Waste Management 146 (2022) 44–52

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Waste Management
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Characterization and comparison of gasification and incineration fly ashes

generated from municipal solid waste in Singapore
Junde Qin a, b, Yunhui Zhang a, c, Stephan Heberlein b, d, Grzegorz Lisak a, b, Yaolin Yi a, *
a
School of Civil and Environmental Engineering, Nanyang Technological University, 639798 Singapore, Singapore
b
Nanyang Environment & Water Research Institute, Nanyang Technological University, 639798 Singapore, Singapore
c
College of Environmental Science and Engineering, Tongji University, Shanghai 200092, China
d
Faculty of Science and Engineering, Åbo Akademi University, 20500 Turku, Finland

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

Keywords: Slagging-gasification has received increasing attention as a municipal solid waste treatment technology.
Municipal solid waste Compared with incineration, slagging-gasification can produce valuable syngas and generates by-products that
Gasification can be easier reusable in different applications in some cases. Among these by-products, the gasification fly ash
Fly ash
(GFA) is the only hazardous solid residue to be landfilled. To explore its potential recycling methods and
Mineralogy
Leaching
maximize its recycling efficiency, the detailed physicochemical properties of GFA are crucial. This study con­
ducted a comprehensive characterization of six GFA samples and the results were compared with one inciner­
ation fly ash (IFA) sample and available data of IFA collected in Singapore in literature. X-ray fluorescence (XRF),
and microwave acid digestion (MAD) followed by inductively coupled plasma optical emission spectroscopy
(ICP-OES) and inductively coupled plasma mass spectroscopy (ICP-MS) were carried out to determine the
physicochemical composition of ashes. X-ray diffraction (XRD) and thermogravimetric analysis (TGA) were
applied to identify their mineralogical composition. The hazard of the material was assessed through one-stage
batch leaching tests. The results showed that the GFAs and IFA were both mainly composed of calcium com­
pounds and chloride salts. However, GFA contained higher amounts of heavy metals especially lead (Pb) and zinc
(Zn) than IFA. Zn contents in tested GFA samples were in a range of 1.4–3.0%, indicating the potential to recover
Zn. The Ca(OH)2 content in GFA samples was up to 24.1%, which could be recovered as a low-grade lime. Based
on the characteristics of GFA, a reusing method combining civil engineering utilization and resource recovery
was suggested.

1. Introduction organic contaminants such as dioxins and furans (PCDD/PCDFs) also

Municipal solid waste (MSW) has become a serious environmental
and social concern around the world owing to its increasing amount and
immature recycling technologies. Incineration is currently one of the
most widely used technologies to treat non-recyclable MSW, which can
reduce the volume of waste by 90% and the weight by 70% (Ontiveros
et al., 1989; Lam et al., 2010; Li et al., 2004; Liu et al., 2016). However,
the incineration process generates incineration bottom ash (IBA) and
hazardous incineration fly ash (IFA), which require further treatment
before final disposal or utilization. Some toxic heavy metals, such as zinc
(Zn), lead (Pb), and cadmium (Cd), volatilize during incineration and
then condense on the surface of IBA and IFA particles (Stuart and Kos­
son, 1994; Aubert et al., 2006; Quina et al., 2018). Additionally, some
exist in IFA as a result of incomplete combustion (Aubert et al., 2006).
Therefore, the treatment of IBA and IFA is still a large burden, especially
for areas with limited landfilling sites, such as Singapore. For a con­
ventional incineration plant, the heterogeneity of MSW makes it a fuel
that is difficult to control and leads to a complex system design (Arena,
2012; Consonni and Viganò, 2012). To get more valuable waste treat­
ment products other than energy and improve the quality of solid resi­
dues, gasification has been increasingly explored in MSW treatment.
Gasification is a technology to convert carbonaceous material into
gaseous fuel containing carbon monoxide (CO), hydrogen (H2), and
methane (CH4). In this process, a gasifying agent (air, oxygen, or steam)
is used to partially oxidize the waste to produce a combustible gas, so-
called syngas (Arena, 2012). Compared with direct waste combustion,

* Corresponding author.
E-mail address: yiyaolin@ntu.edu.sg (Y. Yi).

https://doi.org/10.1016/j.wasman.2022.04.041
Received 4 February 2022; Received in revised form 5 April 2022; Accepted 28 April 2022
Available online 11 May 2022
0956-053X/© 2022 Elsevier Ltd. All rights reserved.
J. Qin et al. Waste Management 146 (2022) 44–52

there is a potential to utilize syngas for advanced power generation or slagging-gasification generates slag, metal alloy, and gasification fly ash
chemical synthesis (Young, 2010; Arena, 2012). Slagging-gasification (GFA) instead of IBA and IFA from incineration (Tanigaki et al., 2012).
(or called gasification-melting) could also optimize the composition of Among these residues, the slag can be applied as construction material
solid residues. Applying a high temperature that could melt most MSW, without additional treatment, and the alloy granulates can be used for

Fig. 1. The process of MSW slagging-gasification (a) and conventional MSW incineration (b).

