Chemosphere 226 (2019) 587e596

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Chemosphere
journal homepage: www.elsevier.com/locate/chemosphere

Using incinerated sewage sludge ash as a high-performance adsorbent

for lead removal from aqueous solutions: Performances and
mechanisms
Qiming Wang, Jiang-shan Li*, Chi Sun Poon**
Department of Civil and Environmental Engineering, The Hong Kong Polytechnic University, China

h i g h l i g h t s g r a p h i c a l a b s t r a c t

The first utilization of ISSA as a high-

performance adsorbent for Pb(II)
removal was investigated.

ISSA can remove lead effectively at a
wide initial pH range from 3.00 to
6.00.

An adsorption capacity of 62.42 mg/g
was achieved at 318 K.

The adsorption mechanisms were
elucidated.

The environmental risk of the ISSA
after adsorption was evaluated.

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

Article history: A substantial amount of ash is produced after the incineration of sewage sludge which is difficult to
Received 12 February 2019 manage. Its potential use as a cost-effective adsorbent for heavy metals is beneficial to both waste
Received in revised form management and wastewater treatment. In this study, the adsorption kinetics, isotherms as well as the
28 March 2019
factors influencing the adsorption performance were assessed through batch sorption experiments. The
Accepted 31 March 2019
Available online 1 April 2019
results show that incinerated sewage sludge ash (ISSA) was effective in adsorbing Pb(II) from aqueous
solution in a wide pH range (3.00e6.00) due to the combined contributions of ion exchange, precipi-
Handling Editor: Y Yeomin Yoon tation and complexation, which was confirmed by systematic investigation through XRD, SEM-EDX, FTIR,
XPS and a sequential extraction procedure (SEP) for Pb(II). Nonetheless, the adsorption of Pb(II) by ISSA
Keywords: would be adversely affected by high ionic strength. The sorption process was fast, and the equilibrium
Incinerated sewage sludge ash data could be well described by the Langmuir model, the maximum uptake capacity for Pb(II) increased
Lead adsorption with temperature and the calculated adsorption capacities at 298, 308 and 318 K for Pb(II) were 58.28,
Waste management 60.06 and 62.42 mg/g, respectively. These findings indicate the ISSA can be recognized as a high-
Wastewater treatment applications
performance adsorbent for Pb(II) removal in wastewater treatment applications.
© 2019 Elsevier Ltd. All rights reserved.

1. Introduction

* Corresponding author. Department of Civil and Environmental Engineering, The
Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong, China.
** Corresponding author. Department of Civil and Environmental Engineering, The
Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong, China.
E-mail addresses: qi-ming.wang@connect.polyu.hk (Q. Wang), jiangshan.li@
polyu.edu.hk (J.-s. Li), cecspoon@polyu.edu.hk (C.S. Poon).
Heavy metals pose a threat to human health and other biological
systems because of their toxicity and carcinogenicity (Kobya et al.,
2005; Peng et al., 2014). Lead (Pb) pollution in waters originated
from human activities including mining, battery manufacturing,
and other solid waste disposal, is conceivably one of the most

