Journal of Cleaner Production 345 (2022) 131055

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Journal of Cleaner Production

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

Physical, mechanical properties and durability of cement mortars

containing fly ash from the sewage sludge incineration process
Tomasz Zdeb *, Tomasz Tracz , Marcin Adamczyk
Faculty of Civil Engineering of the Cracow University of Technology, ul. Warszawska 24, 31-155, Kraków, Poland

A R T I C L E I N F O A B S T R A C T

Handling Editor: Zhen Leng Pursuant to European Union regulations, waste generated during municipal sewage treatment should be
managed in an environmentally friendly manner. In order to eliminate the risk to human health and to the
Keywords: environment, and also to minimise the volume of the resulting sludge, it is subjected to thermal treatment. The
Sewage sludge ash resulting ash contains heavy metals, and thus proper management is required. Since it is known that products of
Cement
cement hydration reactions have a potential ability to immobilise heavy metals, a preliminary verification was
Mortars
conducted of the possibility of disposing of this type of waste by including it in cement composites. For this
Mechanical properties
Durability purpose, suitable tests were carried out on the mechanical properties and durability of cement binders containing
Heavy metals leaching ash from the incineration of sludge produced from municipal sewage (Sewage Sludge Ash – SSA). The tests were
conducted for a standard mortar composition based on Portland cement CEM I and on ash obtained on a tech­
nical scale in a sewage treatment plant at a temperature of about 850 ◦ C. This mineral addition was used to
replace 10%, 20%, 30% and 40% of the cement by weight. The physical and mechanical characteristics were
measured, such as compressive and flexural tensile strength after 14, 28 and 90 days of curing as well as
durability characteristics such as total porosity, the ability to transport chloride ions and resistance to sulphate
ions. The results obtained confirm that replacing 10% of the cement with this admixture has a beneficial effect on
the mechanical and durability characteristics, but greater amounts are reflected in a clear deterioration of these
characteristics.

1. Introduction
The treatment of industrial and municipal sewage involves a prob­
lem with certain types of waste which are produced during this tech­
nological process; this waste, which has the form of sewage sludge (SS),
requires appropriate management due to its properties. This sludge in­
cludes sludge from digester tanks and other parts of the sewage treat­
ment installation. The amount of sludge generated is only 1–3% of the
volume of sewage flowing through the treatment plant; however, given
the increasing urbanisation, the amount of waste being produced is
becoming a serious problem. Among other things, this waste contains
heavy metals and pathogenic organisms which can have a very negative
impact on the natural environment and human health. Therefore, its
proper management and disposal is very important. In order to protect
the environment and human health, and also to minimise the volume of
the resulting sludge, it is subject to thermal treatment. While the ash
produced as a result of incinerating sewage (SSA) does not contain live
pathogenic organisms, the heavy metals present in its composition
remain a problem. On the other hand, this sludge can also have practical
uses before thermal treatment as it contains organic substances and
biogenic elements. The sludge is used for agricultural purposes (as a
fertiliser), since it is a major source of nitrogen and phosphorus. Ac­
cording to the Polish Central Statistical Office, over 130,000 tonnes of
sludge were used in agriculture in 2018. Since 2010, an increase has
been seen in the amount of sewage sludge produced. In 2018, more than
one million tonnes of sludge (in dry matter terms) were produced in
Polish industrial and municipal sewage treatment plants. Moreover,
there has also been a noticeable increase in the amount of thermally
treated sludge, which is in line with the guidelines for sewage sludge
treatment set out in the National Waste Management Plan and in the
National Municipal Sewage Treatment Programme. In 2018, according
to the Central Statistical Office, the amount of thermally treated waste
exceeded 240,000 tonnes, which corresponded to 23.2% of the overall
amount of sludge generated (Domańska Wiesława, 2019).
One of the applications of SSA has been in the building materials
industry. Such waste materials can be incorporated, inter alia, in

* Corresponding author.
E-mail address: tomasz.zdeb@pk.edu.pl (T. Zdeb).

