Science of the Total Environment 795 (2021) 148468

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Science of the Total Environment

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

Perfluoroalkyl substances (PFASs) in leachate, fly ash, and bottom ash

from waste incineration plants: Implications for the environmental
release of PFAS
Shanshan Liu a,1, Shiyi Zhao a,1, Zhihong Liang b, Fei Wang a,⁎, Feiyun Sun c,⁎, Da Chen a
a
Guangdong Key Laboratory of Environmental Pollution and Health, School of Environment, Jinan University, Guangzhou 510632, China
b
The Pearl River Water Resources Research Institute, Guangzhou, Guangdong 510611, China
c
School of Civil and Environmental Engineering, Shenzhen Key Laboratory of Water Resource Application and Environmental Pollution Control, Harbin Institute of Technology, Shenzhen 518055, 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

• PFAS levels in leachate, fly ash, and bot-

tom ash produced from incineration
plants were analyzed.
• PFBA and PFBS were the predominant
PFASs in leachate samples.
• The content of PFASs in leachate was
much higher than that in fly ash and
bottom ash.

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

Article history: Perfluoroalkyl substances (PFASs) are a family of chemicals widely distributed in daily use consumer products.
Received 29 January 2021 Most of these products become municipal solid wastes (MSWs) after they have been used. In the present
Received in revised form 10 June 2021 study, we examined different types of PFASs in leachate, fly ash and bottom ash produced from three MSW incin-
Accepted 10 June 2021
eration plants in southern China. High PFAS levels were found in leachate (mean concentration 215 ng/mL, range
Available online 24 June 2021
21.4–682 ng/mL) from the incineration plants, which indicated large amounts of PFASs in the wastes leached out.
Editor: Jay Gan The average quantities of PFASs annually discharged from the leachates of the three plants were estimated to be
approximately 384 kg (Plant A), 47.3 kg (Plant B), and 2.82 kg (Plant C). Relatively lower levels of PFASs in fly ash
(mean 16.4 ng/g, range 1.46–87.6 ng/g) and bottom ash (mean 14.6 ng/g, range 3.11–77.4 ng/g) indicated that
Keywords: high-temperature incineration destroyed most of the PFASs. The wide array of PFASs concentrations in all
Perfluoroalkyl substances three matrices illustrated that some PFASs-containing industrial wastes were still entered into local MSW. In gen-
Incineration plants eral, short chain PFASs, including perfluorobutyric acid (PFBA) and perfluorobutane sulfonate (PFBS), were the
Leachate primary PFASs in leachate samples. In addition, PFOS was the predominant PFASs in fly ash samples. The results
Fly ash
showed that leachate, fly ash, and bottom ash from MSW incineration plants are important vectors of PFASs.
Bottom ash
© 2021 Elsevier B.V. All rights reserved.

1. Introduction

⁎ Corresponding authors.
Perfluoroalkyl substances (PFASs) have received increasing public
E-mail addresses: [email protected] (F. Wang), [email protected] (F. Sun). concern due to their persistence, bioaccumulation, and long-distance mi-
1
These authors contributed equally to this work. gration ability (Giesy and Kannan, 2002). Among PFASs, perfluorooctane

https://doi.org/10.1016/j.scitotenv.2021.148468
0048-9697/© 2021 Elsevier B.V. All rights reserved.
S. Liu, S. Zhao, Z. Liang et al. Science of the Total Environment 795 (2021) 148468