45
J. Qin et al.
metal recovery (Tanigaki et al., 2012; Heberlein et al., 2022), while GFA
is the only solid residue that is not reused at present.
However, studies on GFA are still very limited. Gómez-Barea et al.
(2009) studied the GFA produced from specific waste including orujillo
(a waste of the olive oil industry) or meat and bone meal instead of
MSW. Some studies mentioned the effect of the gasification process on
the distribution of metals in solid residues. For example, Jung et al.
(2005) raised that the distribution of metals in slag and GFA depends on
the boiling points of metals and Tanigaki et al. (2012) demonstrated that
most Zn and Pb concentrate in GFA while most Cu and Fe are highly
enriched in metal granulates. However, most studies regarding waste
gasification mainly focus on the optimization of the gasification process
and the syngas product quality. Therefore, a detailed characterization
study of GFA is necessary to explore the potential recycling and reuse of
GFA.
This study aims to better understand the nature of GFA and further
explore its potential recycling and reuse methods. The physical and
chemical properties, mineralogical composition, and leaching behaviors
of six GFA samples collected from a pilot slagging-gasification plant in
Singapore were characterized in detail. Through a comparison with
conventional IFA, the characteristics of GFA were analyzed and dis­
cussed, and suggestions to recycle and reuse GFA were given.
2. Materials and methods
2.1. Generation and collection of GFA and IFA samples
Six GFAs and one IFA were used in this study, denoted as GFA1-6 and
IFA. GFA samples in this study were all collected from the Waste-to-
Energy Research Facility (WTERF) at Tuas South in Singapore. The
WTERF is a slagging-gasification plant that continually runs to treat
waste collected from a university campus, and the treatment process of
the WTERF is illustrated in Fig. 1a. The main compositions of the
collected waste are food residue (23%), plastic waste (22%), paper
(19%), horticultural waste (9%), wood waste (5%), and textile (4%)
(Chan et al., 2019). The collected waste is first shredded and then fed
into the gasification and direct melting furnace with biomass charcoal
and limestone. Biomass charcoal in this plant is produced from
carbonized sawdust. The replacement of conventional coal coke with
biomass charcoal as the auxiliary fuel reduced the emission of SO2 by
78% (Heberlein et al., 2022). The added limestone is gravel with a
diameter of 2–6 mm. For each hour, around 480 kg of shredded MSW
and 50 kg of biomass charcoal were fed into the furnace and the amount
of limestone is 0–10 kg depending on the composition of waste. Two sets
of tuyeres are set at different parts of the furnace. The higher set of tu­
yeres inject ambient air for gasification and maintain the temperature
above the fixed bed. It is the main part of the gasification reaction, and
the temperature is maintained at around 600–800 ◦ C. The lower set of
tuyeres inject oxygen-enriched air for the melting process. The tem­
perature at bottom of the furnace can reach 1600–2000 ◦ C which is
much higher than the operating temperatures in conventional inciner­
ation plants, promoting the volatilization of metals such as Pb, Zn, and
Cd with low boiling points. Most ashes from MSW were melted and
collected as slag at this high temperature. Metal alloys with high iron
content (61.5 ± 5.5% iron content) (Heberlein et al., 2022) could be
separated from the slag with magnetic separation. The syngas produced
in the furnace is then burned in the secondary combustion chamber at a
temperature of around 800–1000 ◦ C to generate steam which is used to
produce electricity in a steam turbine. The flue gas temperature from the
boiler is around 300–350 ◦ C. After the cyclonic separation, the flue gas is
cooled down to around 170 ◦ C and a flue gas sorbent that is composed of
96 wt% slaked lime and 4 wt% activated carbon was injected. The
amount of injected sorbent is around 8.8 ± 4.5 kg per hour depending on
the current measured emissions of SO2 and HCl at the stack. Ashes from
the secondary combustion chamber, the boiler, the cyclone separator,
the gas cooling tower, and the bag filter with a flexible container are
46
Waste Management 146 (2022) 44–52
transported with a conveyor into bulk bags. The mixed ash in the big
bags constitutes GFA used in this study. The GFA is collected from the
bulk bags, mixed, and sealed in two layers of plastic bags for storage. The
GFA represents all the slagging-gasification solid residue that is not re-
used and to be landfilled. In this study, six GFA samples were
randomly collected from the WTERF on different days from September
2019 to March 2021 between 9 am to 10 am, and all the samples are
generated under the same operating conditions. Corresponding to 11.5 t
MSW treated per day, 1.2 t biomass charcoal is consumed and 1.12 t slag
(excluding metals), 0.22 t metals, and 0.43 t GFA could be generated per
day.
For comparison, IFA collected from the air pollution control (APC)
unit of an incineration plant in Singapore was used, and the process of
the incineration plant is shown in Fig. 1b. In this study, GFAs and IFA
samples were collected from plants directly and sealed in two layers of
plastic bags for storage. After collection, GFA/IFA was freeze-dried for
72 h before characterization tests. The water contents were also deter­
mined through freeze-drying.
2.2. Physicochemical properties and mineralogical characteristics
A series of experiments were conducted to determine the physico­
chemical properties of GFA and IFA samples. A Malvern Mastersizer
2000 particle size analyzer was applied to determine the particle size
distributions. The chemical compositions of GFA/IFA samples were
determined by X-ray fluorescence (XRF) and microwave acid digestion
followed by ICP-OES. XRF was conducted with a Bruker S8 Tiger X-ray
fluorescence spectrometer. The microwave acid digestion was carried
out by digesting 250 mg of ash samples with 12 mL of a concentrated
HCl (30%) and HNO3 (70%) (v/v = 1/3) mixed solution in the digestion
vessel for 20 min following EPA 3051A. The mixture was then heated in
the microwave oven at a temperature of 175 ◦ C and under high pressure
of 30 bars, and the final solution was diluted with distilled water and
filtered for ICP-OES/MS test to measure trace element concentration.
PerkinElmer Optima 8300 ICP-OES and PerkinElmer Elan DRC-e ICP-MS
were applied to determine the concentrations of selected elements and
three repeated measurements were done for each sample.
X-ray diffraction (XRD) test and thermogravimetric analysis (TGA)
were carried out to determine the mineralogical composition. Crystal­
line minerals were firstly identified by a Bruker D8 X-ray diffractometer
with a Cu Kα source at a rate of 3◦ 2-theta per minute. The accelerating