https://doi.org/10.1016/j.jclepro.2022.131055
Received 21 May 2021; Received in revised form 19 January 2022; Accepted 19 February 2022
Available online 28 February 2022
0959-6526/© 2022 Elsevier Ltd. All rights reserved.
T. Zdeb et al.
building materials which contain cement, because binder hydration
products exhibit considerable capacity to immobilise heavy metals
(Chen et al., 2009; Niu et al., 2018; Vyšvařil and Bayer, 2016). This
concept for managing sludge appears to be very useful because, as
shown by the studies conducted by the authors of (Giergiczny and Król,
2008), these composites have the ability to almost completely immo­
bilise heavy metals. The authors demonstrated that after their intro­
duction into cement mortars in the form of nitrate salts at a rate of 1% of
cement by weight, heavy metals were about 99% immobilised when
their water leachability was tested. The amount of heavy metals in ash
depends primarily on the degree of urbanisation and industrialisation of
the area in question. The contamination of ash with heavy metals poses a
major problem in many developing countries.
As the authors of (Górka J, Cimochowicz-Rybicka M., 2019; Smol
et al., 2015) describe, there are many ways in which SS can be used
without thermal treatment. Research results published in (Chang et al.,
2020; Lin et al., 2012; Rezaee et al., 2019) demonstrate that SS can
already be used at the cement production stage as a raw material in the
clinkerisation process. Moreover, authors of publications (Malliou et al.,
2007; Valls and Vàzquez, 2000) show that SS can be directly added to
cement materials. However, raw sewage sludge contains high amounts
of organic matter which delays the formation of basic cement hydration
products and as a result has a significant impact on the setting process
and the mechanical properties of binders. Therefore, raw sewage sludge
without any pretreatment is not a good substitute for cement. On the
other hand, as the results of the research conducted by the authors
(Hamood et al., 2017) show, the use of sewage sludge with pozzolanic
admixtures such as fly ash opens up new possibilities for the develop­
ment of ecological binders.
Studies on the use of sewage sludge ash SSA as a raw material for the
production of clinker are less recognised in the literature. However, the
literature also shows (King Lam et al., 2010; Lin et al., 2005, 2009), that
such solutions are sometimes practiced. Another method – the most
popular one in fact – is to replace some of the cement by adding SSA
during concrete and mortar production (Chang et al., 2020; Lynn et al.,
2015; Smol et al., 2015). The amount of cement replaced varies widely
(from 0% to 30%) and, as shown by the results of the studies conducted
(Chang et al., 2020), it has a considerable influence on the properties of
the resulting composites. According to the research results published so
far (Baeza-Brotons et al., 2014; Chang et al., 2020; Lynn et al., 2015),
SSA can also be successfully used for producing lightweight concrete. In
this case, incinerated sewage sludge serves as a substitute for light­
weight aggregates (fine fractions) or sand. Moreover, as described by
authors of studies that have been published (Chang et al., 2020; Esmeray
and Atıs, 2019; Smol et al., 2015), SSA can also be used for the pro­
duction of ceramic elements used in the construction industry (bricks,
tiles).
Depending on the amount of SSA added to building materials,
desirable changes in the properties of the composite are often observed.
As some studies (Chang et al., 2020) show, this ash can safely be used as
a raw material providing the basis for the production of environmentally
friendly cement in amounts up to 15% by weight since it has a compo­
sition that is very similar mineral to traditional Portland cement and
exhibits comparable properties. However, greater quantities of ash
cause a deterioration in mechanical properties and an increase in water
demand. These results have also been confirmed by the studies described
in (Lin et al., 2012) where Lin Yiming et al. demonstrated that all
environmentally friendly cement mortars containing SSA in amounts of
up to 15% by weight showed only slightly worse mechanical properties
compared to the reference material. However, special attention should
be paid to the question of the setting time of the organic binder. High
P2O5 content significantly delays both the initial and final setting times
of the cement paste. According to the authors of (Lin et al., 2012),
depending on the amount of ash used, the initial setting time is delayed
by 47%, and the final setting time is delayed by 42% in comparison with
the reference cement.
2
Journal of Cleaner Production 345 (2022) 131055
As shown by the studies discussed in (Chang et al., 2020), using
10–20% SSA as a cement replacement in mortars results in a slight but
acceptable decrease in workability and strength compared to ash-free
specimens. The use of SSA as a substitute for fine aggregate in con­
crete production is also widely described in the literature. In (Baeza-B­
rotons et al., 2014), the results of studies are presented in which quartz
sand was replaced with waste material (SSA) amounting to 10% by
weight. Composites with this share of ash exhibit the most favourable
properties in terms of obtaining the maximum composite density and
tightness as evaluated using the UNE-EN 12390-7 and UNE-83982
methods. The former method determines density and water absorp­
tion, while the latter concerns capillary water absorption. Using both
methods, the authors of the article observed an improvement in the
above properties with a 10% share of SSA. The authors attribute these
results to two physical and chemical effects. On the one hand, the ash
produced by sewage sludge incineration is a fine material which fills the
gaps between relatively large aggregate particles; on the other hand, it is
also a material with identifiable pozzolanic activity. The use of SSA and
of sewage sludge in building materials serves two primary purposes: the
safe management of waste material and the immobilisation of the heavy
metals contained in the sludge through transforming this material into
valuable products while preventing secondary environmental pollution.
Such an effect can be achieved by obtaining a broader knowledge about
the durability of cement composites which contain the ash in question.
In this respect, the literature available remains quite limited. An
exception is the article by Zhiyang Chang et al. (2020), which describes
such characteristics as porosity, absorption, resistance to freezing and
mechanical properties under accelerated carbonation. A significant
publication on advances in cementitious composites containing SSA is
(Cyr et al., 2007). In addition to presenting a broad survey of literature
on the topic, the authors have characterised this type of mineral
admixture to cementitious binders in detail, and demonstrated changes
in the technological and mechanical properties of binders containing
SSA. Substituting 25 and 50% of Portland cement with this mineral
addition resulted in a significant reduction in mechanical properties, but
it was confirmed that this reduction depends on hydration time and
decreases as it becomes longer. The authors attribute this effect to the
involvement of the glassy phase and its ability to undergo a slow
pozzolanic reaction.
The study results presented in this publication are meant to charac­
terise as comprehensively as possible the ash produced by the inciner­
ation of sewage sludge in a Polish wastewater treatment plant. The
paper describes, inter alia, its chemical composition, phase composition,
grain size distribution, specific surface area and pozzolanic reactivity
determined using one of the chemical methods as well as the mechanical
method. It also presents changes in the technological properties of
binders in which cement was replaced with SSA in amounts ranging
from 0 to 40% by weight in steps of 10%. On the other hand, studies of
mechanical properties of standard mortars demonstrated that at a low
(10%) SSA content, an improvement in mechanical properties was
achieved together with an associated increase in durability confirmed by
a reduction in total porosity and lower diffusion of chloride ions. The
microstructure of the produced binders containing SSA has also been
described alongside the presentation of the main mechanism by which
sulphate ions cause corrosion in such materials.
2. Materials and methods
The waste material (WM) used in the study was ash produced during
the incineration of sewage sludge from the Płaszów sewage treatment
plant operated by the Cracow Waterworks in Poland. The plant has its
own sludge thermal treatment station with a capacity of about 64 tonnes
of dry matter per day. The ash is produced by incinerating dried and
centrifuged sludge in a fluidised bed furnace at a temperature of around
850 ◦ C. The basic chemical composition of ash is shown in Table 3. On
the other hand, the basis for producing the binder was pure CEM I 42.5 R
T. Zdeb et al. Journal of Cleaner Production 345 (2022) 131055