sulfonate (PFOS) and perfluorooctanoate (PFOA) are the most widely- products of PFASs during the incineration process. Furthermore, the
used, and are listed as persistent organic pollutants in the Stockholm amount of PFASs discharged from the leachate, fly ash and bottom ash
Convention, which calls restrict their production due to their adverse in the MSW incineration plants were estimated. This study represents
effects on the environment and organisms (UNEP, 2009; UNEP, 2018). one of the earliest studies of PFAS on the distribution and concentration
However, most PFASs have unique flame retardancy and water and oil levels in different matrices in MSW incineration plants.
resistance properties, leading to their irreplaceable use in industrial
production and consumer applications, such as mist suppressants, fire- 2. Materials & methods
fighting foams, and fabric coatings, etc. (Giesy and Kannan, 2002;
Schultz et al., 2003; Choi et al., 2019). As a result, PFAS-containing 2.1. Chemicals and materials
products have been massively produced in developing countries, including
China and India (Li et al., 2011; Sharma et al., 2016). For example, the pro- Perfluorobutanoic acid (PFBA), perfluoropentanoic acid (PFPeA),
duction of PFOA and its salts in China has increased from approximately perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA),
30 t in 2004 to approximately 90 t in 2012 (Li et al., 2015). Most of these perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA),
PFAS-containing consumer products eventually become municipal solid perfluorodecanoic acid (PFDA), perfluoroundecanoic (PFUdA),
wastes (MSWs) that are disposed into landfills or incineration plants. perfluorododecanoic acid (PFDoA), perfluorotridecanoic acid (PFTrDA),
Therefore, the investigation of their final destination (such as leachate) is perfluorotetradecanoic acid (PFTeDA), perfluorobutane sulfonate (PFBS),
of great significance for studying the environmental migration and trans- perfluorohexane sulfonate (PFHxS), perfluoroheptane sulfonate (PFHpS),
formation of PFASs. perfluorooctane sulfonate (PFOS), perflurodecatane sulfonate (PFDS),
Detection and quantification of PFASs in landfill leachate and ambi- perfluorohexylphosphonic acid (PFHxPA), perfluorooctylphosphonic
ent air have been intensively studied in recent years. In many cases in acid (PFOPA), perfluorodecylphosphonic acid (PFDPA), sodium bis
the USA, perfluoroalkyl carboxylic acids (PFCAs) have been reported (1H,1H,2H,2H-perfluorooctyl)phosphate (6:2 diPAP), sodium bis
to be the primary PFASs in landfill leachates (contributed 20–90%), (1H,1H,2H,2H-perfluorodecyl)phosphate (8:2 diPAP), and perfluoro-n-
with a concentration ranging 10–8900 ng/L (Huset et al., 2011; Allred [1,2-13C2] octanoic acid (M2PFOA), and sodium perfluoro-1-[1,2,3,4-13C4]
et al., 2015). In Canada, the total concentrations of PFCAs, perfluoroalkyl octane sulfonate (M4PFOS) were purchased from Wellington Laboratories
sulfonic acids (PFSAs), fluorotelomer acids (FTAs), and perfluorooctane (Guelph, Canada). M2PFOA was used as the recovery standard, and
sulfonamides (FOSAMs) in landfill leachates ranged from 27 to M4PFOS was used as the internal standard. Methanol (UHPLC grade)
36,000 ng/L (Benskin et al., 2012; Li et al., 2012). PFASs in landfill was purchased from Fisher Scientific (Pittsburgh, PA), and ammonium ac-
leachates from European countries were reported to be in the range of etate used to prepare the mobile phase in liquid chromatography-tandem
1–1800 ng/L, and had decreased detection frequencies and lower con- mass spectrometry (LC-MS/MS) analysis was obtained from Sigma–
centrations than in the USA and Canada (Bossi et al., 2008; Busch Aldrich (St. Louis, MO).
et al., 2010; Perkola and Sainio, 2013; Fuertes et al., 2017). PFCA and
PFSA levels in leachates from Australia were determined to be 2.2. Sampling
5700 ng/L and 1900 ng/L, respectively (Lang et al., 2016). Notably,
that extremely high levels of PFASs were detected in leachates collected Leachate (n = 26), fly ash (n = 20), and bottom ash (n = 24) sam-