https://doi.org/10.1016/j.chemosphere.2019.03.193
0045-6535/© 2019 Elsevier Ltd. All rights reserved.
588 Q. Wang et al. / Chemosphere 226 (2019) 587e596
ubiquitous environmental issues and has been considered as one of
the priority pollutants in most countries (Brown et al., 1999; Cao
et al., 2009; Li et al., 2017c). It is imperative to remove Pb(II) from
polluted waters, which can be achieved by methods such as ion
exchange, chemical precipitation, evaporation, electrodialysis,
membrane filtration and adsorption (Kobya et al., 2005).
Among these methods, adsorption is an attractive option
because of its simple operation and high efficiency. However, the
extensively applied and studied adsorbents including activated
carbon and biochar are comparatively costly due to the relatively
high energy input during the material production processes.
Therefore, to find low-cost alternatives is of considerable research
and commercial interests (Inyang et al., 2012; Karunanayake et al.,
2018; Mohan and Gandhimathi, 2009). As such, industrial wastes
are among the potential alternatives since most of them can be
obtained almost free of charge (Qiu et al., 2018). Some wastes
including steel slag, coal fly ash, and red mud have been verified to
adsorb heavy metals effectively (Ahmaruzzaman, 2011; Nguyen
et al., 2018; Wang and Wu, 2006). The utilization of waste mate-
rials as adsorbents benefits not only wastewater treatment, but also
management of the waste. Therefore, exploration of waste-based
adsorbents for heavy metal removal is of crucial importance.
Incinerated sewage sludge ash (ISSA) has many similarities with
coal fly ash, which is a byproduct from the incineration process of
dewatered sewage sludge generated from sewage sludge inciner-
ation plants. Specifically, the ISSA was confirmed to be porous and
had a huge amount of pore surface areas (Pan and Tseng, 2001). The
dominant components in the ISSA are silicon oxide, aluminum
oxide, ferric oxide, calcium oxide and phosphate compounds. These
characteristics make it a potential material for the adsorption of
heavy metals in aqueous solutions. Nevertheless, most ISSAs are
landfilled even though various recycling and recovery options
including using ISSA as sintered materials, glass-ceramic, (light-
weight aerated) cementitious materials and phosphate recovery
have been investigated (Donatello and Cheeseman, 2013). To our
knowledge, little work has been done on the application of the
industry produced ISSA as an adsorbent for heavy metal removal
from wastewater. The ISSAs used in previous studies as adsorbents
were actually produced in the laboratory through heating or
combustion process of sewage sludge in a small scale, and their
characteristics were remarkably different from those generated in
real incineration plants (Bouzid et al., 2008; Pan et al., 2003).
Additionally, only the copper (Cu) adsorption capacities had been
studied by Bouzid et al. (2008) and Pan et al. (2003) and were
estimated to be 3.28e4.14 mg/g and 6.98 mg/g, respectively. Since
ISSA contains significant amounts of Fe2O3 and phosphate minerals
which are recognized to be effective in Pb(II) removal (Rajput et al.,
2017; Zhang et al., 2018), it is thus worthwhile to explore the uti-
lization of the ISSA as a value-added and low-cost adsorbent for
removing Pb(II) from wastewaters.
Additionally, ISSA itself is often rich in some heavy metals, even
though it can be regarded as a non-hazardous material (Li et al.,
2017a). Very few researchers assessed the potential environ-
mental risks associated with applying waste materials as adsor-
bents. Therefore, it is indispensable to evaluate the potential
environmental risks of the ISSA after adsorption of the metals from
the wastewater. In this study, the possible use of ISSA as an
adsorbent for Pb(II) removal from aqueous solutions was investi-
gated. Batch experiments were conducted to optimize the
adsorption process, and the adsorption mechanisms involved were
elucidated using various microstructural analytical techniques and
a sequential extraction procedure (SEP) (Li et al., 1995). To under-
stand the possible environmental impacts of using ISSA as an
adsorbent for Pb(II) removal from wastewater, the solubility char-
acteristics of various chemical species associated with the ISSA after
the adsorption process were analyzed and the toxicities of the ISSA
before and after adsorption were checked by the Toxicity Charac-
teristic Leaching Procedure (TCLP) (US EPA, 1992).
2. Materials and methods
2.1. Materials
The ISSA was collected from the Sludge Treatment Facility
T$Park in Hong Kong. Prior to the experiments, the as-received ISSA
was dried at 105  C for 24 h. Some basic physical and chemical