voltage of the test was 40 kV and the current intensity was 40 mA. TGA
and derivative of thermogravimetry analysis (DTG) were then applied to
estimate the content of different compositions. The test was conducted
with PerkinElmer TGA 4000 from 30 ◦ C to 900 ◦ C with a heating rate of
10 ◦ C/min in an air environment.
2.3. Leaching test
Leaching tests were conducted according to EN 12457–2 to evaluate
the metal leachability. A total of 90 g of dry samples was mixed with
900 mL of distilled water was mixed in a 2 L polypropylene plastic
bottle. After the rotation for 24 (±0.5) hours at a speed of 7 rpm, the pH
value of the mixture was determined, and the leachate was filtered with
a 0.45 μm filter. The leached heavy metal concentrations were then
determined by ICP-OES and ICP-MS. The leached Cl− and SO2− 4 con­
centrations were measured through an ion chromatography (IC) test
with a Dionex ICS-1000. Dissolved organic carbon (DOC) in the leachate
was determined by a Shimadzu TOC-L analyzer.
3. Result analysis
3.1. Appearance and particle size distribution
Pictures of GFA and IFA samples used in this study are shown in
Fig. S1 in the supporting information. GFA2, GFA3, and GFA4 were
J. Qin et al.
light brown while other samples were gray or light gray. It should be
caused by the relatively high iron content in GFA2-4. The water content
of IFA samples (12.52%) was relatively higher compared with GFA
samples (0.39%, 0.52%, 1.85%, 1.02%, 1.64%, and 0.81%). Hamernik
and Frantz (1991) reported that IFA tended to absorb water from the
environment and Goh et al. (2003) raised that the weather of collection
may affect the water content of IFA. According to previous studies
regarding IFA in Singapore, moisture contents of IFA were distributed in
a large range from 0.19% to 19.52% (Goh et al., 2003; Yin et al., 2018).
The GFA particles tended to agglomerate together loosely despite their
low water contents. Fig. 2 showed the particle size distribution of ash
samples. Particle size distributions of GFA samples were similar. For all
GFA samples, 80% of GFA particle size was below 40 μm, and median
values were between 13.9 and 20.4 μm. IFA had a larger median size of
158.5 μm. Through previous studies, the mean particle size of IFA in
Singapore was usually below 50 μm (Goh et al., 2003, Wu and Ting,
2006, Liu et al., 2016). The larger particle size of IFA in this study may
be due to the carbonation reaction induced by the relatively higher
water content. In a wet environment, fly ash particles may bind together
and form larger particles due to the reaction between the remaining lime
and CO2 in the environment.
3.2. Bulk chemical characterization
Table 1 presents the chemical compositions of GFAs and IFA from the
XRF test. Goh et al. (2003) measured the chemical compositions of 44
IFA samples collected from the incineration plant in Singapore at
different times of the year, and the results were also listed for compar­
ison. Due to the high chlorine (Cl) content in GFA/IFA, the XRF result
was presented in element form instead of oxide form, and elements with
low content (<0.5% in all samples) were not included. For GFAs and IFA
used in this study, Ca, Cl, O, Na, and K were the five main elements that
account for around 85% of the total weight. Attributed to the slaked lime
added to the air pollution control system, the Ca contents of tested
samples were high, which ranged from 16.1% to 40.2%. The relatively
low Ca contents in GFA3 and GFA4 might be due to the varying dust
amounts produced from MSW which led to different dust to flue gas
sorbent ratios in the fly ashes. The high Cl content is regarded as a
characteristic for MSW thermal treatment fly ashes, and 40–50% of Cl is
from PVC (Li et al., 2004). For GFA/IFA generated in Singapore, Cl from
food could not be ignored since food accounts for a large proportion of
incinerated waste (0.6 million tons in 2.62 million tons) (MSE, 2021).
Fig. 2. Particle size distributions of GFAs and IFA.
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Waste Management 146 (2022) 44–52
Na and K were also detected through XRF, which together accounted for
around 8–23% of the total weight. The contents of Na and K in GFA
samples were slightly higher than those of IFA. Zn and Pb were two
concerned heavy metals in waste incineration residues. It is shown that
the Zn contents ranged from 1.4% to 3.0% in GFA samples, suggesting a
high potential for zinc recovery, which is an expensive metal. As for the
IFA sample, the zinc content was much lower at 0.6% (0.3–1.4% in Goh
et al. (2003)). Pb contents in GFA1 and GFA2 were 0.5% and 0.4%,
slightly higher than other samples. There was no significant difference in
the content of other elements, i.e., S, Si, Al, P, and Mg. Particularly, Fe
contents in GFA2, GFA3, and GFA4 were relatively higher than other ash
samples, explaining the light brown color of these three samples
(Fig. S1).
Table 2 presents the trace element contents determined through
microwave acid digestion. Compared with other heavy metals, the high
Zn content was notable, especially for GFAs. After microwave acid
digestion, 9240 to 23200 mg/kg of Zn were extracted from GFAs, much
higher than that of IFA (3090 mg/kg). Consistent with the XRF result,
the Pb contents in different samples varied. GFA1 and GFA2 contained
higher Pb than other samples, which were measured to be 2750 and
1815 mg/kg, respectively. The IFA sample was determined to contain
the lowest amount of Pb (488 mg/kg). According to EUR-Lex (2008),
lead compound and zinc compound were classified as aquatic chronic 1
(H410) substance. The sum of lead compound content and zinc com­
pound content in GFAs multiped by 100 was likely to exceed the limit
concentration of 25%, and GFA should be classified as ecotoxic waste
(HP14) (EUR-Lex, 2007). For all samples, the contents of Cu and Mn
were in a range of 200–1200 mg/kg and the contents in GFAs were
slightly higher than that in IFA. Ti contents in GFAs were between 500
and 1300 mg/kg and Ba contents in GFA were between 300 and 800 mg/
kg, which were close to the contents in IFA. Hg and concentrations in all
samples were below the lowest detection limit (10 mg/kg) in this study,
which is because the product containing Hg is strictly limited in
Singapore. In total, GFA contained higher amounts of heavy metals than
IFA, which also indicated that heavy metals in MSW were better
concentrated in fly ash through slagging-gasification compared with
direct combustion (incineration). The contents of heavy metals in IFA/
GFA mainly depend on the volatilization of heavy metals (Jung et al.,
2005). Comparing the boiling points of heavy metals and their oxides/
chlorides, the relationship between concentrations of heavy metals in fly
ash and the treatment condition could be roughly explained. According
to the study by Jung et al. (2005), the reducing atmosphere promotes the
J. Qin et al. Waste Management 146 (2022) 44–52