from China, as high as 214,000 ng/L for PFCAs and 416,000 ng/L for ples were collected from three MSW incineration plants (referred to as
PFSAs (Yan et al., 2015). For the landfill ambient air, PFASs concentra- Plant A, Plant B, and Plant C) located in Shenzhen, China from the year
tions were nearly 2–30 times higher than in control sites, and of 2015 to 2017. Annual MSW treatment capacities in Plant A, Plant B,
fluorotelomer alcohols (FTOHs) were the dominant compounds in land- and Plant C were approximately 14,000,000 t/y, 760,000 t/y, and
fill ambient air (Ahrens et al., 2011; Weinberg et al., 2011; Vestergren 170,000 t/y, respectively. Leachate productions in Plant A, Plant B, and
et al., 2015). Plant C were approximately 2, 800 t/d, 700 t/d, and 130 t/y, respectively.
Many studies have focused on PFASs in landfill leachates (Benskin It has been estimated that the production of fly ash is 1–3 wt% and
et al., 2012), but very little data is available regarding PFASs in leachate, bottom ash is 20–25 wt% (Tian et al., 2020). Before fresh MSW was
fly ash, and bottom ash from MSW incineration plants. Some studies transferred into the incinerator, the leachate samples were collected
have been conducted to evaluate decomposition of PFASs under ther- from waste storage using polypropylene (PP) containers, and the fly
mal conditions (Ellis et al., 2001; Krusic and Roe, 2004; Chen et al., ash and bottom ash after incineration were collected with using PP
2008; Kitahara et al., 2009). Krusic and Roe (2004) investigated the bags. Considering that the water content of MSW is the most important
thermal decomposition kinetics of ammonium perfluorooctanoate factor affecting the concentrations of sample PFASs, half of the samples
(APFO) using a gas-phase nuclear magnetic resonance (NMR) tech- were collected during the rainy months (June 2016 and May 2017),
nique. The thermogravimetric analysis–differential thermal analysis and half were collected during the dry months (November 2016 and
(TGA–DTA) showed that the decomposition temperatures of PFOS and January 2017).
PFHxS were both approximately 450 °C, which were much higher
than that of FOSA and PFOA (100–150 °C) (Wang et al., 2013; Xie 2.3. Sample preparation
et al., 2013; Wang et al., 2015; Xiao et al., 2020). Furthermore, our pre-
vious studies also showed that PFASs can react with the matrices in Leachate samples were extracted using the solid phase extraction
waste and sludge to form CaF2 or Ca5(PO4)3F under thermal conditions (SPE) method by Loi et al. (2011) with minor modifications. First, the
(Wang et al., 2015). These findings indicate that different PFASs might leachate was centrifuged at 10,000 rpm for 15 min to remove large par-
have different thermal behaviors during the process of waste incinera- ticles, and 5 mL supernatant was placed into a 15 mL pre-rinsed PP tube.
tion. The temperature for waste incineration is typically greater than Ammonium hydroxide was added to adjust the pH of the supernatant to
850 °C, at which most PFASs are degraded under idle conditions. It re- 7–8, followed by adding 50 μL M2PFOA (100 ng/mL). Second, the super-
mains unclear whether PFASs can be completely decomposed during natant was extracted using Oasis WAX cartridges (60 mg, 6 cc) (Waters,
the waste incineration process, and whether PFASs can be identified in Corp., Milford, MA), which were preconditioned using 4 mL of metha-
the matrices after incineration, such as bottom ash and fly ash. nol, 4 mL of 0.1% ammonium hydroxide (in methanol), and 4 mL of
In the present study, three types of matrices (leachate, fly ash, and Milli-Q water at a rate of 1–2 drops per second prior to loading the
bottom ash) produced from three MSW incineration plants were col- leachate samples. The cartridges were then washed using 4 mL of
lected to study the levels and migration of PFASs. The TGA–DTA method 25 mM ammonium acetate buffer (pH = 4) and dried under vacuum
was used to explore the reaction mechanism and the intermediate to remove residual water. Target compounds were eluted using 4 mL