Portland cement whose chemical characteristics, phase composition and the (PN EN 12457-4, 2006) Characterisation of waste - Leaching -
main physical properties are shown in Table 1. Conformity test for leaching of granular waste materials and sludges -
During tests of binders containing SSA, pastes and mortars were Part 4: One-stage static test with a liquid to solid ratio of 10 l/kg for
produced containing 10%, 20%, 30% and 40% of ash by weight (as a materials with a particle size less than 10 mm (with or without dimen­
replacement for cement). The mortars produced for the purposes of sion reduction). In order to study the total heavy metal content in SSA
mechanical and durability tests were characterised by a constant w/b and cement, the materials were mineralised in aqua regia (3 ml HCl + 1
ratio of 0.5 and a constant binder to aggregate ratio of 1:3. SSA exhibits ml HNO3 + 0.5 g solid) in a closed microwave mineraliser at 180 ◦ C for
very high water demand, and therefore both plasticizer and super­ 45 min. The process was carried out in accordance with EN 13346 –
plasticizer were used in order to obtain an optimal, uniform consistency. Characterization of sludges – Determination of trace elements and
All mortars had a very similar consistency as determined by the EN phosphorus – Aqua regia extraction methods. The content of heavy
1015-3 method with a flow diameter of around 15 cm. With 40% ash metals: Sb, As, Se was tested using the ICP (Inductively Coupled Plasma)
content and the maximum amount of superplasticiser added, the desired method in accordance with the (PN EN ISO 11885, 2010). To determine
consistency could not be achieved. The compositions and exact flow the level of chromium leachability, the AAS (Atomic Absorption Spec­
diameters for individual specimens are given in Table 2. The specimens trometry) method was used in accordance with the (PN EN 1233, 1997).
were cured for 14, 28 and 90 days under conditions preventing water In other cases of heavy metals the tests were performed in accordance
evaporation according to EN 196-1. with the (PN EN ISO 8288, 1986) Water quality - Determination of co­
The tests conducted were divided into three parts. The first part was balt, nickel, copper, zinc, cadmium and lead - Flame atomic absorption
focused on chemical tests of the SSA admixture, in the second part there spectrometric methods. The content of chloride and sulphate ions is
were tests concerning the physical and mechanical properties of the determined using the spectrophotometric method. For this purpose, it is
binders received, and the third part was composed of tests of its dura­ necessary to prepare a distilled water solution and a fragmented sample
bility characteristics. The chemical composition of SSA were determined in the proportion of 5:1, and then filter it after 24 h. The result obtained
by the XRF method with the use of MiniPal 4 analyser PANalytical B.V. is given in [mg/l].
In the case of phase composition, the studies of SSA and binders were Chapelle’s test generally consists of a reaction between 2 g of calcium
carried out using the Philips PW1830 apparatus, determining the con­ hydroxide and 1 g of the test material in aqueous solution at 90 ◦ C over a
tent of crystalline phases using the diffractometric method - XRD (Cu-Kα period of 16 h. Pozzolanic activity is determined on the basis of the
lamp in the angular range 10–60◦ 2Ɵ, step 0.05). Due to the high content relationship (2.1) (Ferraz et al., 2015)
of oxides (SiO2, Al2O3 and Fe2O3), the potential pozzolanic activity of
2⋅(V1 − V2 ) 74
the ash was additionally verified by a chemical method (Chapelle’s test) PASSA = ⋅ ⋅1000 [mg / g] (2.1)
V1 56
and compared to materials with known pozzolanic activity values, i.e.
silica fume, fly ash and metakaolin. Pozzolanic activity was also deter­ where:
mined by a mechanical method in accordance with EN 450-1; this
consisted in the production of a standard mortar containing binder PASSA – Pozzolanic Activity of SSA expressed as the number of mil­
which consisted of 75% CEM I 42.5 reference cement and 25% SSA by ligrams of Ca(OH)2 bound per 1 g of SSA;
weight. According to the recommendations included in the standard, the V1 –volume of 0.1 N HCl (in cm3) used for the titration of the blind
compressive strength value after 28 days (i.e. the strength activity index sample (containing no SSA).
– SAI) should be higher than 75% of the reference value, i.e. the strength V2 –volume of 0.1 N HCl (in cm3) used for the titration of the sample
of the mortar without the admixture. Moreover, the value of this index that contained 1 g of SSA.
after 90 days of curing should not be less than 85% of the reference
value. The BET specific surface area of the SSA mineral addition was
Heavy metal leachability tests were carried out in accordance with determined using the Quantachrome NovaWin 2200 apparatus, while
the grain size distribution was determined with a particle size analyser
(Malvern Instruments Mastersizer 2000 with a Hydro 2000 wet disper­
Table 1
sion unit) using the laser diffraction method.
Chemical and phase composition and basic properties of CEM I 42.5 R cement.
Microstructure observations were conducted using a Zeiss EVO10M
Component Quantity scanning microscope equipped with an EDS detector. In order to be able
[-] [% by weight] to observe the cross-sectional morphology of SSA grains, polished cross-
Chemical composition sections were produced by dipping them in resin. The cross-section
SiO2 19.8 surfaces were first polished using corundum grinding powders with
CaO 64.6 grain sizes ranging from 90 μm to 3 μm, and subsequently using pol­
MgO 1.0 ishing pastes with grain sizes ranging from 3 μm to 0.25 μm. The surfaces
Al2O3 4.9
Fe2O3 2.7
thus prepared were then cleaned and degreased in acetone.
SO3 2.9 Tests of physical characteristics concerned the water demand of
Na2Oe 0.48 newly produced binders and their initial and final setting times ac­
Cl− 0.024 cording to the EN 196-3 standard. In the case of mechanical character­
P2O5 –
istics, compressive strength and tensile strength at three-point bending
LOI 2.9
Phase composition were determined after 14, 28 and 90 days of curing. The tests were
C3S 59.8 conducted on cement mortars produced in accordance with the EN 196-
C2S 5.5 1 standard. Therefore, flexural strength was determined by testing three
C3A 8.5 40 mm × 40 mm × 160 mm specimens each time, and compressive
C4AF 8.5
Physical properties
strength was determined by testing six 40 mm cubic specimens.
Water demand [%] 27 Tests of durability characteristics included the determination of total
Initial setting time [min] 195 porosity conducted by comparing bulk (volumetric) density ρbulk to true
Final setting time [min] 245 density ρtrue determined using a helium pycnometer.
Blaine specific surface area [cm2/g] 3460
Compressive strength after 2 days fc,2 [MPa] 26.1 ρbulk
P= × 100 % (2.2)
Compressive strength after 28 days fc,28 [MPa] 59.8 ρtrue

3
T. Zdeb et al. Journal of Cleaner Production 345 (2022) 131055

Table 2
Mortars composition.
Label Ingredients Consistency

Sand Cement Water Sludge Plasticizer Superplasticiser w/b Flow diameter

[g] [g] [g] [g] [g] (% c.wt.) [g] (% c.wt.) [-] [cm]

