Applied Clay Science 53 (2011) 561565

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Applied Clay Science

j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / c l a y

Research Paper

The effect of incorporation of a Brazilian water treatment plant sludge on the

properties of ceramic materials
S.R. Teixeira , G.T.A. Santos, A.E. Souza, P. Alessio, S.A. Souza, N.R. Souza
Department of Physics Chemistry and Biology, Univ. Estadual Paulista, UNESP, Rua Roberto Simonsen, 305, P.O. Box 266, 19060-080, Presidente Prudente, SP, Brazil

a r t i c l e

i n f o

Article history:
Received 14 September 2010
Received in revised form 2 May 2011
Accepted 4 May 2011
Available online 8 June 2011
Keywords:
Water treatment sludge
Clay
Texture
Red ceramic
Physical properties

a b s t r a c t
We evaluated the feasibility of incorporating sludge from decantation ponds of a water treatment plant (WTP)
into a ceramic body used in ceramic brick manufacturing. The sludge grain-size distribution (silt, sand and
clay) and the effects of its incorporation on the properties of the ceramic body were studied. Samples were
collected during a period of ten months. The chemical and mineralogical compositions of the WTP sludge
varied according to the month of sludge production, but the compositions are similar to those of the natural
raw material used by the red ceramic industry. Technological tests of ceramic probes showed that this residue
can be incorporated into clays used to produce ceramic bricks. The concentration of sludge to be incorporated
depends on its properties (grain-size distribution and chemical and mineral composition), but mainly on the
properties of the raw material (matrix) used.
2011 Elsevier B.V. All rights reserved.

1. Introduction
Conventional water treatment plants (WTPs) transform crude
water into potable water utilizing a series of processes: coagulation,
occulation, decantation and ltration. The process of coagulation
involves the use of Fe or Al salts that form occules with impurities in
water, which sediment (or oat) and are later ltered out. This
treatment produces a solid residue (alum or ferric sludge) with a high
water content, whose composition depends on the origin of the crude
water collected (surface water or groundwater through wells), the
type of soil of the region, the material discharged into the river,
chemical products present, the process of treatment employed, etc.
The main components of the sludge from WTPs are (sometimes
known as water treatment residues): clay minerals, very ne-grained
minerals (mainly oxides and hydroxides of aluminum and iron),
organic matter and contaminants from the discharge of urban and
industrial efuents and other human activities.
In general, this sludge is dumped directly into rivers and streams
or into the drain system, causing a signicant environmental impact,
which compromises the quality of drinking water and the health of
the public and animals that utilize it. The growing concern of
environmental organizations, due to the risks to health and to the
environment, has led to the restriction or prohibition of discharging
this residue into the environment (streams, landlls, soil, etc.).
Currently, there are more than 7500 complete cycle (or conventional)
WTPs in Brazil, and even though there is legislation prohibiting it, the

Corresponding author. Tel.: + 55 18 322953 55; fax: + 55 18 3221 5682.

E-mail address: rainho@fct.unesp.br (S.R. Teixeira).
0169-1317/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.clay.2011.05.004

amount of sludge released into waterways is still substantial

(Monteiro et al., 2008). A comprehensive study about biosolids was
published by Andreoli (2006) where he presented the state of the art
in alternatives for recycling of sanitation waste in the manufacture of
red ceramics.
The sludge generated in WTPs is a solid residue that should be
properly treated and disposed without causing harm to the environment. One of the techniques used to prepare sludge for disposal is
dehydration, resulting in a cake with a concentration of solids of 60 to
70%. This cake can be used as fertilizer, incinerated, disposed in landlls
for urban waste, and composted with urban waste, among other
alternatives. More recently, the alternatives in which the residue is
utilized or transformed into products that are useful to society
have been studied. An important one of them is the utilization of
residues in making cement and ceramic bodies. Its incorporation
into ceramic bodies for the production of bricks and roof tiles is a
viable practice, and could be of interest to ceramic manufacturers
(Andreoli, 2006; El-Mahllawy and El-Sokkary, 2008; Huang et al., 2001,
2005; Jordan et al., 2005; Kayaci et al., 2010; Li et al., 2005, 2006;
Menezes et al., 2002; Monteiro et al., 2008; Oliveira et al., 2006; Teixeira,
2006; Teixeira et al., 2002, 2006; Ueno and Leite, 2007; Vieira et al.,
2008; Weng et al., 2003; Zou et al., 2009).
The recycling of residues can reduce environmental impacts,
increase the useful life of the mineral raw materials used, and lower
nal production costs. The ceramic industry is a very important sector
in Brazil and is widespread. Brazilian consumption of clay has
surpassed 150 million tons/year since 2005 (MME, 2009). Sludge
from WTPs, mainly from the treatment of surface water, can be
incorporated into ceramic bodies; sludge contains minerals that are
common in clays, and therefore, its composition facilitates the clay/