properties of the ISSA are present in Table 1 (Wang et al., 2018a).
The pH of the point of zero charge (pHPZC ) for the ISSA was deter-
mined by the method “trial of the 11 points” described by
Regalbuto and Robles (2004). The specific surface area was deter-
mined using a Micromeritics ASAP 2020 Accelerated Surface Area
and Porosimetry System (ASAP, 2020 Plus, Micromeritics).
All chemicals and reagents used were of analytical grade. A stock
aqueous Pb(II) solution (2000 mg/L) was prepared by dissolving
PbðNO3 Þ2 in deionized water. The desired concentration of Pb(II)
was obtained by diluting the stock solution with deionized water.
2.2. Lead adsorption
All experiments were performed by mixing 20 mL aqueous
Pb(II)-containing solution with the ISSA in a 50 mL tube and reacted
in a thermostatic shaker (HZ-9211KB, HLDKQ) at 200 rpm. Solu-
tions of 0.1 N HCl and NaOH were used for pH adjustment. The
suspensions after Pb(II) adsorption were centrifuged and filtered
through 0.45 mm glass fiber filters for the measurement of metal
concentrations by inductively coupled plasma/optical emission
spectrometry (FMX 36, SPECTROBLUE). The concentration of SO2
4
and PO3
4 were measured by ion chromatography (DIONEX
INTEGRION HPIC, Thermo Scientific) and a spectrophotometer (UV-
11, MRC) respectively.
2.2.1. Effects of pH and adsorbent dosage
To examine the pH effect on adsorption, tests were conducted by
adding 0.15 g ISSA into 20 mL Pb(II)-containing solutions (40 mg/L)
with varying pH values (2.00e6.00) at 298 K for 24 h.
The effect of ISSA dosage on adsorption were evaluated by
adding different amounts of the ISSA (0.05e1.0 g) into 20 mL Pb-
containing Pb(II) solutions (300 mg/L) with an initial pH value of
4.00 at 298 K for 24 h.
2.2.2. Adsorption kinetic
0.15 g ISSA was added into 20mL Pb(II)-containing solutions
(10e500 mg/L) with an initial pH of 4.00 and a temperature of
298 K, and samples were withdrawn at time intervals in the
following 24 h.
Table 1
Chemical and physical properties of the ISSA.
Items Value
Physical properties Density (g=cm3 ) 2.49
Specific surface area (m2 =g) a 1.83
Loss on ignition (%) 0.99
pHPZC a 8.00
Chemical composition (%): Na2O: 6.96; MgO: 2.73; Al2O3: 15.24; SiO2:
33.90; P2O5: 9.33; K2O: 2.74; CaO: 7.45;
Fe2O3: 16.42; ZnO: 0.5; CuO: 0.15; Cr2O3:
0.05; NiO: 0.02
a
This study.
 Q. Wang et al. / Chemosphere 226 (2019) 587e596
2.2.3. Adsorption isotherm
0.15 g ISSA was added into 20 mL Pb(II)-containing solutions
(0e2000 mg/L) with an initial pH of 4.00. The samples were
collected after shaking at 298, 308 and 318 K for 24 h.
2.2.4. Effect of ionic strength
Batch sorption experiments were conducted under varied
background electrolyte types (NaCl and CaCl2) and concentrations
(0.01e1.0 N) to investigate the influence of ionic strength on Pb(II)
sorption by the ISSA.
All the sorption experiments were conducted in duplicate, and
the arithmetic mean values were reported. Additional analyses
were conducted whenever two measurements showed a difference
larger than 5.0%. The kinetic and isotherm models and the calcu-
lation of thermodynamic parameters are described in the Appendix
(Text A.1).
2.3. Microstructural and chemical analysis
The solid samples were analyzed by X-ray diffraction (XRD,
RigakuSmartLab) with 2q angle ranging from 5 to 60 at 0.02
intervals to identify the crystalline phases in the samples. A
JEOLJSM-6490 scanning electron microscope equipped with energy
dispersive X-ray spectroscopy (SEM-EDX) was applied to check the
morphology and elemental distributions of the solid samples.
Fourier Transformation Infrared (FTIR, Bruker Vertex 70 Hyperion
1000) spectra were obtained to characterize the samples’ surface
functional groups. The interaction between Pb(II) and the ISSA was
probed by X-ray photoelectron spectroscopy (XPS, ESCALAB 250Xi,
Thermo Fisher) with binding energies calibrated according to the
C1s peak at 284.8 eV and a program (CasaXPS) was used to analyze
the XPS results.
Fig. 1. SEM images of the ISSA before (a) and after (b) Pb(II) adsorption (the EDX spectrum (c) and elemental mapping (d) of the Pb-ISSA).
589
2.4. Potential environmental risk evaluation
TCLP and SEP were used to study the potential environmental
risks of the ISSA after Pb(II) adsorption, the brief descriptions of
these methods are shown in Appendix (Text A.2). The solubility
characteristics of various chemical species associated with ISSA
after the adsorption process were measured as well.
3. Results and discussion
3.1. Material characterization
3.1.1. SEM-EDX
Fig. 1 displays the SEM images of the ISSA before and after Pb(II)
adsorption. The porous ISSA had very irregular shapes and the