REF 1350 450 225 – – – 0.5 ⁓15

SSA 10 405 45 4.50 (1.0) –
SSA 20 360 90 2.25 (0.5)
SSA 30 315 135 9.00 (2.0)
SSA 40 270 180 10.3 (2.3) No workability

where: Xt = Δlt (Na2 SO4 ) − Δlt (H2 O) (2.4)

P – porosity [%] where:

ρbulk – bulk (volumetric) density [g/cm3]
ρtrue – true (helium) density [g/cm3] Xt – expansion value [%]
Δlt (Na2SO4) – arithmetic mean of the change in beam length in
Apart from the total porosity of cement mortars, the impact of the sodium sulphate solution [%]
amount of SSA in the binder on their ability to transport chloride ions Δlt (H2O) – arithmetic mean of the change in beam length in distilled
was also determined. The value of the Cl− diffusion coefficient was water [%]
determined according to NT BUILD 492 using equation (2.3).
( √̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅ ) 3. Study results and discussion
0.0239(273 + T)L (273 + T)L × xd
Dnssm = × xd − 0.238 (2.3)
(U − 2)t U− 2
3.1. Chemical and physical properties

where:
Referring to the publication (Cyr et al., 2007), where the authors
− 12 2 compared SSA compositions in more than 30 regions of the world, the
Dnssm – non-steady-state chloride migration coefficient [×10 m /
chemical composition of the SSA analysed is not different from the
s];
average compositions determined in other countries. The only deviation
T – temperature [◦ C]
is the elevated content of iron (expressed as Fe2O3) at 22.5% and P2O5 at
L – specimen thickness [mm]
18.0% (see Table 3). The ash in question is mainly composed of silicon
U – DC voltage [V]
(SiO2), aluminium (Al2O3) and iron (Fe2O3) oxides, which suggests that
t – test duration [h]
the material has the potential to react with calcium hydroxide, and thus
xd – average Cl-penetration depth determined after reaction with
to exhibit pozzolanic properties. Regardless of the season in which the
AgNO3 [mm]
sewage sludge is produced, the sum of these oxides exceeds 65% of ash
by weight. Therefore, during further tests, pozzolanic activity was
Tests of resistance to sulphate attack were conducted in accordance
determined using Chapelle’s test and compared to the values for known
with Polish standard PN-B 19707. To this end, 20 mm × 20 mm × 160
pozzolanic admixtures such as silica fume, fly ash and metakaolin. In
mm beams made of standard mortar were used. Tests were conducted
addition, the SAI (strength activity index) of the SSA addition was
after 28 days of curing. Expansion Xt after 52 weeks, and then after every
verified using the mechanical method according to the EN 450-1 stan­
four weeks, was determined for specimens stored in a sodium sulphate
dard. Moreover, the large quantity of P2O5 found in the ash may result in
solution with a SO42− concentration of 16.0 ± 0.5 g/l in relation to
a significant increase in the setting time of binders with SSA added,
control specimens, i.e. those stored in distilled water. The Xt expansion
which was later confirmed in tests. The presence of corrosive ions such
value is calculated from relationship 2.4.
as sulphates, chlorides or alkali ions appears to be low and safe, given
the criteria stated in the EN 450-1 standard for fly ash (FA). After

Table 3
Chemical composition of SSA against literature values and comparison to other waste materials.
Component SSA SSA (Cyr et al., 2007) Granite (Nasr et al., 2020) Glass (Mirzahosseini and Riding, 2014) Clay brick (Olofinnade et al., 2016)

min - max mean

Quantity [% by mass]

SiO2 29.9 14.4–65.0 36.1 72.4 73.5 60.6

Al2O3 9.6 4.4–34.2 14.2 8.1 0.1 14.2
Fe2O3 22.5 2.1–30.0 9.2 1.9 0.3 4.9
CaO 13.5 1.1–40.1 14.8 1.5 9.0 0.3
Na2Oe 1.0 0.01–6.8 0.9 3.7 12.7 1.9
SO3 0.1 0.01–12.4 2.8 – – –
P2O5 18.0 0.3–26.7 11.6 – – 0.9
Cl− 0.6 – – – – –
LOI 0.3 0.2–41.8 6.1 – – –