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sludge mixture (Monteiro et al., 2008). One of the main contaminants

of sludge is associated with the type of occulants used for its
precipitation. In previous work, we observed that the sludge obtained
with aluminum-based chemical is more deleterious to ceramic
properties than those obtained with iron compounds (Teixeira et al.,
2002, 2006).
This paper presents the results of a study conducted over ten
months with the aim of evaluating the variation of grain-size
distribution (texture) in sludge from water treatment. Also, we
assessed the technological properties of ceramic bricks obtained with
the addition of sludge to clayey material used by ceramic industry.

2. Materials and methods

From 2001 to 2004, samples were collected on the washing dates
of the rst decanter of the WTP of the state sanitation company
SABESP (Companhia de Saneamento Bsico do Estado de So Paulo) in
Presidente Prudente County, located 558 km west of So Paulo, the
capital city of the state of So Paulo. This company uses the
conventional coagulationocculationsedimentation pretreatments
in its water purication system. During this period, three different
coagulants were utilized (aluminum sulfate, ferric chloride and
aluminum polychloride), and samples were collected monthly over
ten months. The aluminum polychloride coagulant was adopted by
SABESP due to its higher efciency in the coagulation of solid particles
in treated water. Therefore, the sludge incorporated in the ceramic
material for technological tests was obtained with this chemical and
called sludge-Al. The tank was divided into six parts, and two liters of
sludge were obtained from each one, totaling twelve liters per
sampling. The samples were mixed and dried in an oven at 110 C,
broken up and pulverized in a blade mill, and the resultant material
was then passed through a # 40 sieve (0.42 mm).
Concentrations of organic matter (OM) were determined by the
WalkleyBlack method (EMBRAPA, 1998) and the concentrations of
the sand, silt and clay fractions by the pipette method, in the samples
of sludge and clay, with prior oxidation of the organic matter using
hydrogen peroxide (Dixon and White, 1996; Klute, 1986). The main
minerals in the clay were determined in a previous study (Teixeira et
al., 2001). The sludge minerals were identied using a D/MAX-2100/
PC, Rigaku X-ray diffractometer (copper radiation, Ni lter and 0.02
step). These samples were K or Mg saturated and oriented (spread) on
glass plates (Dixon and White, 1996; Moore and Reynolds, 1997).
Chemical analysis of a sample of sludge, to test for the presence of
heavy metals, was carried out in a laboratory certied for chemical
analysis using atomic absorption spectrophotometry (AAS), in
accordance with established standards. A thermogravimetric system
(TG-209, NETZSCH Instruments) and a differential scanning calorimetry
apparatus (DSC 291A, TA Instruments) were used to characterize the
samples, at 10 C/min in air (50 ml/min).
Ceramic probes (CPs) were pressed uniaxially (19 MPa, 60
20 ~5 mm 3) in triplicate, using clay from the oodplains of the
Paran River (on the Bauru Sandstone), which is also used to produce
bricks by the ceramic industry located in the Presidente Prudente
region, So Paulo state, Brazil. This raw material has 57 wt.% clay,
37 wt.% silt, 6 wt.% sand, a high plasticity limit (40.6%) and low
concentration of organic matter (5.57 wt.%) (Teixeira et al., 2001). The
sludge concentration added to the clay ranged from 0 to 30 wt.%. After
ring in a laboratory kiln at ve temperatures varying from 850 to
1200 C, the CPs were submitted to technological tests according to
Brazilian norms for the evaluation of ceramic properties. Water
absorption (WA), apparent porosity (AP) and apparent specic mass
(ASM) were determined using an analytical balance and the
Archimedes method. Linear shrinkage was determined by measuring
the length of the samples before and after ring using a caliper. The
exural rupture strength (FS) was determined by the three-point

bending test using a universal machine (EMIC, model DL 2000)