Table 1
Chemical compositions of GFAs and IFAs (%).
GFA1 GFA2 GFA3 GFA4 GFA5 GFA6 GFA mean value IFA IFA (Goh et al. 2003)
and Mean value (Range)
standard error

Ca 29.9 ± 2.92 36.7 ± 0.42 19.7 ± 1.78 17.6 ± 0.91 35.1 ± 1.51 42.3 ± 1.92 30.2 ± 9.32 33.2 ± 0.70 30.2 (21.6–35.8)
Cl 24.3 ± 1.41 14.0 ± 1.10 23.8 ± 0.08 20.2 ± 2.18 19.1 ± 0.85 13.3 ± 0.38 21.2 ± 4.60 25.4 ± 0.19 NM
O 22.9 ± 0.42 27.7 ± 0.40 25.8 ± 0.64 25.5 ± 0.56 24.5 ± 0.58 26.4 ± 0.1 23.2 ± 4.40 24.2 ± 0.30 NM
Na 6.8 ± 1.78 4.3 ± 0.42 9.4 ± 2.10 11.7 ± 2.90 6.8 ± 1.37 5.1 ± 1.50 7.3 ± 3.02 4.16 ± 0.56 2.9 (1.7–5.9)
K 5.1 ± 0.23 3.2 ± 0.49 7.6 ± 0.79 9.2 ± 0.17 6.0 ± 0.30 3.6 ± 0.68 5.8 ± 2.23 3.7 ± 0.13 4.3 (2.5–8.9)
Zn 3.3 ± 0.22 2.2 ± 0.13 1.8 ± 0.19 2.2 ± 0.17 2.0 ± 0.16 1.5 ± 0.12 2.2 ± 0.56 0.6 ± 0.04 0.8 (0.3–1.4)
S 1.9 ± 0.02 2.7 ± 0.09 3.4 ± 0.03 1.2 ± 0.12 1.8 ± 0.06 1.6 ± 0.05 2.5 ± 0.80 2.4 ± 0.05 NM
Si 1.3 ± 0.03 2.4 ± 0.18 2.7 ± 0.07 2.5 ± 0.24 1.2 ± 0.09 1.6 ± 0.15 1.9 ± 0.65 1.7 ± 0.10 2.5 (1.1–4.9)
Fe 1.0 ± 0.11 2.0 ± 0.20 2.0 ± 0.19 2.4 ± 0.25 1.3 ± 0.15 1.4 ± 0.18 1.7 ± 0.53 0.7 ± 0.04 0.6% (0.3–1.8)
Al 0.7 ± 0.01 1.2 ± 0.09 1.0 ± 0.03 1.2 ± 0.12 0.5 ± 0.03 0.8 ± 0.06 0.9 ± 0.28 1.4 ± 0.09 1.5% (0.8–3.1)
Pb 0.6 ± 0.04 0.6 ± 0.11 0.1 ± 0.02 0.2 ± 0.03 0.1 ± 0.02 0.3 ± 0.05 0.3 ± 0.21 0.1 ± 0.02 0.3% (0.2–0.6)
Ti 0.3 ± 0.01 0.8 ± 0.01 0.5 ± 0.02 0.6 ± 0.01 0.2 ± 0.01 0.5 ± 0.01 0.5 ± 0.18 0.5 ± 0.01 NM
Mg 0.7 ± 0.10 0.9 ± 0.07 0.7 ± 0.02 0.8 ± 0.14 0.5 ± 0.01 0.8 ± 0.02 0.7 ± 0.14 0.9 ± 0.04 1.0% (0.5–1.3)
P 0.4 ± 0.04 0.6 ± 0.01 1.0 ± 0.03 0.7 ± 0.15 0.4 ± 0.01 0.4 + 0.01 0.6 ± 0.21 0.4 ± 0.02 NM