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S. Liu, S. Zhao, Z. Liang et al. Science of the Total Environment 795 (2021) 148468

of methanol and 4 mL of 0.1% ammonium hydroxide (in methanol). (n = 8), Plant B (n = 8), and Plant C (n = 10). PFAS concentrations in the
Finally, the eluate was concentrated to nearly dry under a gentle stream leachates from the incineration plants ranged from 21.4 ng/mL to
of nitrogen gas and subsequently reconstituted with methanol to a final 682 ng/mL, among which the PFAS levels in the leachate from Plant A
volume of 0.5 mL. This was filtered through a Nylon syringe filter (125–682 ng/mL) were significantly higher than those from Plant B
(0.22 μm, Anpel). The injection standard M4PFOS (50 μL, 100 ng/mL) (27.6–333 ng/mL) and Plant C (21.4–110 ng/mL) (Table 1). In Plant
was then added, and the extract was analyzed using LC-MS/MS. A, PFBS was the most abundant PFAS with a concentration of
For the fly ash and bottom ash samples, a 200 mg sample was placed 77.4–611 ng/mL (mean concentration 323 ng/mL), followed by PFBA
into a 15 mL PP tube after being lyophilized and homogenized in a (77.3 ng/mL), PFDPA (10.4 ng/mL), PFOA (8.84 ng/mL), PFHxA
solvent cleaned pestle and mortar. This was followed by adding 1 mL (8.72 ng/mL), PFPeA (7.02 ng/mL), and PFHpA (5.38 ng/mL) (Table 2).
0.1 mol/L sodium hydroxide to the digestion. After soaking for 30 min, For Plant B and Plant C, the mean contributions of PFBA (45.8% in Plant
10 mL of methanol was added, and the samples was ultrasonicated for B and 25.3% in Plant C) and PFBS (40.4% in Plant B and 22.6% in Plant
30 min at 60 °C. In addition, 100 μL of 1 mol/L of hydrochloric acid C) to PFASs were similar. In addition, PFOS (mean contribution 18.4%),
was used to neutralize the sample, and the sample was subsequently PFDPA (14.7%), PFPeA (4.04%), and PFOA (3.16%) in Plant C were detected
centrifuged at 9000 rpm for 15 min. The supernatant was transferred at higher levels. The total concentration of PFASs in leachates from the
into a new glass tube. The extraction procedure was repeated twice, MSW incineration plants showed a trend of Plant A > Plant B > Plant C.
and the final solution was concentrated to 0.5–1 mL under nitrogen. Due to the imperfect MSW classification and recycling system in
The same SPE procedure as for leachate extraction was used for fly ash China, the moisture content of MSW with complex composition is
and bottom ash samples. high (45–60%) and has a negative impact on incineration (Ren et al.,
2018). Therefore, MSW should be placed in storage for 2–10 days
2.4. PFASs determination prior to transfer into the incinerator, which will produce a large amount
of leachate (Ye et al., 2014). The different levels of PFASs among these
The concentrations of PFASs were determined using an ultra-high- plants can potentially be explained by different storage time and treat-
performance liquid chromatography system (UHPLC, Shimadzu LC-30 ment capacities. The leachate samples from MSW incineration plants
CE, Japan) equipped with a 100 × 2.1 mm ACQUITY® UPLC BEH C18 with larger MSW treatment capacities contained higher levels of
Column (1.7 um particle size) (Waters, Ireland) and coupled to an AB PFASs in this study. Moreover, with increased of storage time, more
Sciex Q TRAP 5500 mass spectrometer (CA, USA). An auto injector was PFASs will be released into the leachate. It has been reported that
used to inject 5 μL of each sample to the LC system. Column temperature MSWs after the MSWs enters into a recycling system, it consists of
was maintained at 45 °C, and a polyetheretherketones (PEEK) tube was food remnants (51.1%), plastics (14.7%), paper (8.40%), texture (6.9%),
used to replace the PTFE and fluoropolymer materials in the instru- ash (6.8%), glass (3%), tile (2.1%), and metal (1.1%), and high amounts
ments to avoid contamination from the PFTE tube. A gradient mobile of PFASs have been detected in leathers, carpets, textiles, constructions
phase of methanol (UHPLC Grade, Fischer Scientific) and 2 mmol/L am- and demolition wastes, and papers (Tai et al., 2011; Herzke et al., 2012;
monium acetate in Milli-Q water were used. At a flow rate of 0.2 mL/ Becanova et al., 2016). Furthermore, some industrial waste containing
min, the mobile phase gradient was ramped from 20% to 90% methanol PFASs (such as mist suppressants) were treated as MSWs and sent to in-
from 1 min to 4 min followed by a 2 min hold before returning to 10% in cineration plants, resulting in a higher content of PFASs in the leachate
0.1 min. The total run time of each injection was 8 min. Multiple reac- (Bjornsdotter et al., 2019). Among the three incineration plants, Plant
tion monitoring (MRM) mode was used to acquire data. The MS was A was located in an industrial development area whose wastes, particu-
equipped with a TurboIonSpry electrospray ionization (ESI) probe oper- larly industrial waste, could contain more types and contents of PFASs,
ating in negative ionization mode, and ions were detected in selective while Plant C was located in an area dominated by service industries.
ion monitoring mode according to the related parameters in Table S1. Among the PFASs in the leachates, short chain PFCAs and PFSAs
accounted for greater than 86% (Fig. 1). In addition, PFSAs contributed
2.5. Quality control and data analysis to 79% in Plant A and 63% in Plant C, which were higher than the short
chain PFCA contributions. However, the contributions of short chain
Procedural blanks were prepared at an interval of every six to eight PFCAs (49%) and PFSAs (48%) in Plant B were similar. Generally, PFCAs
samples to determine if contamination had occurred during sample ex- accounted for the majority of PFASs in the leachate from landfills be-
traction. Solvent blanks containing methanol and calibration check cause of fluorotelomer precursor degradation to PFCAs (Huset et al.,
standards were prepared to run after every eight samples to monitor 2011; Yan et al., 2015; Fuertes et al., 2017). However, compared with
the background contamination. Calibration curves were constructed landfills, a short leaching time (2–10 days) might not be sufficient for
using a series of PFAS concentrations (0.5, 1, 2, 5, 10, 20, 50, and transformation of PFCAs from precursors, which could explain the pre-
100 ng/mL). Matrix recovery tests were conducted in duplicate, and dominance of PFSAs. The low concentration of diPAPs could have been
the matrix recoveries ranged from 56 to 107% for leachate, 25–91% for due to the absence of known diPAP precursors (Allred et al., 2015).
fly ash, and 32–129% for bottom ash (Table S2). The recovery standard, Although diPAPs are likely to biologically transformed to short chain
M2PFOA, and the internal standard, M4PFOS, were separately spiked PFCAs such as PFHxA (De Silva et al., 2012), there was no significant
into three types of samples prior to extraction and detection. After
this, their concentrations were determined, and the recoveries of
M2PFOA were 82–135% for leachate, 47–170% for fly ash, and 43–124% Table 1
∑PFASs (Perfluoroalkyl substances) concentrations in leachate (ng/mL), fly ash (ng/g)
for bottom ash. The limit of detection (LOD) was determined to be three and bottom ash (ng/g) from MSW incineration plants.
times that of the signal-to-noise ratio (S/N). Statistical analysis was per-
formed using Origin and SPSS software. MSW incineration plant Matrix Mean Medium Range