4
T. Zdeb et al. Journal of Cleaner Production 345 (2022) 131055

Table 4 the silica contained in the ash is likely to remain in crystalline form,
SSA pozzolanic activity values compared to traditional pozzolanic concrete which exhibits low reactivity (see Fig. 1). Moreover, as confirmed by the
admixtures. test results and the literature studies of the BET specific surface of the
Pozzolana type Pozzolanic activity [mg/g] ash, this ingredient has a significantly smaller reaction area compared to
SSA (sewage sludge ash) 193
silica fume or fly ash. SSA specific surface area usually ranges from 500
SF (silica fume) 1751 to 4000 m2/kg (Chang et al., 2020; Lynn et al., 2015), while that of silica
metakaolin 910–1560 (Ferraz et al., 2015; McCarter and Tran, 1996) fume ranges from 13,000 to 23,000 m2/kg (Kurdowski, 2014) and that
FA (fly ash) 768 (Záleská et al., 2018) of fly ash from 8800 to 16,500 m2/kg (Wang et al., 2018). In the case of
the mineral addition in question, this figure is relatively high in com­
parison to other SSAs and amounts to 3900 m2/kg.
burning, SSA no longer contains any dangerous bacteria and
The morphology, grain size and distribution of the main elements
micro-organisms or organic matter. Pursuant to the Act on Waste of
contained in the ash have been identified through SEM observations and
2012 (Dz.U. RP 2013 poz. 21, 2013) it is stabilised, but the ash still
additional EDS analysis. The grain size shown in Fig. 2 corresponds well
contains heavy metals; in qualitative terms, these are mainly Ti, V, Mn,
with the results of the grain size distribution study performed by the
Co, Ni, Cu and Zn. The exact SSA composition is summarised in Table 5.
laser method (see Fig. 3). It is characterised by a unimodal pattern with a
As concerns the chemical compositions of other mineral additions
distinct peak at grain diameters between 40 μm and 50 μm. The full
considered in recent years, many of those have a high content of
range of grain sizes is from 0.3 to 100 μm, with d10, d50 and d90 grain
structure-forming oxides (SiO2, Al2O3 and Fe2O3), which are responsible
sizes being 1.8, 25.8, and 63.0 μm, respectively. These parameters
for the material’s potential ability to undergo a pozzolanic reaction. In
confirm the limited SSA surface available to react with Ca2+ ions
the case of granite powder, the sum of these oxides admittedly exceeds
compared to SF or FA. The morphology of the observed grains varies
80%, but according to (Nasr et al., 2020), this admixture is inert in
depending on the phase analysed. The mapping of the distribution of
character. On the other hand, brick powder is another waste material
elements on the surface of the polished cross-section enables the indi­
used in the manufacture of cementitious composites. According to the
vidual phases identified by XRD to be detected. In the foreground, two
studies conducted (Olofinnade et al., 2016) and (Bediako, 2018), the
solid quartz grains characterised by irregular edges can be seen. The
sum of SiO2, Al2O3 and Fe2O3 oxides in this material ranges from 70% to
second phase visible in the X-ray diffractogram (Fig. 1) is hematite.
more than 80%. Research results (Bediako, 2018) demonstrate that the
Typical Fe2O3 manifestations are spheroid shaped crystals, an example
consumption of portlandite in cement pastes containing brick powder as
of which can be found in the lower left corner of the image (see Fe-KA
compared to the control specimen is significant at 25% after just 7 days
Fig. 2). The most irregular grains with porous structures contain min­
of curing. Very similar Ca2+ consumption results were obtained by
erals derived from calcium and aluminium phosphates, which represent
(Mirzahosseini and Riding, 2014) for powdered glass cullet, which is
attributed to its amorphous structure.
According to the X-ray diffractogram presented (see Fig. 1), the ox­
ides identified form the following crystalline phases. Silica occurs
mainly in the form of β-quartz. Its highly crystalline nature may be due
in part to its relatively low alkali content compared to other SSAs as
reported in (Cyr et al., 2007), which was determined at Na2Oe = 1.0%. A
higher alkali content could enable the formation of local eutectics,
which in turn could result in the transformation of quartz to its amor­
phous form. Iron, which occurs mainly in the oxidation number three,
mainly forms the hematite phase, but is also present as inclusions in
phosphate minerals. Additionally, due to the high P2O5 content in
sewage sludge, which is attributed mainly to detergents, a crystalline
form of calcium aluminium phosphate salt with the overall formula
Ca9Al(PO4)7 emerges during the combustion process in an industrial
fluidised bed furnace.
The limited reactivity of SSA compared to silica fume is mainly due
to the high proportion of silica structure which has not been converted
to an amorphous state. The relatively low temperature at which sludge is
Fig. 1. XRD pattern of SSA admixture.
treated in a fluidised bed furnace and the low alkali content mean that

Table 5
Total mass of heavy metal in SSA and cement and leachability from mortars.
Sb As Cr Zn Cd Cu Ni Pb Hg Se Cl− SO42-

[mg/kg]
SSA* 14 9.3 446 3532 <8 668 156 124 0.4 <2 n/a n/a
CEM I 42.5 R* 9 7.8 <40 926 <8 125 <40 53 0.1 3 n/a n/a
[mg/l]
REF 0.04 0.03 <0.2 <0.08 <0.04 <0.06 <0.2 <0.2 <0.0003 0.03 20 52.2
SSA 30 0.038 0.03 <0.2 <0.08 <0.04 <0.06 <0.2 <0.2 <0.0003 0.034 30 246
Inert waste (Dz.U. RP 2015 poz. 1277, 2015) <0.06 <0.5 <0.5 <4 <0.04 <2 <0.4 <0.5 <0.01 <0.1 <800 <1000
Non-hazardous wastes (Dz.U. RP 2015 poz. 1277, <0.7 <2 <10 <50 <1 <50 <10 <10 <0.2 <0.5 <15000 <20000
2015)
Hazardous wastes (Dz.U. RP 2015 poz. 1277, 2015) <5 <25 <70 <200 <5 <100 <40 <50 <2 <7 <25000 <50000
Sewage discharged into water and soil (Dz.U. RP <0.3 <0.1 <0.5 <2 <0.2 <0.5 <0.5 <0.5 <0.03 <1 <1000 <500
Poz. 984 Nr. 137/2006, 2006)
Surface water intended for the abstraction of – <0.05 <0.05 <5 <0.005 <0.5 <0.2 <0.05 <0.001 <0.01 <250 <250
drinking water A3 (Dz.U. RP Poz. 1747, 2019)

* Total mass of heavy metals dissolved in aqua regia.

5
T. Zdeb et al. Journal of Cleaner Production 345 (2022) 131055

Fig. 2. SEM image of SSA grains with the distribution of the main elements, magnification 1000×.

a significant proportion of the studied SSA. In addition to the main

Fig. 3. Grain size distribution on the SSA.
phases mentioned above, the analysed chemical composition of indi­
vidual grains gives grounds for assuming that other minerals such as
alkali feldspars, anhydrite, or perkovaite are present as well.
In addition to the chemical analysis of SSA pozzolanic reactivity
conducted using Chapelle’s test, activity tests using the indirect method,
which consists in determining the SAI (strength activity index), were
performed as well. The results of this test are surprisingly positive.
Relative compressive strength after 28 days was as high as 86% of the
reference value, and after 90 days of curing this ratio reached 94%. It
should be recalled that the criteria adopted according to the EN 450-1
standard for fly ash (FA), which is known for its pozzolanic activity,
are 75 and 85% after 28 and 90 days of curing, respectively. These re­
sults are presented in Figs. 4 and 5. The authors of the (Lynn et al., 2015)
review article tracked more than a dozen other reports on this subject.
They demonstrated that in most cases, the substitution of cement with
SSA, when done in accordance with standards, meets the criteria for the
pozzolanic activity index. In those studies, the SAI ranged from 75 to
85% of the reference value after 28 days of curing.
Given the SSA reactivity values shown in Chapelle’s test, it is difficult