(Santos, 1989; Teixeira, 2006).
3. Results and discussion
3.1. Grain-size distribution
Texture analysis showed that the fractions of clay, silt and sand of
the sludge varied monthly. The percentages of these fractions differ
according to the time of the year in which the sludge was produced.
Fig. 1 shows the variation of the fractions and of organic matter, in the
ten sampling months and, the variation of the water level measured
using a xed ruler in the river where water was drawn for the WTP.
The changes in river levels were associated with the amount of rainfall
in the region. The concentration of organic matter showed no
apparent variation. On the other hand, sand showed a tendency to
vary inversely with the level of the river, while clay decreased at the
lowest river level. During the sampling period (10 months), clay
concentration varied from 30 to 60 wt.%. As shown by the lowest river
levels (Fig. 1), the months of June to September had the lowest rainfall
in the region, which is normal at this time (winter) in the southern
hemisphere.
The ideal grain-size distribution for each type of product for the
red ceramic industry is represented in the classical Winkler diagram
(Monteiro and Vieira, 2004). It consists of a triaxial scheme where
each axis represents the sand, silt and clay fractions and, it can be
organized in regions in which each component may have a variable
composition as shown in Table 1. According to these ranges, the
sludge had a concentration of clay that gave it an ideal plasticity for
making roof tiles and ridge caps. It was also evident that the
concentrations of clay greater than 40% conferred high plasticity to
the ceramic body, causing problems in the drying and ring of ceramic
pieces. In some cases, the concentration of sand (non-plastic material)
was also very high, which can worsen the properties of the ceramic
material. Therefore, the sludge to be used for mixing with the ceramic
raw material should have concentrations of clay and non-plastic
materials compatible with those ranges shown in the Winkler
diagram. As the raw material used in this paper has high plasticity,
we used the sludge with the highest concentration of sand.
3.2. X-ray diffraction and chemical analysis
X-ray diffraction analysis (Fig. 2) of the clay material and of
oriented clay plates showed kaolinite (0.723 and 0.359 nm) as the
predominant clay mineral, along with the presence of mica (1.068 and

Fig. 1. Variation of the grain-size fractions and of organic matter in the sampling
months and, the variation of the river water level at the point of water collection.

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563

Table 1
Ideal grain-size distribution for ceramic masses according to the Winkler diagram
(Monteiro and Vieira, 2004).
Type

Clay 2 m

Silt 220 m

Sand 20 m

I. Plasticity very high

(difcult workability)
II. Roof tiles and ridge caps
III. Perforated bricks
IV. Heavy bricks

