludge made mortar is the only one
which present a higher compressive strength (+32%).
After 28 days, the same tendency is observed: the compressive
strength of the C4-CEM remains the highest one, and the only one
higher than the reference mortar.
Considering the activity index (Fig. 7), the highest compressive
strength was expected for the C2-CEM, while the lowest one was
expected on the C3-CEM. But no relationship between the com-
pressive strength and the activity index was observed, calling for
new explanatory factors.
The difference between the CEM and the sludge-made CEM
compressive strength could be attributed to a higher porosity in
the sludge-made mortars. It is well known that the higher the con-
crete porosity is, the lower the compressive strength is [26]. Nev-
ertheless, few differences are observed when comparing the CEM
porosity with the one of the sludge-made CEM (Table 14).
As neither the porosity nor the activity index seem to explain
the variability of the compressive strengths, the influence of per-
centage of fraction A in sludge and in mortars was studied. Calcu-
lations were performed with the Statgraphics Centurion software
with the input data shown in Table 15, and the results of the mul-
tiple linear regressions are detailed in Table 16. Two variables were
studied: wA/wS refers to the percentage of fraction A in sludge
while wA/wM refers to the percentage of fraction A in mortars.
Their influence on the 28-days compressive strength was deter-
mined through the p-value. A p-value lower than the defined sig-
nificance level means that the variables have a significant
influence on the measured parameter. On the contrary, a p-value
higher than the defined significance level means that there is no
significant influence of the variables on the measured parameter.
As the p-values in Table 13 for the two studied variables are
both below 0.05 (significance level of 95%), a significant relation-
ship exists between wA/wS and wA/wM and the compressive
strength. This relationship was then defined as:
wA wA
rðMPaÞ ¼ 57:6487 þ 0:1844  20:3565
2S wM
The validity of the model is proven by a p-value lower than 0.05.
Moreover, the R2 coefficient correlation is very closed to 100%,
which means that the whole experimental variability can be
explained by the variables wA/wS and wA/wM. Given the model
798 M. Audo et al. / Construction and Building Materials 112 (2016) 790–799

Fig. 12. Comparison of the released hydration heats of CEM and CEM’ mortars (left: cumulative; right: non-cumulative).

Table 13
Calorimetric characterizations of the mortars made with limestone and dry sludge.

CEM mortar C1-CEM C2-CEM C3-CEM C4-CEM

DQcum (J/g of cement) +12.8 +38.0 +35.1 +36.0 +29.2
Dt (min) 15 125 15 105 15

Table 16
Multiple linear regression.

Coefficient p-value
Constant 57.6387 0.0028
wA/wS 0.184367 0.0121
wA/wM 20.3565 0.0037

R2 = 99.99%.

Table 17
Compressive strengths of the mortars made with wet sludge.

CEM C1-CEM C2-CEM C3-CEM C4-CEM

7 days 23.1 (±0.8) 18.7 (±2.0) 19.4 (±2.4) 20.7 (±0.4) –
28 days 30.6 (±1.6) 19.6 (±3.5) 26.3 (±2.3) 22.8 (±0.8) –

Fig. 13. Compressive strengths of the mortars made with dry sludge.
Table 14
Relationship between compressive strength and porosity.
the compressive strength. Said differently, the compressive
strength decreases when the substitution rate of the sand fraction
increases.

CEM C1- C2- C3- C4- 3.2.4.2. Comparison between wet sludge and dry sludge. In order to
CEM CEM CEM CEM industrialize the recycling of sludge into concrete in ready-mixed
7-days compressive 23.1 16.6 18.3 20.5 30.5 concrete plants, sludge must be used at their wet state. Conse-
strength (MPa) (±0.8) (±0.5) (±0.6) (±2.0) (±1.9) quently, mortars were also made with wet sludge in order to high-
28-days compressive 30.6 21.1 23.4 28.8 35.7
light any influence of the drying process on rheological and
strength (MPa) (±1.6) (±2.7) (±3.2) (±3.7) (±1.2)
28-days porosity (%) 23.5 23.7 22.8 24.1 23.0 mechanical resistance. Firstly, wet sludge impacted significantly
the fresh state rheological properties of the mortars, as less super-
plasticizer needed to be added to obtain the same slump. Secondly,
Table 15 the compressive strength obtained on those mortars (C1-, C2- and
Model input data. C3-CEM) are given in Table 17. Given the experimental uncertain-
C1 C2 C3 C4 ties, equivalent compressive strengths were measured on mortars
made with dry or wet sludge. Those results validate the dry-sludge
wA/wS 0.236 0.416 0.241 0.407
wA/wM 0.0020 0.0021 0.0016 0.0014 approach in laboratory for the prediction of wet-sludge industrial
Compressive strength (MPa) 21.15 23.43 28.76 35.70 approach.

equation, the most influent parameter on the compressive strength 4. Conclusions and prospects
is the fraction A content in the mortars. The more fraction A in the
mortars, the lower the compressive strength. On the other side, for The work presented herein has focused on the effect of the
one given wA/wM ratio, the higher is the wA/wS ratio, the higher is incorporation of sludge coming from ready-mixed concrete plants
 M. Audo et al. / Construction and Building Materials 112 (2016) 790–799
into mortars. As the sludge heavy metals and metalloid elements
contents are close to the criteria of acceptance of inert wastes at
landfills, it seems appropriate to propose a new valorization way:
the incorporation in concrete as mineral addition.
Firstly, the use of this kind of sludge as limestone fillers substi-
tutes alters the rheology of the fresh state mortar. It becomes less
plastic and some superplasticizer must be added in order to obtain
the same class of slump as the reference mortar. The superplasti-
cizers added quantities remain acceptable for the industrial. Even
though, several options could be applied in order to limit this phe-
nomenon, including the use of binary mixes between sludge and
limestone fillers.
Then, the 28-days compressive strengths are between 30%
lower to 17% higher when the dry sludge are used instead of lime-
stone fillers. This variation may be attributed two main factors:
- the fraction A content in the mortars;
- the substitution rate of the sand fraction of the mortars.
Nevertheless, sludge coming from others ready-mixed concrete
plants must be studied in order to confirm those results.
Acknowledgments
The authors would like to acknowledge the French Agency for
Environment and Energy Management for the financial support,
as well as all the industrial partners of the project and the trainees
of the project.
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