6
T. Zdeb et al.
Fig. 4. Compressive strength after 28 and 90 days of curing.
Fig. 5. Pozzolanic activity after 28 and 90 days of curing.
to speak of the pozzolanic activity of this mineral addition. Analysing
the values shown in Table 4, SSA reactivity was just 10% and 25%
compared to SF or FA, respectively. Therefore, the fulfilment of the
criteria with respect to SAI should rather be attributed to the favourable
physical effects of this admixture which seals the structure of the test
mortar since the specific surface of SSA is more developed than that of
cement by a factor of around ten.
Fig. 6. Water demand of cement pastes containing SSA.
7
Journal of Cleaner Production 345 (2022) 131055
3.2. Physical properties of binders
The water demand of binders containing SSA was determined ac­
cording to the EN 196-3 standard. To this end, cement pastes containing
0%, 10%, 20%, 30% and 40% ash were prepared. The results are pre­
sented in Fig. 6. Owing to its grain size distribution and composition,
SSA exhibits a very high water demand, so as the share of this admixture
in mortars and pastes increased, their workability was significantly
reduced. A gradual, steady increase in water demand was observed with
each 10% increase in the amount of ash added. For the maximum
amount of SSA, an increase of 13% compared to the reference value was
recorded. Similar qualitative relationships have been observed by many
of the researchers mentioned in the publication (Cyr et al., 2007).
Having observed the increase in water demand of binders containing
SSA as reflected by the rheological properties of mortar mixes, a team of
researchers (Monzó et al., 2003) (Monzó et al., 1996) also confirmed the
negative effect of this mineral addition and explained that this was
mainly due to the irregular shape of the grains.
Owing to the high content of phosphates in the composition of SSA,
the setting time for the binders containing this mineral addition was
examined. The results are presented in Fig. 7. An addition of SSA of up to
30% of binder weight results in a steady increase in both initial and final
setting times. The initial setting time is almost twice as long, while the
final setting time increases by around 60%. Relatively small differences
of a few percent can also be noticed between these parameters when the
SSA share in the binder ranges from 20 to 30%. However, there is no
doubt that a 40% proportion of ash in the binder changes the values of
these parameters dramatically, increasing both initial and final setting
times by a factor of more than four, which makes the process last up to
21 h. This phenomenon, which has been observed by numerous re­
searchers (Tkaczewska, 2012), (Cau Dit Coumes and Courtois, 2003)
and (Bénard et al., 2005), can be attributed to the retarding effect of
phosphate ions which hinder the hydration of cement grains.
3.3. Mechanical properties
The results of tests on mechanical properties are presented in
Figs. 8–11. The most important observations include the fact that irre­
spective of the amount of cement replaced by SSA, no decrease in
strength was observed as the curing period became longer, and a mod­
erate increase up to 90 days was even recorded. In addition, it can
generally be concluded that the addition of 10% SSA to the cement
binder has favourable effects reflected in an improvement in mechanical
properties.
In the case of flexural strength, this increase is not as spectacular and
unambiguous since it fluctuates around the limit of the natural variation
in this characteristic at the level of a few percent. In a binder containing
Fig. 7. Setting time for binders containing SSA.
T. Zdeb et al.
Fig. 8. Flexural strength for individual curing periods and proportions of ash
dry matter in the mortar.
Fig. 9. Relative flexural strength for individual curing periods and proportions
of ash dry matter in the mortar.
Fig. 10. Compressive strength for individual curing periods and proportions of
ash dry matter in the mortar.
20% ash, a decrease in strength by about 10% can be observed after 14
and 28 days of curing. After a longer curing period, i.e. 90 days, flexural
strength reaches a value close to the reference one. A similar relation­
ship can be observed in the study conducted by (J.Payá et al., 2004). In
tests of mortars containing 15% of SSA by weight in the binder, flexural
strength does not exceed the reference value in the early curing period, i.
e. after 3, 7 and 14 days of curing. Later, i.e. after 28, 60 and 90 days,
these values become equal. For composites in question containing 30%
SSA, a clear deterioration in mechanical properties is observed for each
curing period, i.e. 20%, 22% and 8% at 14, 28 and 90 days, respectively
(see Fig. 9). The results of the (J.Payá et al., 2004) study confirm this
8
Journal of Cleaner Production 345 (2022) 131055
Fig. 11. Relative compressive strength for individual curing periods and pro­
portions of ash dry matter in the mortar.
relationship.
With regard to compressive strength, a 10% share of SSA is slightly
more conducive to an improvement in this characteristic than in the case
of flexural tensile strength. In the case of a 14-day curing period, the
increase compared to the reference value is as much as 30%. For other
curing periods, the increase does not exceed 10%. It is worth empha­
sising that composites containing 20% ash exhibit compressive strength
values which deviate slightly from the reference values. A similar rela­
tionship was shown by (J.Payá et al., 2004), but for SSA share at 15% of
cement binder. A clear reduction in this parameter only occurs when
30% of the cement is replaced by ash. This phenomenon occurs
regardless of the curing period and the compressive strength ranges
between 83 and 89% of the reference value. As shown in the studies
cited above, SSA at 30% of binder significantly reduces the compressive
strength of mortars, but this effect is particularly pronounced in the
early curing period.
3.4. Density and total porosity
The results obtained with respect to density and total porosity are
presented in Fig. 12. It can be noticed that with 10% and 20% ash there
is a decrease in porosity which results in the material being tighter. With
10% ash, porosity decreases by as much as 4.2%, while with 20% ash,
porosity is also lower than for the reference sample, but by just 2.9%.
These decreases in porosity are reflected in the mechanical character­
istics shown in Figs. 6–9. At 30%, porosity exceeds the reference value
by 2.6% which also entails a deterioration in mechanical properties.
Changes in porosity are also reflected in other characteristics, especially
durability.
Fig. 12. True and bulk density values together with the calculated
total porosity.
T. Zdeb et al.
3.5. Leachability of heavy metals
Table 5 shows the total content of heavy metals for SSA and cement
as well as the leachability of heavy metals for a cement mortar con­
taining an addition of 30% SSA and for the reference mortar. These
results were compared with the criteria for waste and sewage discharged
into the environment and surface waters.
The heavy metal content measurements presented in Table 5 show
that their total amount in SSA is similar to those observed in the liter­
ature (Cyr et al., 2007), with the exception of zinc whose concentration