NM: Not mentioned.

minerals were different. Calcium compounds, such as CaCO3, Ca(OH)2,

Table 2
and CaSO4, were all detected in GFAs and IFA. According to XRF results,
Acid digestion results of GFAs and IFA (unit: mg/kg).
GFA3 and GFA4 contained lower amounts of Ca compared with other
GFA1 GFA2 GFA3 GFA4 GFA5 GFA6 IFA samples, leading to the lower intensities of peaks representing Ca
Zn 23200 15700 12100 18400 14900 9240 3090 compounds in XRD patterns. For IFA, intensities of CaCO3 peaks were
± 259 ± 84 ± 257 ± 171 ± 130 ± 217 ± 25 higher, while peaks representing Ca(OH)2 were more noticeable in
Pb 2750 ± 3150 619 ± 1120 ± 572 ± 1100 488
patterns of GFA. Ca(OH)Cl was detected in samples except for GFA3 and
3.7 ± 21.3 5.0 10.9 0.5 ± 8.3 ± 0.7
Cu 906 ± 766 ± 980 ± 1180 ± 646 ± 664 ± 309
GFA4, it was a characteristic calcium compound reported to exist in IFA
3.4 11.3 12.2 7.9 2.3 14.6 ± 0.9 (Bodénan and Deniard, 2003), which formed due to the reaction of
Ni 26.5 ± 38.4 ± 56.7 ± 68.5 ± 32.0 ± 55.2 56.2 excess lime with HCl in the flue gas. Bodénan and Deniard (2003)
0.1 0.0 0.3 1.0 0.2 ± 0.2 ± 0.6 pointed out that the reaction condition of solid–gas interaction leads to
Cr 99.7 ± 129 ± 205 ± 227 ± 103 ± 121 ± 76.5
less completed neutralization, and therefore Ca(OH)Cl became the final
0.8 0.6 0.8 1.8 1.3 1.8 ± 0.5
Cd 190 ± 51.4 ± 42.3 ± 52.9 ± 24.2 ± 23.6 76.2 product rather than CaCl2. In addition to these calcium compounds,
0.2 0.5 1.8 1.1 0.2 ± 0.3 ± 0.4 NaCl and KCl could be both detected in GFA and IFA. Similar to con­
Mn 252 ± 385 ± 1010 ± 1030 ± 437 ± 654 ± 243 ventional IFA, CaCO3, Ca(OH)Cl, NaCl and KCl were the main mineral
2.2 3.2 16.6 6.4 2.5 4.7 ± 2.0
components in GFAs, while Ca(OH)2 content in GFA was much higher.
As 17.2 ± 14.0 ± 10.6 ± 14.4 ± 14.4 ± 18.8 15.2
2.6 6.2 1.2 3.4 4.2 ± 7.3 ± 8.0
Mo 3.4 ± 4.3 ± 4.4 ± 6.4 ± 2.3 ± 3.0 ± 5.8 ±
0.2 0.4 0.4 0.2 0.1 0.2 0.2 3.4. TGA
Ti 1210 ± 990 ± 924 ± 536 ± 1090 ± 1150 913
10.0 4.0 4.0 1.8 9.8 ± 11.6 ± 4.8 TGA/DTG curves of tested samples are presented in Fig. 4. The
Ba 602 ± 545 ± 639 ± 764 ± 383 ± 512 ± 661
weight loss between 30 and 200 ◦ C was related to the loss of bounded
4.4 1.7 2.6 1.8 3.3 4.6 ± 3.3
Sb 193 ± 106 ± 65.4 ± 88.6 ± 43.6 ± 24.6 143 water and occurred in all samples. The presence of Ca(OH)2 at
4.7 1.6 1.1 0.6 1.4 ± 0.7 ± 6.3 380–460 ◦ C (Bodénan and Deniard, 2003Collier, 2016) was confirmed
Sr 149 ± 164 ± 160 ± 167 ± 140 ± 154 ± 179 in GFA but not evident for IFA, agreeing with the inference from XRD
0.8 0.3 0.4 0.1 0.7 0.9 ± 0.3
results. The weight loss between 465 and 600 ◦ C corresponded to the
Se 30.0 ± 27.2 ± 20.6 ± 20.2 ± 15.0 ± 6.5 ± 14.5
0.8 0.6 0.3 0.3 0.4 0.3 ± 0.4
destruction of oxychlorination phases (Bodénan and Deniard, 2003),
Hg <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 proving the existence of Ca(OH)Cl in GFA and IFA. The decomposition of
CaCO3 was identified in the range of 600 ◦ C to 800 ◦ C (Bodénan and
Deniard, 2003; Collier, 2016) for all samples. This result is consistent
volatilization of Zn in MSW; the boiling point of Zn is 907 ◦ C while for with the findings from XRD that CaCO3, Ca(OH)2, and Ca(OH)Cl were
ZnO it is 2360 ◦ C. The boiling points of Pb and PbO are 1749 ◦ C and the three mineral contents in GFA. NaCl and KCl were not detected in the
1470 ◦ C, respectively), and the high temperature in the gasification TGA test due to their high destruction temperature. Based on the weight
furnace promotes the concentration of Pb in fly ash. Jung et al. (2005) loss at corresponding temperatures, the Ca(OH)2 and CaCO3 contents in
also pointed out that Cl in feedstock increased Pb and Cu contents in fly IFA and GFA could be estimated as listed in Table S1 in the supple­
ash since the boiling points of PbCl2 and CuCl2 950 ◦ C and is 993 ◦ C, mentary information. Except for GFA4, CaCO3 contents in other
respectively. The Zn and Pb contents determined by microwave acid samples were around 20%, which formed through the reaction between
digestion were relatively lower than those detected by XRF. Due to the lime in the air pollution control system and CO2 contained in the flue
banning of hydrofluoric acid in the laboratory, metal in the form of gas. The Ca(OH)2 contents varied in different batches of GFA. In GFA6,
silicates or wrapped in silicates could not be digested, which may cause the Ca(OH)2 reached 24.1%. But in GFA3 and GFA4, Ca(OH)2 contents
differences in results. The variances between specific samples may also were low at around 1.0%, which is closed to the IFA sample. The lower
affect the results. CaCO3 and Ca(OH)2 contents in GFA3 and GFA4 are consistent with
their lower Ca contents in the XRF result. Through TGA results, it should
3.3. XRD be noted that the specific contents of different calcium compounds in
different samples vary a lot. It is due to the difference in the composition
From the XRD patterns of GFAs and IFA in Fig. 3, the minerals of the exhaust gas (including HCl, CO2, and SO2) at different times.
detected in GFAs and IFA were similar, but the peak intensities of some Identification of the contents of different calcium compounds for a