adsorption of Pb(II) had negligible effect on the morphology of the
ISSA. But the successful sorption of Pb(II) onto ISSA was confirmed
by EDX analysis. As the content of Pb(II) on the ISSA surface
increased, the content of Ca(II) and Na(I) on the surface of the ISSA
reduced considerably, which reflected that ion exchange between
Pb(II) and Ca(II)/Na(I) ions might occur during the adsorption
process (Fig. 1(c)). The elemental mapping evidenced the adsorp-
tion of Pb(II) onto ISSA as well, but Pb(II) was unevenly distributed
on the surface. Pb(II) was closely related to phosphorus (P) and
sulfur (S) as shown in Fig. 1(d) which suggested that the Pb(II)
might have reacted with P and S compounds. Table 2 summarizes
the concentrations of dissolved sulfate and calcium ions in the
solutions after adsorption. However, phosphate was not detected in
all the solutions including the blank samples (i.e., solutions pre-
pared by adding the same amount of ISSA into DI water with an
initial pH of 4.00) which could be attributed to that CaeP in the
ISSA was transformed to AleP or PbeP compounds (confirmed by
590 Q. Wang et al. / Chemosphere 226 (2019) 587e596
Table 2
Concentrations of dissolved SO2
4 and Ca
2þ
in the solutions after Pb(II) adsorption (dosage: 7.5 g/L; contact time: 24 h; pH: 4.00; Pb(II) concentration: 0e1500 mg/L).
Initial Pb(II) concentration (mg/L) 0 50
Dissolved Ca2þ (mg/L) 26.67 33.69
Dissolved SO2
4 (mg/L) 81.68 79.38
Molar ratio of dissolved SO2
4 /adsorbed Pb(II) e 0.10
Note: N.D. ¼ not detected.
XRD). The concentration of dissolved calcium ions increased with
the adsorbed amount of Pb(II). The dissolved sulfate ions however
reduced with the increasing adsorbed amount of Pb(II), and the
molar ratio of dissolved sulfate to adsorbed Pb(II) ions increased
from 0.10 to a maximum of around 0.40. These results revealed that
both the cation exchange between Ca(II) and Pb(II) ions and the
precipitation of Pb(II) with sulfate/phosphate occurred during the
adsorption process.
3.1.2. XRD and FTIR analysis
The XRD patterns of the ISSA before and after Pb(II) adsorption
are shown in Fig. 2(a). The identified main crystallize phases in the
ISSA were quartz (SiO2 ), hematite (Fe2 O3 ), and whitlockite
(Ca9 ðMgFeÞðPO4 Þ6 PO3 ðOHÞ). After Pb(II) adsorption, quartz and
hematite remained in the ISSA. Yet the peaks of whitlockite dis-
appeared, new peaks associated with anglesite (PbSO4 ) appeared
confirming that Pb(II) had precipitated with sulfate. Besides, small
peaks of bearthite (Ca2 AlðPO4 Þ2 ðOHÞ) and lead phosphate hydrox-
ide (Pb5 ðPO4 Þ3 ðOHÞ) emerged. Thus, CaeP in the ISSA was partially
dissolved resulting in active adsorption sites associated with P for
Pb(II) precipitation. These could be the reasons for the close dis-
tributions between Pb(II) and P/S on the surface of the ISSA.
The FTIR spectra in the range of 1500e400 cm1 of the ISSA
before and after Pb(II) adsorption are shown in Fig. 2(b). A broad
band centered near 1030 cm1 was assigned to SieOeSi group and
was observed in ISSA before and after adsorption. The symmetric
stretching of PeOeP groups in the ISSA centered at 777 cm1,
which was shifted to around 775 cm1 after Pb(II) adsorption. This
showed that the Pb(II) adsorption was partially related with these
groups (Liu et al., 1997). Bands centered at 590 and 430 cm1 were
attributed to FeeO bond (Durdureanu-Angheluta et al., 2009). After
Pb(II) adsorption they were shifted to 592 and 428 cm1 . This
demonstrated that FeeO influenced the Pb(II) adsorption, which
was also confirmed by the sequential extraction experiment.
Because a substantial portion of Pb(II) was in the form of F3 (Fig. 7).
Fig. 2. XRD and FTIR spectra of the ISSA before and after Pb(II) adsorption.
100 200 300 500 800 1500
35.12 39.10 29.91 42.24 45.24 44.55
71.00 54.76 29.59 6.23 2.27 N.D.
0.23 0.29 0.38 e 0.39 0.39
It had been reported that the surface of iron oxide would be covered
with FeO groups in water, which could directly coordinate with
Pb(II) (Rajput et al., 2017).
3.1.3. XPS
Fig. 3 exhibits the typical results of XPS spectra for the ISSA
before and after Pb(II) adsorption. The wide scan spectra indicate
the presence of O, S, C, Fe, and P in both the ISSA and Pb-ISSA. No
peaks corresponding to Pb(II) were observed in the ISSA surface,
since the high-resolution spectrum of Pb4f showed no evident peak
above the noise level. However, Pb(II) peaks emerged after the
adsorption experiment with a content of around 2.2% (atomic %).
The peaks of Ca2s and Na1s were reduced significantly after Pb(II)
adsorption, again indicating that the ion exchange between Pb(II)
and Ca(II)/Na(I) played a vital role for Pb(II) adsorption by the ISSA.
The high-resolution spectrum of the ISSA after Pb(II) adsorption