is as much as two orders of magnitude higher. The situation is similar for
copper and lead, but their concentrations are around one order of
magnitude higher. As concerns their leachability from mortars, the
majority of heavy metals were below detection level even with the
maximum amount of sewage sludge ash admixture, which is 30%.
Comparing the leachability of heavy metals from the mortar containing
SSA with the reference one containing no waste materials, it can be
concluded that their content and in fact leachability level, does not pose
a threat to the natural environment because no significant differentia­
tion was observed in relation to all the heavy metals analysed. The
leachability values obtained were compared to the criteria for various
categories of waste, i.e. inert, non-hazardous and hazardous. Regardless
of the composition of mortars, the leachability of all heavy metals was
below the limit, even for inert waste. Moreover, with all of the mortars
investigated, the eluent composition meets the requirements for
post-production wastewater. The exception is the selenium content,
which exceeds the permissible value in the case of surface water inten­
ded for the abstraction of drinking water. It should be mentioned here
that with respect to the leachability of heavy metals from cement mor­
tars containing SSA at 25%, the authors of the publication (Coutand
et al., 2006) showed that the concentrations of Ti, V, Cr, Ni, Cu, Zn, As,
Cd, Sn, Sb and Pb in the elution solvent meet the requirements for
drinking water set by the World Health Organization. With respect to
Cl− and SO42− anions, their concentrations do not exceed the limit
values with regard to even the most restrictive requirements, i.e. those
concerning surface water.
3.6. Diffusion of chloride ions
The change in material tightness resulting from the addition of SSA
in various proportions should also be reflected in the material’s ability to
transport chloride ions. To test this characteristic, cylindrical specimens
with the following dimensions: φ = 100 mm and L = 50 mm were
prepared and saturated in a calcium hydroxide solution according to the
methodology stated in Section 2.3. The test stand is shown in Fig. 13.
On the test stand shown in Fig. 13, three specimens were tested
simultaneously. The tightness ranges of all test materials made it
possible to perform tests concerning the accelerated transport of chlo­
ride ions under the same time and current conditions. Each specimen
was tested for 24 h at a constant voltage of 20 V. Average results ob­
tained during the testing of three specimens are shown in Fig. 15. The
chloride-migration fronts for the REF, 10%, 20% and 30% specimens are
shown in Fig. 14.
Fig. 13. Test stand made in accordance with NT BUILD 492.
9
Journal of Cleaner Production 345 (2022) 131055
Where the share of ash in cement composite amounts to 10%, a
significant decrease in the diffusion coefficient of chloride ions is
observed. This reduction, which is as much as 62%, is due to the
reduction in material porosity confirmed by the tests described above.
For the material containing 20% SSA, a slightly increased structural
tightness vis-à-vis the reference material can also be observed (see
Fig. 12). This is reflected in a reduction of the Cl− diffusion coefficient,
which amounts to slightly over 10%. With a higher share of ash, i.e.
30%, the Dnssm factor slightly exceeds the reference value. This confirms
the very strong correlation between total porosity and the Cl− ion
diffusion coefficient, but the population of the results obtained is too
small, which makes it impossible to formulate a credible model
describing the correlation between these characteristics.
3.7. Resistance to sulphate attack
Resistance to sulphate corrosion mainly depends on the type of
cement, and more specifically on its calcium aluminate content, espe­
cially the C3A phase. Cements which are resistant to sulphate ions (SR
and HSR) are mainly those which contain a significantly reduced
amount of Portland clinker, and are mostly included in the CEM III
group of cements. The CEM I 42.5 R cement used in this test does not
have the ability to inhibit expansion in the presence of sulphate ions,
since it contains 8.5% C3A, but the observed increase in material
tightness and the decrease in C3A content in the binder containing SSA
served as signals that this characteristic should be examined. Results of
the studies conducted are presented in Fig. 16.
As the studies conducted have demonstrated, the use of SSA as a
substitute for cement clearly caused a deterioration in the mortar’s
resistance to sulphate ions irrespective of the amount of ash used. The
reference specimen reached its expansion limit of 0.5% after 28 weeks.
Specimens containing ash, irrespective of its amount, reached that limit
approximately at the same time: 8 weeks after the start of the study.
However, further expansion differed for each type of material. The more
cement was replaced by SSA, the greater the expansion value. In the case
of specimens containing 20% and 30% ash, destruction followed after 28
weeks, while reference samples and those containing 10% ash were
destroyed after 40 weeks from the start of the study. It is generally
known and also included in European standards that the resistance to
the sulphate attack of cements containing pozzolanic admixtures,
including those from the CEM II or CEM IV group, is increased. However,
in the case of the SSA addition, as shown in the reactivity tests with the
Chapelle test (see Chapter 3.1.), the chance of creating an additional,
sealing composite structure C–S–H phase is rather low or requires a
significantly longer hydration period. Moreover, tightness tests of
mortars containing 20 and 30% SSA confirm the increase in potential
migration of SO42− ions into the composite and the reaction with hy­
drated calcium aluminates.
3.8. Microstructure
Irrespective of SSA content, the XRD phase composition analysis of
cement pastes confirmed the presence of minerals typical of this type of
materials. Relics of unreacted cement grains can be observed in the form
of alite or belite reflections. Subsequently, portlandite was revealed as a
product of the reaction between cement and water, alongside the calcite
phase produced by the carbonation of the tested paste. The β-quartz
phase, on the other hand, comes directly from the SSA admixture (see
Fig. 1). There is an interesting discussion in the literature about the
presence of brushite, the phosphate phase that emerges when the
amorphous iron phosphate present in SSA reacts with calcium hydrox­
ide. This phase is thought to improve the mechanical characteristics of
mortars (Chen and Poon, 2017). However, there are also reports that
may contradict the stability of this phase in cement pastes with high pH
(Bohner, 2000; Brown, 1999). The additional solubility tests of the
phosphate phases present in SSA, conducted according to the procedure
T. Zdeb et al.
Fig. 14. Surface of specimen fracture after the chloride ion migration test: (a) REF; (b) containing 10% SSA; (c) containing 20% SSA; (d) containing 30% SSA.
Fig. 15. Chloride ion diffusion in cement mortars containing SSA from sewage
sludge incineration.