48
J. Qin et al.
Fig. 3. XRD patterns of GFAs and IFA.
specific batch of GFA is important before its recycling.
3.5. Leaching analysis
The leaching results of GFA and IFA samples with distilled water
were listed in Table 3. The results revealed that, compared with the acid
digestion results, only a small amount of heavy metal leached out during
water leaching. The condition during leaching is one of the main factors
determining the leached concentrations. Despite the difference in the
content of calcium compounds, the pH values of GFA leachates were all
between 12.2 and 12.5, close to the pH of saturated lime, and the
alkaline condition limits the leaching of heavy metals. The leaching of
heavy metals is greatly affected by the pH value. For example, the op­
timum pH to immobilize Pb is around 9.5 (Li and Yi, 2019; Wilk, 1997),
and the leached Pb concentrations from GFA1 and GFA2 were higher
compared with other GFA samples because of their relatively high pH
values. In addition to pH, the presence of other ions also influences the
leaching of heavy metals. The leached Zn concentrations from all GFA/
IFA samples were around 20 mg/kg. For conventional IFA, Jiao et al.
(2016) detected CaZn(OH)6⋅2H2O in washed IFA and ZnCl2 mixture and
raised that CaZn(OH)6⋅2H2O was the probably Zn precipitation product
during the distilled water leaching of IFA. The XRD pattern of water
washed GFA in Fig.S3 indicates that CaZn(OH)6⋅2H2O is the product of
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Waste Management 146 (2022) 44–52
water leaching of GFA and this result suggests that excess Ca in GFA
limits the leaching of Zn. For Cl− in GFA, it mainly exists in the form of
soluble chlorides, the leached Cl− concentrations are closed to the total
Cl content estimated through XRF tests. According to EUR-Lex (2003)
for the acceptance of waste in landfill, leached Pb and Se concentrations
from GFAs and IFA all highly exceeded the non-hazardous values.
Leaching concentrations of Zn from GFAs and IFA were below the non-
hazardous standard but exceed the inert value. For part of the GFA
samples, leached Ni and Mo concentrations exceeded the inert values.
The results Proper treatments have to be conducted before applying
GFA/IFA in other fields, such as construction engineering.
4. Discussions
Similar to IFA, GFA contained a high amount of Ca and Cl. Mean­
while, GFA contained higher content of heavy metals than conventional
IFA. Considering differences and commonalities and referring to current
studies on IFA application, recommendations for recycling and reuse
GFA could be given.
Metal recovery, especially Zn recovery from IFA, receives plenty of
attention in recent years (Schlumberger et al., 2007, Quina et al., 2018).
Containing even higher contents of Zn and Pb, GFA is also a potential
material for heavy metal recovery. According to the characterization
J. Qin et al. Waste Management 146 (2022) 44–52

Fig. 4. TGA and DTG curves of GFAs and IFAs.