showed a pair of spin-orbit-split peaks at 143.7 eV (4f5/2) and
138.9 eV (4f7/2). The O1s and S2p (Fig. 6(b) and (c)) high-resolution
spectra showed that the peak of O1s was shifted from 531.56 eV to
531.50 eV, while a new broad peak centering at 162.60 eV together
with the S2p peak shifting from 168.86 eV to 168.10 eV were
observed. The binding energy of the peaks related to O and S in the
Pb-ISSA decreased, which was due to the bonding of Pb(II) to the
oxygen atoms and thus the electron density toward the oxygen
atoms was increased.
3.2. Lead adsorption
3.2.1. Effect of initial pH
The solution pH is one of the controlling factors for the sorption
of Pb(II) since it determines both the dominant species of Pb(II) ions
in the solution and the surface properties of the adsorbent (Gao and
Wang, 2007). Fig. 4(a) shows the influence of initial pH on Pb(II)
sorption, considering the potential environmental risks, the con-
centrations of detectable leached heavy metals (Sr, Zn and Cu) were
also recorded. The Pb(II) removal rate dramatically increased from
 Q. Wang et al. / Chemosphere 226 (2019) 587e596
Fig. 3. XPS spectra of the ISSA before and after Pb(II) adsorption (a: wide scan spectra; b, c and d: high-resolution spectra of O1s, S2p and Pb4f).
31.6% to more than 99.0%, when the initial pH was increased from
2.00 to 3.00. Afterwards the Pb(II) removal rate reached a plateau.
In this study, Pb(II) was effectively removed from the Pb(II)-
containing solutions with pH values lower than the pHPZC (8.00)
because of the alkali nature of the ISSA and the strong bonding
reaction between Pb(II) and the ISSA. The final pH value was
sharply increased from around 2.72 to 5.73, when the initial pH was
increased from 2.00 to 3.00 (Table A1). Thus a great deal of Hþ in
the solution was consumed leading to less competition between
Pb(II) and Hþ for the activate adsorption sites. In addition, the re-
action between Pb(II) and ISSA was strong enough to overcome the
electrostatic repulsion since part Pb(II) precipitated with S/P com-
pounds. Similar results were obtained by Feng and Guo (2012), who
showed that the Pb(II) removal rate by NaOHeCaCl2 modified or-
ange peel was around 99.0% in the pH range of 3.50e5.50.
Milojkovic et al. (2014) also found that the optimal initial pH value
for Pb(II) adsorption by M. spicatum and its compost was around
5.50 below their pHPZC values and the authors attributed this to the
reaction of Pb(II) with the functional groups on the sorbents which
could overcome the electrostatic repulsion. Comparatively, when
ISSA was used to adsorb copper, it was sensitive to the system pH
(Donatello and Cheeseman, 2013). This study demonstrated that
the solution initial pH (3.00e6.00) would not significantly affect
Pb(II) adsorption suggesting that ISSA was a superior adsorbent for
Pb(II) removal from aqueous solution in regards of the solution
initial pH.
Only Zn(II), Sr(II) and Cu(II) were detected in the solutions after
591
Pb(II) adsorption by the ISSA. The leaching concentration of Zn(II),
Sr(II) and Cu(II) were sharply reduced from 2.16, 0.62 and 0.85 mg/L
to 0.21, 0.28 and 0.12 mg/L when the initial pH value was increased
from 2.00 to 3.00 (Fig. 4(a)). Further decreases of the metal leaching
were observed when the initial pH reached 4.00. To increase the
Pb(II) removal rate and eliminate the amount of dissolved heavy
metals, the pH value of 4.00 was selected for the removal of Pb(II)
ions by the ISSA. Compared with other sorbents ISSA can effectively
remove Pb(II) in a larger pH range (Rajput et al., 2017; Wang et al.,
2014), especially in a relatively acidic environment.
3.2.2. Effect of dosage
Fig. 4(b) depicts the effect of the ISSA dosage on the adsorption
performance of Pb(II). The Pb(II) adsorption capacity declined with
increasing ISSA dosage, and the maximum adsorption capacity was
obtained with an ISSA dosage of 2.5 g/L. Nonetheless, the Pb(II)
removal rate increased appreciably from 42.8% to 94.9% when the
ISSA dosage was increased from 2.5 to 7.5 g/L. A further increase in
the ISSA dosage from 7.5 to 10.0 g/L induced only a marginal in-
crease of Pb(II) removal rate at around 3.6%, thereafter the Pb(II)
removal rate reached a plateau. At a low ISSA dosage, the active
sites available for Pb(II) ions were effectively occupied, whereas, at
a higher ISSA dosage, the active sites were not fully utilized. The
final pH values after the adsorption reaction showed a continuous
increasing trend, but within a range of 4.00e6.00 (Table A1).
Considering both the removal rate and the utilization of the active
sites, the optimal dosage was selected as 7.5 g/L.
592 Q. Wang et al. / Chemosphere 226 (2019) 587e596