Fig. 16. Resistance to sulphate corrosion of mortars made using CEM I cement
with the addition of ash from the incineration of sludge from a sewage treat­
ment plant.
described in EN 450-1 (Annex C), i.e. in a solution with a pH of 8.5,
resulted in a value of 21.4 mg/kg of dry mass of SSA. This result makes it
possible to determine the amount of available P2O5 at the level of 0.18%
of its total content in ash. It should also be mentioned that this value may
be significantly lower due to the high pH of the cement paste. Therefore,
10
Journal of Cleaner Production 345 (2022) 131055
Fig. 17. XRD pattern of blended paste SSA 30.
taking into account the amount of available P2O5 and the composition of
the mortars tested (with SSA content ranging from 10 to 30% in the
binder), it is difficult to suppose that phosphate phases contribute
significantly to the strength of mortars containing SSA admixtures. The
experimental results presented in Fig. 17 did not reveal the presence of
any crystalline phosphate phases.
Microstructure observations of polished cross-sections of mortar
specimens containing 30% SSA made it possible to explain the main
reason for the rapid progress of sulphate corrosion in these composites.
As can be observed in Fig. 18, quartz sand grains are visible in the
foreground, around which calcium ions accumulate in slightly higher
concentrations compared to the binder. This demonstrates the formation
of a distinct interfacial transition zone (ITZ). The main causes of its
formation are believed to be the adsorption of water on the surface of
unreacted aggregate grains, which leads to a local increase in the water-
cement ratio in this area, and the uneven distribution of cement grains
around the aggregate surface – the so-called wall effect. Thus, a local
increase in porosity and in the hydration degree of cement as well as
heterogeneous nucleation on the surface of aggregate grains of those
phases for which the solubility equilibrium is exceeded, i.e. primarily Ca
(OH)2, can be expected, which has been confirmed in many publications
(Diamond, 2001), (Kurdowski, 2014). In addition, a local increase in the
hydration degree of cement leads to increased paste shrinkage, which
may in turn result in the paste debonding from the aggregate. All these
local variations in binder matrix uniformity increase the potential for
corrosion processes. Unfortunately, these phenomena were not reduced
T. Zdeb et al.
Fig. 18. SEM observations and EDS mapping of a polished SSA 30 mortar cross-section subject to sulphate ion corrosion.
in the microscopic areas observed due to the low pozzolanic reactivity of
SSA. Total porosity and chloride ion diffusion tests confirmed the
increased potential of liquid and gaseous media migration, especially for
the SSA 30 mortar. However, it was the ITZ where the corrosive sulphate
ion solution was easily able to infiltrate the structure of the material,
which is illustrated by the clearly defined envelope of sulphur atoms
around quartz grains. The shapes of the crystals observed in this zone
suggest that 52 weeks of exposure of mortars to a sodium sulphate so­
lution with a SO42− concentration of 16.0 g/l result in mainly ettringite
crystallising.
4. Summary and conclusions
Despite the significant changes in the technological characteristics of
binders which contain SSA, mainly concerning their setting time, it
appears that this type of waste material can be used for producing
cement composites, replacing up to 30% of cement by weight. Regard­
less of the composition of the test mortar, the leachability of the heavy
metals was very similar and in most cases below detection level. The
mortar with 30% SSA addition meets the leachability requirements for
inert wastes and also meets requirements for surface waters and there­
fore has no environmental impact. The low level of leachability is
related to the high degree of immobilisation of heavy metals in the
cement matrix, the quantification of which may be the subject of further
research.
The SSA admixture in the cement binder increases the water demand
of the binder and significantly extends its setting time. A 30% proportion
of SSA doubles the initial setting time and extends the final setting time
by approximately 60%. As the study of the technological characteristics
shows, it is not recommended to use SSA in larger quantities.
A relatively small addition of sewage sludge ash, i.e. not exceeding
10% of cement weight, even has a positive effect on both the mechanical
properties of cement mortars and their tightness. A slight increase in
compressive strength and tensile strength at bending is observed
regardless of the progress of hydration over a period of 14–90 days. This
increase is recorded at an average level of over a dozen percent. This
increase is attributed to the physical sealing of the composite structure
(a reduction of more than 4% in total porosity) rather than the pozzo­
lanic reactivity of the SSA. Indeed, the Chapelle test showed the reac­
tivity of this material at a low level, about 10% compared to the silica
fume.
A further increase in the amount of SSA from 20 to 30% of cement
weight causes the properties of the mortars tested to deteriorate, but in a
controlled manner and to an acceptable degree. In the case of 20% SSA
content, irrespective of the progress of hydration, the level of
compressive and tensile strength at bending is close to the properties of
the reference material. When the proportion of SSA is increased up to
11
Journal of Cleaner Production 345 (2022) 131055
30%, the mechanical properties are reduced by an average of 20%
compared to the material without SSA added.
With regard to the durability characteristics of the test mortars, in
particular the diffusion of chloride ions, a qualitative relationship was
confirmed relating to the total porosity of cement mortars containing
variable amounts of the SSA admixture and their ability to transport
chlorides. Physical sealing of the microstructure of mortars containing
10% SSA in the binder effectively reduces the value of the Cl− diffusion
coefficient by a factor of more than two.
The results of other durability tests confirmed that a binder CEM I
with a high content of C3A at the level of 8–9% replaced with SSA in the
range from 10 to 30%, completely lacks resistance to aggressive external
environments associated with the presence of sulphate ions.
The test results of cementitious binders obtained and the properties
of mortars containing sewage sludge ash will allow for further research,
also carried out on a technical scale, on the properties of concretes
containing the addition of this waste material.
CRediT authorship contribution statement
Tomasz Zdeb: Conceptualization, Methodology, Writing – original
draft, Visualization, Funding acquisition. Tomasz Tracz: Data curation,
Validation, Supervision. Marcin Adamczyk: Visualization, Investiga­
tion, Writing – review & editing.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgements
The research presented in this article was carried out in collaboration
of the Cracow University of Technology and Cracow Waterworks in
Poland as a part of the POIR.04.01.02-00-0032/17 project financed by
The National Centre for Research and Development.
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