Table 3
EN 12457-2 leaching results of GFA and IFA (Unit: mg/kg).
GFA1 GFA2 GFA3 GFA4 GFA5 GFA6 IFA EU Non-hazardous EU Inert
Value* Value*

Pb 499 ± 9.33 326 ± 11.46 40.4 ± 0.28 77.4 ± 1.29 62.6 ± 0.34 99.0 ± 2.32 72.6 ± 1.09 10 0.5
Zn 21.7 ± 0.74 20.4 ± 1.84 25.1 ± 0.41 25.1 ± 0.23 28.6 ± 0.18 26.4 ± 0.82 21.9 ± 1.37 50 4
Cr 0.12 ± 0.01 0.96 ± 0.01 8.91 ± 0.07 6.43 ± 0.07 1.00 ± 0.01 1.05 ± 0.02 4.14 ± 0.04 10 /
Cd 0.01 ± 0.001 0.02 ± 0.002 0.01 ± 0.001 <0.01 <0.01 <0.01 <0.01 1 0.04
Cu 1.23 ± 0.097 0.22 ± 0.011 0.42 ± 0.005 0.18 ± 0.022 0.21 ± 0.006 0.07 ± 0.008 <0.01 50 2
Ni 0.53 ± 0.003 0.14 ± 0.010 0.51 ± 0.007 0.28 ± 0.004 0.05 ± 0.002 0.03 ± 0.002 0.37 ± 0.006 10 0.4
Mn <0.01 0.02 ± 0.004 0.63 ± 0.025 0.60 ± 0.015 0.62 ± 0.006 0.58 ± 0.013 <0.01 / /
As <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 2 0.5
Mo 2.42 ± 0.15 1.63 ± 0.04 0.65 ± 0.04 1.29 ± 0.08 0.40 ± 0.02 0.29 ± 0.06 0.38 ± 0.01 10 0.5
Ba 4.22 ± 0.03 2.64 ± 0.01 2.32 ± 0.01 1.77 ± 0.01 4.40 ± 0.02 7.28 ± 0.02 7.39 ± 0.25 100 20
Sb 0.01 ± 0.001 <0.01 <0.01 0.01 ± 0.002 <0.01 <0.01 <0.01 0.7 0.06
Sr 18.8 ± 0.03 25.6 ± 0.05 13.4 ± 0.01 11.7 ± 0.03 25.0 ± 0.17 32.6 ± 0.12 59.1 ± 0.31 / /
Se 3.66 ± 0.04 1.38 ± 0.07 1.72 ± 0.17 2.48 ± 0.08 1.36 ± 0.05 1.42 ± 0.07 3.34 ± 0.04 0.5 0.1
Hg <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 0.2 0.01
Cl− 235000 ± 6290 131000 ± 5940 206000 ± 6810 171000 ± 2570 153000 ± 9110 107000 ± 1360 245000 ± 2380 15,000 800
SO2−4 17800 ± 134 16100 ± 101 26400 ± 270 42800 ± 406 13200 ± 115 5540 ± 59 8610 ± 230 20,000 1000
F− <5 <5 <5 <5 <5 <5 <5 150 10
DOC 394 ± 38.8 508 ± 12.0 464 ± 16.2 557 ± 10.5 457 ± 5.8 623 ± 3.5 993 ± 19.6 800 500
pH 12.42 12.36 12.32 12.32 12.24 12.35 12.06
*
Non-hazardous value and inert value are from EUR-Lex (2003) based on one stage batch leaching (EN 12457-2) for the acceptance of waste in landfill.

results, around 9–24 kg Zn is potential to be recovered from 1 t GFA,
which is worth around 32–86 dollars (Zn price in Jan 2022 was 3600
dollars per ton (Markets insider, 2022). Okada et al. (2007) tried to
recover Zn and Pb from GFA through different chemical leaching
methods and proposed that acid extraction was more effective to extract
Pb and Zn from GFA compared with alkaline leaching and ammonia/
chloride leaching. However, Okada et al. (2007) also pointed out that
using pure acid to conduct acid extraction is too expensive for metal
recovery due to the strong alkaline of GFA. The problem of high acid
consumption can be solved by applying waste acid. For example, Zn
recovery from IFA has been realized in some European countries such as
Denmark and Switzerland. Acid flue gas scrubbing solution produced
during waste thermal treatment was recycled to extract Zn from IFA
(Schlumberger et al., 2007; Quina et al., 2018).
Through TGA results, the Ca(OH)2 content in GFA could reach 20%
in some samples, which makes it a potential civil engineering material.
Considering the high calcium content, some studies tried to use IFA to
replace cement or as a material to produce cement (Aubert et al., 2004;
Keppert and Polozhiy, 2014; Viet et al., 2020). However, the existence of
Zn and Cl will influence the strength if GFA or IFA is directly applied in
civil engineering. When applied together with Portland cement, Zn will
react with OH− and Ca2+, forming CaZn2(OH)6⋅2H2O and retarding the
formation of calcium-silicate-hydrate (C-S-H), leading to the reduction
of final strength (Roy et al., 1991; Minocha et al., 2003; Li et al., 2019).
Applied with cementitious material in civil engineering, Cl leads to
problems including the rapid setting of cement, bleeding of water during
hydration, and the corrosion of steel bars in concrete components. To
avoid the effect of Cl, water washing was usually applied as a pre-
treatment to remove chlorides in these studies. In Denmark, salts recy­
cled from IFA are suggested to be used to melt snow in winter (Quina
et al. 2018). To limit the influence of Cl, using treated GFA in coastal
areas as a filling material may be a good option. Applied in a seawater
environment, the negative effect of Cl could be reduced. Marine clay
could prevent metal leaching from IFA (Lim et al., 2004) and IFA could
improve the permeability and plastic index of clay (Goh and Tay, 1993;
Show et al., 2003), similar attempts could be made for GFA.