Fig. 4. Effects of (a) initial pH (dosage: 7.5 g/L; contact time: 24 h; Pb(II) concentration: 40 mg/L; temperature: 298 K), (b) dosage (contact time: 24 h; initial pH: 4.00; Pb(II)
concentration: 300 mg/L; temperature: 298 K), and (c) ionic strength (dosage: 7.5 g/L; contact time: 24 h; initial pH: 4.00; Pb(II) concentration: 300 mg/L; temperature: 298 K) on
Pb(II) removal.

Fig. 6. Adsorption isotherm of Pb(II) onto the ISSA at 298, 308 and 318 K (dosage: 7.5 g/
L; contact time: 24 h; initial pH: 4.00; Pb(II) concentration: 0e2000 mg/L).
Fig. 5. Effects of contact time on the adsorption of Pb(II) (dosage: 7.5 g/L; contact time:
0e24 h; initial pH: 4.00; Pb(II) concentration: 10e500 mg/L; temperature: 25  C).

The presence of ions leads to high ionic strength of the solutions,

which may inevitably affect the performance of the adsorption
3.2.3. Effect of ionic strength
process (Chen et al., 2010). Sensitivity of Pb(II) sorption to ionic
Heavy metal containing wastewaters derived from various in-
strength was analyzed in the Pb(II) solution as shown in Fig. 4(c).
dustries also contain diverse types of suspended solids and salts.
 Q. Wang et al. / Chemosphere 226 (2019) 587e596
Fig. 7. Leaching concentration of metal/metalloid of ISSA before and after Pb(II) adsorption evaluated by TCLP (a) and their metal speciation distribution (b).
The presence of both Na(I) and Ca(II) in the solution impeded the
Pb(II) removal by the ISSA. The increase of NaCl concentration
significantly reduced the Pb(II) removal rate from 98.2% to around
34.3% when the concentration of NaCl was increased from 0 to
0.3 mol/L. After that, the removal rate of Pb(II) stayed at around
34.0%. By contrast, CaCl2 had a stronger detrimental effect on the
Pb(II) removal rate. The Pb(II) removal rate remarkably decreased
from 98.2% to 40.6% when the CaCl2 concentration was increased
from 0 to 0.1 mol/L, and further increase of CaCl2 concentration to
1.0 mol/L would slightly lower the Pb(II) removal rate to around
28.1%.
Normally, metal uptake by the adsorbent is sensitive to the
changes in the concentration of the surrounding electrolyte if
electrostatic attraction is the dominant mechanism for metal
removal (Pehlivan et al., 2008). Therefore, the electrostatic attrac-
tion was also considered vital for Pb(II) adsorption by the ISSA.
However, irrespective of the electrolyte type and concentration (up
to 1.0 mol/L), around 30.0% Pb(II) was removed from the aqueous
solution by the ISSA which could be due to the high affinity be-
tween Pb(II) ions and the ISSA and formed stronger bonds such as
the specific inner-sphere complexation or precipitation of Pb(II)
with some anions such as phosphate or sulfate.
3.2.4. Adsorption kinetics
The sorption of Pb(II) was rapid in the first 5 min and then
slowly reached an equilibrium at 60 min (Fig. 5). The rapid increase
at the initial stage was ascribed to the sufficient vacant sites on the
surface of the ISSA and the high concentration gradient of Pb(II)
between the solution and the adsorbent. With the gradual satura-
tion of these sites, the subsequent adsorption became slower,
suggesting that the mechanism responsible for the sorption
changed. The Pb(II) removal rate (Table A2) was found to be high,
when the Pb(II) concentrations were 10, 30, 50, 200 and 300 mg/L,
at 99.2%, 99.7%, 99.9%, 97.3% and 98.2%, respectively. It dropped to
76.8% when the Pb(II) concentration was increased to 500 mg/L. On
the contrary, the adsorbed amount of Pb(II) persistently increased
with the Pb(II) concentration. This result revealed that a higher
Pb(II) concentration would promote the adsorption of Pb(II) by the
ISSA. The increase of the concentration of Pb(II) magnified the
driving force of the Pb(II) towards the active sites on the ISSA which
eventually resulted in the increase of Pb(II) adsorption amount.
Adsorption kinetic models are pivotal for assessing the practi-
cality of the process as they give invaluable insights to the rate of
the solute uptake (Bouabidi et al., 2018). Generally, the uptake of
solutes is consisted of three main processes 1) mass transfer
593
(boundary layer diffusion); 2) sorption of ions on sites, and 3)
intraparticle diffusion (Ho et al., 1996). To investigate the adsorp-
tion of Pb(II) onto the ISSA, the intraparticle diffusion model was
used to fit the kinetic data. The plot of qt versus t 1=2 did not fit well
with the linear fitting. While it could be divided into two distinct
regions with different slopes (Fig. A1). The first region with a
steeper slope at the initial stage could be regarded as an external
surface sorption of Pb(II) through boundary diffusion (Chen et al.,
2010), and the values of kint1 were in the range of 0.593e18.598
mg$g 1 $min0:5 which increased when the initial Pb(II) concen-
tration was increased (Table A3). The second region with a gentler
slope could be the inconsiderable diffusion of Pb(II) inside the ISSA
particles. However, a higher concentration could promote the
diffusion of Pb(II) into the ISSA because of the elevated kint2 values
(Table A3). Similar results were also found when using P. Americana
and modified P. Americana to adsorb Pb(II) (Wang et al., 2014).
The kinetic data of Pb(II) adsorption were also described by the
most commonly employed kinetic models, i.e., Lagergren pseudo-
first-order and pseudo-second-order models, to acquire the po-
tential influences of the different physical/chemical processes on
the adsorption rate. The poor fit (low R2 and the inconsistence
between the experiment-based and estimated qe values) made the
pseudo-first-order model inappropriate to describe the experi-
mental data. The pseudo-second-order model, on the contrary,
could well describe most of the current data (shown in Table 3).
Over all, the equilibrium time in the case of Pb(II) adsorption by
ISSA was apparently shorter than many waste materials derived
adsorbents for Pb(II) sorption (Inyang et al., 2012; Karunanayake
et al., 2018; Wang et al., 2014; Xu et al., 2014), thus it would be of
great potential for the application of ISSA in practice.
3.2.5. Adsorption isotherm
Generally, the equilibrium sorption isotherm reflects the inter-
action between the adsorbate and the sorbent, which can be
established between the adsorbed metal on the adsorbents and the
Table 3
Parameters corresponding to the pseudo-second-order kinetic model of Pb(II)
adsorption by the ISSA.
C0 (mg/L) qe (mg/g) k2 ðg=ðmg$minÞ Þ R2
200 23.13 0.04097 0.956
300 38.86 0.12697 0.999
500 46.93 0.0228 0.974
594 Q. Wang et al. / Chemosphere 226 (2019) 587e596
Table 4