40 to 50

20 to 40

20 to 30

30 to 40
20 to 30
15 to 20

20 to 50
20 to 55
20 to 55

20 to 40
20 to 50
25 to 55

0.500 nm), goethite (0.415 nm) and quartz (0.333 nm). This clay also
contained, at lower concentrations, other iron oxides, titanium oxides,
gibbsite and other 2:1 type minerals such as smectites (Dixon and
White, 1996; Moore and Reynolds, 1997). The ceramics factories of
the region use oodplain clays which have a similar mineralogical
composition, as observed in a previous work (Teixeira et al., 2001).
Considering the major minerals and texture of the sludge used, we
observed that this material has a composition similar to that
characteristic of non-plastic material (high concentration of sand
and silt) used to mix with raw material (predominantly kaolinitic
clays) with high plasticity (high concentration of clay minerals). The
sludge collected during the rainy season (October to May) has a
particle size distribution (high plastic clay concentration and low
concentration of non-plastic material) close to that observed for
kaolinitic clays used in brick production (Monteiro et al., 2008;
Teixeira et al., 2001). Fig. 3 shows the diffractogram of the oriented
clay slide of the sludge sample, collected in the month of August,
obtained using aluminum polychloride as coagulant. Here, the main
clay minerals noted above can be identied.
Chemical analysis (X-ray uorescence XRF) of a sample of
sludge showed that iron, silicon, aluminum and titanium were the
main components of the sample, with a small concentration of
calcium. Quantitative analysis by atomic absorption spectrophotometry (AAS) showed that the concentrations of the heavy metals
Pb (0.42 ppm), Cr (4.60), Zn (31), Mn (121), Al (0.43) and Cu (15)
were below the limits recommended for agricultural recycling of
sewage sludge (Mota, 2003). This result was expected since this is
a farming region with little industry. The concentration of Fe
(130,800 ppm) was high due to the coagulant used, which has an
iron base. The presence of heavy metals in the sludge does not
prohibit its incorporation into ceramic materials, considering that
these metals can be incorporated and made inert in the crystalline
structure of vitreous phases formed during the sintering process of
ceramics.

Fig. 2. X-ray diffraction pattern of clay material used by ceramic industry (Enclosed
XRDP of saturated (K and Na) and oriented clay slides).

Fig. 3. X-ray diffraction pattern of oriented clay minerals in the WTP sludge.

3.3. Thermal analysis

Fig. 4 shows the thermograms (TG/DTG) for two samples of sludge
with iron and one with aluminum, collected in different periods. The
thermogravimetric analysis data showed that there was a loss of
moisture of approximately 9% (near 65 C), loss of water due to
decomposition of hydroxides (aluminum and iron) and burning of
organic matter on the order of 7% (close to 265 and 315 C), and loss of
structural water from kaolinite of 7% (around 500 C) (Monteiro et al.,
2008; Teixeira et al., 2008).
Fig. 5 shows the data for differential scanning calorimetry (DSC) of
WTP sludge with two different coagulants used (Fe and Al), clay used
for the production of bricks, and kaolin from Georgia (USA).
Comparing the diagrams, it can be seen that all three samples showed
kaolinite as the main clay mineral. Besides the loss of free water
(~70 C), there was an exothermic band (200450 C) that was
greater in the samples with WTP sludge, characteristic of organic
matter oxidation and also to the crystallization of amorphous phases
of iron and aluminum (gels) (Gastuche et al., 1964), formed during
the chemical treatment of the water to precipitate the sludge. The
narrow peak observed at 573 C is characteristic of the phase
transition of quartz, present in the clay sample. The book edited by
Dixon and Weed discusses the possible transformations of iron
(Schwertmann and Taylor, 1989) and aluminum (Hsu, 1989)
hydroxides into oxides and polymorphic transformations of silica.

Fig. 4. Thermogravimetric data TG and DTG (Derivative TG curve) of WTP sludge (using
iron chloride and aluminum sulfate).

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Fig. 5. Differential scanning calorimetry (DSC) data of clay material, kaolin and sludge
using different coagulants.

Fig. 7. Three-point exural strength (FS) for ceramic probes with (0, 10, 15 and 20 wt.%)
incorporated sludge.

3.4. Technological tests

The results with sludge obtained using the coagulant aluminum
sulfate (sludge-Al) were always poorer than those with ferric chloride
(sludge-Fe) as observed in a previous work. In general, the aluminum
increased the refractivity and the friability of ceramic material, while
the iron improved the properties of material resulting from the
reaction with mica in the formation of a glassy phase (Teixeira et al.,
2006).
In general, the results of the technological tests showed that the
incorporation of sludge from WTP consistently worsened the
technological properties of the ceramic materials, as also observed
in other studies (Jordan et al., 2005; Monteiro et al., 2008; Teixeira
et al., 2006; Weng et al., 2003). However, research results show that it
is possible to produce materials within the limits specied by the
regulations of each country, controlling the amount of sludge to be
added to the ceramic material and the sintering temperature.
Figs. 6 to 8 show the results of technological tests for clay with
sludge-Al (10, 15 and 20%) collected in the month of August, which
had a greater concentration of sand. In general, the variation in the
properties of the samples was approximately equal for the additions
of 15 and 20% sludge. The graphs show that the incorporation of
sludge increased water absorption and decreased apparent specic
mass (Fig. 6) and exural strength (Fig. 7). These effects are mainly