50
J. Qin et al. Waste Management 146 (2022) 44–52

Considering these issues, Table 4 lists some potential applications of Table 4

GFA and provides some suggestions. Zn recovery has been proved to be Suggested potential application methods for GFA.
feasible for conventional IFA and should be suitable for GFA that con­ Suggested application Advantages Difficulties to be overcame
tains a higher amount of Zn. The main difficulty of Zn recovery from method
GFA is to develop a complete process to maximize the economic benefit Zn Recovery Recover valuable Zn from Recovery efficiency;
and recovery efficiency. Referring to the current process for IFA GFA, heavy metals are Economic issue;
(Schlumberger et al., 2007; Quina et al., 2018), utilization of acid in flue removed through acid Environmental effect;
gas produced in the slagging-gasification process could be considered, extraction Variances between samples
Low graded lime Take advantage of alkali Environmental effect;
but the relationship between the amounts of GFA and flue gas should be recovery calcium compounds in Supply-demand balance;
further studied, especially considering the variations between different GFA, potential material Variances between material;
batches of GFA. Containing high amounts of Ca(OH)2 and Ca(OH)Cl, low for industry and Regulatory approval
graded lime recovery should be considered and water washing could be engineering
Filling material (with Marine clay adsorbs heavy Environmental effect;
applied to remove unwanted chlorides in GFA. A water washing test
binders and other metals in GFA, and lime in Regulatory approval; Public
with a liquid to solid ratio of 10/1 was conducted on GFA1, and the XRF, material such as GFA improves the response
XRD, and TGA results were presented in Table S2, Fig. S2, and Fig. S3, marine clay) engineering properties of
respectively. Results showed that after water washing, chlorides marine clay; Different
including NaCl and KCl could be effectively removed, and Ca(OH)Cl in wastes are combined used

GFA could be converted to Ca(OH)2 since Cl− was removed during water
washing. After washing, most chlorides were removed and low graded
lime mainly composed of CaCO3 and Ca(OH)2 could be obtained. After
proper purification, the low graded lime could be used as a raw material
to produce lime or cement for industrial or engineering applications.
After evaluating the effectiveness to adsorb acid gases (HCl and SO2), it
is also practical to recycle part of GFA to the furnace or to the flue gas at
the entry point for slaked lime and activated carbon. It could also be
applied as an activator for alkaline activated cement after suitable
treatment to remove remaining heavy metals and sulfate. Another po­
tential application is using GFA as a filling material with marine clay (Yi
et al., 2015, 2017, 2018). Proper binders such as Portland cement could
be added to enhance the strength and immobilize heavy metals in GFA.
Considering the high chlorides content, the coastal area may be suitable
for this filling material because the influence of chlorides could be
minimized. However, an assessment of the long-term environmental
effect should be conducted, and regulatory approval is also necessary.
To improve the efficiency of these application methods, a preliminary
separation such as cyclone separation and heavy medium separation
could be tried first to initially concentrate heavy metals in GFA based on
the density difference between heavy metal compounds and calcium
compounds. A preliminary cyclone separation test was conducted for
GFA1, and the equipment for the cyclone separation is presented in
Fig. S4. The Pb and Zn concentrations in different fractions of separated
GFA were assessed through an acid extraction test and the results are
listed in Table S3. 22700 mg/kg Zn and 2900 mg/kg Pb could be
extracted from the lower fraction after separation while 15300 mg/kg
Zn and 1200 mg/kg Pb could be extracted from the higher fraction. The
efficiency of the separation should be further optimized till it could
improve the overall efficiency of following processes such as metal re­
covery or lime recovery. It should be noted that the suggestions are
provided simply based on the characterization results of the GFA. To
realize the practical application, further studies are required, and issues
including the economy, the supply–demand balance, the regulatory
approval, the social response, the environmental properties, and the
environmental impact potential should all be considered.
5. Conclusions
This study conducted a comprehensive characterization of six GFAs
and one IFA collected in Singapore. As thermal treatment residues of
local municipal wastes, both GFA and IFA had a high amount of Ca and
Cl with CaCO3, Ca(OH)Cl, Ca(OH)2, CaSO4, NaCl, and KCl as main
mineral components. XRF and digestion results revealed that GFA con­
tained higher content of heavy metals than IFA, especially for Zn and Pb.
The zinc content in GFA samples was in the range of 1.4% to 3.0%,
around 2 to 6 times that of IFA. A leaching test was also carried out to
assess the leaching of heavy metals from GFA, and the results indicated
that it is not suitable to use GFA in practice before metal immobilization
or removal. Through the results of characterization, the higher heavy
metal contents in GFA make it possible for Zn and Pb recovery. TGA
results indicated that Ca(OH)2 content in GFAs was up to 24.1%, which
could be recovered and applied as a neutralizer for industrial flue gas or
used as industrial or construction materials after further purification. In
short, GFA has a high potential for reutilization in metal and lime re­
covery due to its high Ca(OH)2 and Zn content.
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.
Acknowledgment
This research is supported by the Ministry of Education, Singapore,
under its Academic Research Fund Tier 1 grant (RG139/20). The authors
appreciate the National Environment Agency (NEA), Singapore, for
providing ashes used in this study, and Nanyang Environment and Water
Research Institute (NEWRI) for its support.
Appendix A. Supplementary material
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.wasman.2022.04.041.
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