Parameters corresponding to the Langmuir and Freundlich isotherm models of Pb(II) sorption by the ISSA.
Temperature (K) Langmuir
qm (mg/g) KL (L/mg) RL
298 58.23 0.128 0.004
308 60.06 0.074 0.007
318 62.42 0.121 0.004
residual metal concentration during the sorption process (Feng
et al., 2011). The sorption of Pb(II) onto the ISSA at different tem-
peratures were assessed as a function of equilibrium Pb(II) con-
centration. The experimental data and the fitted curves by
Freundlich and Langmuir models are present in Fig. 6, the esti-
mated parameters are also present in Table 4.
The qe increased with Ce until equilibrium due to the availability
of active sites at ISSA surface for the attachment of Pb(II). When the
Ce was low (<200 mg/L), the equilibrium isotherm curve was steep,
signifying a high affinity of the ISSA towards Pb(II) (Pehlivan et al.,
2008). The fit between experimental data and isotherm models
were evaluated by the R2 and the APE values. And the experimental
data were better described by the Langmuir model. Because the R2
values of Langmuir isotherm model (0.985, 0.978 and 0.969 at 298,
308, and 318 K) were larger than those for the Freundlich model
(0.822, 0.792, and 0.888 at 298, 308, and 318 K) and the APE values
for Langmuir model were smaller than that of Freundlich model.
Therefore, the adsorption of Pb(II) followed a monolayer adsorption
model on the homogeneous surface (Petrovi c et al., 2017). The
calculated RL values based on the Langmuir model were
0.004e0.007, which were in the range of 0 and 1. The n values based
on the Freundlich model were in the range of 2e10. All these
indicated that Pb(II) were adsorbed by ISSA favorably under the
studied conditions (Chen et al., 2010).
The estimated qm values for the ISSA were 58.28, 60.06, and
62.42 mg/g at 298 K, 308 K, and 318 K, respectively, which showed
an increasing trend with temperature. This denoted that the
adsorption process could be endothermic. Compared with other
adsorbents derived from waste materials (shown in Table A3), the
ISSA had a better adsorption capacity for Pb(II) from aqueous
solution.
3.2.6. Thermodynamic studies
The calculated thermodynamic parameters are given in Table 5.
The value of DH o was positive which supported that the adsorption
of Pb(II) by the ISSA was endothermic. The DGo were all less than
0 indicating the adsorption process occurred spontaneously. In
addition, the DGo value declined when the reaction temperature
increased manifesting that higher temperature could facilitate the
adsorption process. The calculated DSo was 26.56 J/mol K, this
positive value indicated the increasing randomness at the solid/
liquid interface during the adsorption of Pb(II) onto the ISSA.
3.2.7. Pb(II) removal from synthetic battery-manufacturing
wastewater
Pb(II) is commonly found in battery-manufacturing or recycling
industry wastewater with a strong acidic environment. Typically,
Table 5
Pb(II) adsorption thermodynamic parameters.
Temperature (K) DH o (kJ/mol) DGo (kJ/mol) DSo (J/mol K)
298 4.456 3.447 26.561
308 3.743
318 3.978
Freundlich
R2 APE (%) KF ðmg=gÞ=ðmg=g1=n Þ n R2 APE (%)
0.985 12.1 20.97 6.376 0.822 31.8
0.978 11.8 17.51 5.360 0.792 39.8
0.969 16.9 21.05 2.931 0.888 26.8
the Pb(II) concentration is in the range of 5.00e15.00 mg/L. In
addition, sodium, calcium and magnesium ions often coexist with
Pb(II) in such kind of wastewater (Dermentzis et al., 2012; Khalid
and Rahman, 2010; Mansoorian et al., 2014). The effectiveness of
using ISSA as an adsorbent for the removal of Pb(II) from synthetic
battery-manufacturing industry wastewater was explored and the
results are shown in Fig. A2. The presence of Na(I), Ca(II) and Mg(II)
within the concentration range of 10e100 mg/L had little effect on
the removal of Pb(II) by the ISSA. Because the final Pb(II) concen-
tration was below 0.05 mg/L in all the experiments which complied
with the lead emission standards for battery-manufacturing in-
dustry in China and the US (Environmental Protection Agency,
1986; Ministry of Environment, 2014). In addition, due to the al-
kali properties of the ISSA, the final pH of the wastewater was
increased to 6.00e6.60 which could also reduce the cost to
neutralize the wastewater pH.
3.3. Evaluation of the environmental risks of the ISSA after
adsorption
The metal leaching potential assessed by TCLP and metal
speciation distributions of the ISSA before and after Pb(II) adsorp-
tion are critical to understand their potential impact on the envi-
ronment. According to Li et al. (2017a), the ISSA in Hong Kong could
be regarded as non-hazardous material evaluated by TCLP. The ISSA
used in this study was a different batch of ISSA collected from the
same sewage sludge incineration plant in Hong Kong, the TCLP
leaching results of the ISSA before and after Pb(II) adsorption are
presented in Fig. 7(a). The metal leaching concentrations of the as-
received ISSA by TCLP were similar to the previous study, sub-
stantiating that the ISSA was non-hazardous based on TCLP. After
using the ISSA as Pb(II) adsorbent, the leaching concentrations of
most metals were comparable or lower than the as-received ISSA
except for Ba(II) and Pb(II). Particularly, the leaching concentration
of Pb(II) was increased from below the detecting limit to approxi-
mately 14.55 mg/L, exceeding the toxic limit (5 mg/L) stipulated by
TCLP and National Standard of China (GB5085.3e2007). The ISSA
after adsorption was classified as a hazardous material, which must
be properly treated before disposal (Li et al., 2017b).
The metal speciation distribution results of the ISSA before and
after adsorption are shown in Fig. 7(b), and the data are summa-
rized in Table 6. The exchangeable fraction of Sr(II) and Zn(II) were
8.3% and 0.3% respectively, which were relatively higher than the
other metals and was the reason why these two metals were
detectable during the adsorption experiment. The majority of the
metals in the original ISSA were in the forms of F3, F4 and F5, which
was in agreement with our previous study confirming their low
mobility risk (Li et al., 2017a). After adsorption, except Pb(II), the
metals became less mobile due to the increasing fraction of F3, F4
and F5 compared with the original ISSA. The distribution of Pb(II) in
the ISSA after adsorption followed the order of F3 (53.1%) > F2
(31.0%) > F1 (15.0) > F4 (0.8%) > F5 (0.1%), indicating most Pb(II) in
the ISSA was bounded with Fe/Mn oxides which could be reflected
from the FTIR results. It should be noted the Pb(II) content should
be around 57.97 mg/g according to the isotherm equilibrium data.
 Q. Wang et al. / Chemosphere 226 (2019) 587e596 595