due to the high concentration (29%) of organic matter in sludge,

which increases the porosity of the sample during ring.
The behavior of the properties (WA, ASM, LS) of ceramic bodies
with sludge were similar to those of pure clay material (Teixeira et al.,
2004), showing that it determines the nal properties of the material.
All the properties of clay with sludge showed little variation below
1000 C. At this temperature up to 1100 C, the variation was abrupt,
and then for the greater concentrations of sludge the properties
tended to stabilize. This effect, of the improvement of ceramic
properties with increase in temperature, was already expected since
a liquid phase occurs above 1000 C, with greater densication of the
ceramic probe. However, the slowdown of the reaction between 1100
and 1150 C was not expected, indicating that with sludge the
densication reactions occurred at temperatures lower than those for
pure clay, and crystallization of new phases could have occurred with
the production of microssures. The highest concentration of quartz
due to the sludge may contribute to an increase in porosity and
microcracks generated by its alpha-beta transition (573 C) during
cooling of the ceramic bodies. These microssures tend to increase
water absorption and decrease apparent specic mass and mechanical
resistance.
Linear ring shrinkage (Fig. 8) changed little at low temperatures
(up to 900 C) due to the high concentration of sand (non-plastic
material) in sludge. Above this temperature there was a substantial

Fig. 6. Water absorption (WA) and apparent specic mass (ASM) of ceramic probes
with (0, 10, 15 and 20 wt.%) incorporated sludge.

Fig. 8. Linear ring shrinkage of ceramic probes with (0, 10, 15 and 20 wt.%)
incorporated sludge.

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increase in linear shrinkage due to the formation of a liquid phase, up to

1100 C. At this temperature range, LS was more evident for CPs with
added sludge due the presence of uxing material (mica and goethite)
in sludge (Fig. 3). Again, there was a change in behavior at 1150 C for
samples with a greater (15 and 20%) concentration of sludge.
Despite the fact that the addition of sludge worsened the
technological parameters, some of these values were still in
accordance with the Brazilian standards established for ceramics:
exural strength (bricks N 2.0 MPa, perforated bricks N 5.5 MPa, roof
tiles N 6.5 MPa), water absorption (perforated bricks b 25%, roof
tiles b 18%), linear ring shrinkage (bricks b 6%), and apparent specic
mass (N1.6 g/cm 3) (Santos, 1989; Teixeira, 2006). These limits are
approximately equal to the values established by the Chinese National
Standards (CNS) (Weng et al., 2003).
4. Conclusions
Particle size analysis showed that the amounts of sand, silt and clay
varied depending on the time of year that the sludge was produced.
The sludge shows characteristics of a plastic material due to the high
concentration (N30%) of clay minerals and organic matter. In general,
ceramic industries mix two or more clays with different grain-size
compositions to obtain the ceramic body appropriate for each
product. Thus, sludge can be one of the components of the mixture.
The quantity of sludge that can be incorporated will be determined by
the ring temperature, the properties of the sludge and mainly by the
raw material properties used as the matrix.
Considering the Brazilian technical standards, we can conclude
that: (a) the addition of 10% sludge allows the manufacture of solid
bricks for ring temperatures lower than 1000 C; (b) above this
temperature, up to 20% sludge can be incorporated into the raw
material for the production of bricks and also roof tiles.
Acknowledgements
The authors thank SABESP of Presidente Prudente for their
collaboration, FAPESP for fellowships and grant support (PROC.
2008/04368-4), and the CNPq/PIBIC program for the Student Scientic
Initiation grants. Dr. A. Leyva helped with the English editing of the
manuscript.
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