Table 6
Metal speciation in the ISSA before and after Pb(II) adsorption.

F1 (mg/g) F2 (mg/g) F3 (mg/g) F4 (mg/g) F5 (mg/g) Sum (mg/g) TD (mg/g) Sum/TD

Pb-ISSA Ba 2.45 2.93 84.33 16.13 28.93 134.77 113.33 1.19

Cd 0.10 0.64 1.59 1.00 2.40 5.73 5.87 0.98
Cr N.D. N.D. 14.56 N.D. N.D. 14.56 57.92 0.25
Cu 0.58 22.80 240.27 9.47 166.00 439.12 468.80 0.94
Mn 0.93 15.87 139.47 0.93 19.87 177.07 133.33 1.33
Ni N.D. N.D. 10.49 N.D. 35.20 45.69 52.36 0.87
Pb 4778.67 9819.73 16828.00 242.33 24.80 31693.53 32117.33 0.99
Sr 9.26 11.49 172.13 0.60 3.47 196.95 189.93 1.04
Zn 12.11 74.83 774.53 14.60 1185.73 2061.80 2097.33 0.98
ISSA Ba 2.66 1.15 60.13 11.26 21.60 96.80 128.80 0.75
Cd 0.11 0.80 1.35 1.00 1.87 5.13 5.60 0.92
Cr N.D. N.D. 18.67 N.D. N.D. 18.67 46.67 0.40
Cu N.D. 30.27 205.87 7.73 116.80 360.67 448.00 0.81
Mn 0.64 27.36 116.35 N.D. 14.67 159.02 97.33 1.63
Ni N.D. 0.11 13.13 N.D. 29.60 42.84 56.00 0.77
Pb N.D. 2.08 10.70 0.87 N.D. 13.65 18.40 0.74
Sr 21.26 21.28 142.47 N.D. 4.00 189.01 255.20 0.74
Zn 6.82 144.42 821.33 8.93 778.93 1760.43 1984.80 0.89

Note: 1) sum ¼ F1 þ F2 þ F3 þ F4 þ F5; 2) TD: the metal content based on total digestion; 3) N.D. ¼ not detected.

Nonetheless, the Pb(II) content based on total digestion was References

32.12 mg/g, and the sum of F1 to F5 of Pb(II) was 31.69 mg/g. The
difference between the calculated Pb(II) content with the digestion
results should be attributed to the washing of the ash samples by
deionized water after Pb(II) adsorption. This indicated that around
44.0% of the adsorbed Pb(II) was poorly bonded on the surface of
the ISSA and could be removed by water. In summary, Pb-ISSA
could pose a high environmental risk, which might be mitigated
through cement-based solidification/stabilization (S/S) and recy-
cled in construction materials, such as concrete blocks (Chen et al.,
2018; Wang et al., 2018b).
4. Conclusions
This exploration provides a new insight into the management of
ISSA instead of direct landfilling or simply reused as a construction
material. The adsorption of Pb(II) by the ISSA was ionic strength
dependent and initial pH (3.00e6.00) independent. The adsorption
of Pb(II) was fast and effective. The isotherm followed the Langmuir
model, and the maximum Pb(II) adsorption capacities reached
58.28, 60.06 and 62.42 mg/g at 298, 308 and 318 K respectively,
showing an endothermic and spontaneous nature of the sorption
process. The microstructural analysis and SEP further confirmed
the possible mechanisms for the adsorption of Pb(II) by the ISSA
mainly included ion exchange, complexation and precipitation.
Nevertheless, the remaining ISSA after Pb(II) adsorption required
further treatment before its disposal. Overall, the ISSA can be used
as an effective adsorbent for Pb(II) removal in wastewaters. The
forming of ISSA into pellet to facilitate effective separation of the
ISSA from the heavy metal-laden wastewaters will be explored in
our future work to help the full-scale application of this adsorbent.
Acknowledgement
The authors would like to thank the financial supports of the
Hong Kong Research Grants Council (PolyU 152132/14E).
Appendix A. Supplementary data
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