A Leachate (n = 8) 409 403 125–682

3. Results and discussion Fly ash (n = 6) 33.4 17.7 7.14–87.6
Bottom ash (n = 8) 15.7 5.66 3.35–77.4
B Leachate (n = 8) 205 234 27.6–333
3.1. PFASs in leachate Fly ash (n = 7) 4.02 3.01 1.55–7.19
Bottom ash (n = 7) 10.3 7.56 3.92–23.4
A total of 21 PFASs compounds (Table S1), including short chain PFCAs C Leachate (n = 10) 67.9 71.3 21.4–110
(C ≤ 7), long chain PFCAs (C > 7), PFSAs, PFPAs and polyfluoroalkyl phos- Fly ash (n = 7) 12.7 6.35 1.46–58.6
Bottom (n = 9) 17.0 14.1 3.12–67.3
phoric acid diesters (diPAPs) were detected in the leachates from Plant A

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S. Liu, S. Zhao, Z. Liang et al. Science of the Total Environment 795 (2021) 148468

Table 2
Summary of PFASs concentrations in leachate, fly ash and bottom ash from MSW incineration plants.

Leachate (ng/mL) Fly ash (ng/g) Bottom ash (ng/g)

A B C A B C A B C

PFBA 77.3 108 32.1 4.00 1.68 4.71 3.23 4.39 15.4
PFPeA 7.02 2.98 5.12 ND ND 0.230 0.591 0.267 0.657
PFHxA 8.72 0.791 1.60 0.264 0.0396 0.178 6.82 0.142 0.156
PFHpA 5.38 1.02 2.48 0.111 0.0391 0.0781 0.347 0.5211 0.249
PFOA 8.84 3.42 4.01 1.90 1.18 0.375 1.88 ND 0.890
PFNA ND ND ND 0.441 0.111 0.268 0.243 0.403 0.330
PFDA 0.406 0.362 1.26 0.0824 0.0915 0.0218 0.0578 0.0298 0.0311
PFUdA 0.131 0.142 0.0894 0.0195 ND 0.0130 0.0790 0.0443 0.0165
PFDoA 0.371 0.704 0.642 0.0125 0.0109 0.0158 0.0944 0.121 0.0967
PFTrDA 0.156 0.138 0.144 ND 0.0272 0.0358 ND 0.0755 0.0262
PFTeDA 0.140 0.152 0.261 0.0311 0.0540 0.0525 0.0263 ND 0.0134
PFBS 323 95.4 28.7 11.6 0.0871 0.0961 2.52 0.929 0.527
PFHxS 2.05 1.43 3.64 0.120 0.0260 0.0515 0.316 0.0857 0.0949
PFHpS 0.447 0.206 1.38 0.198 0.0252 0.302 0.0933 0.0996 0.0292
PFOS 0.150 7.25 23.4 15.0 1.55 8.89 24.3 10.9 1.67
PFDS ND 0.2875 0.206 ND ND ND ND ND 0.416
PFHxPA 1.34 0.675 0.782 0.189 0.0712 0.0815 0.443 0.517 0.320
PFOPA 3.70 2.04 2.15 ND ND ND 0.459 1.19 0.371
PFDPA 10.4 10.3 18.6 ND ND ND 1.42 4.51 1.65
6:2diPAP 0.0847 0.0417 0.0494 0.00701 ND 0.0256 0.0185 0.0561 0.0409
8:2diPAP 0.283 0.323 0.267 ND ND 0.120 0.119 0.214 0.250

ND: not detected.

correlation between short chain PFCAs and diPAPs in this study of the rain, increased leachate production could have diluted the con-
(Table S3). Moreover, significant correlations (p < 0.05) were observed centration of PFASs, which was consistent with the lower PFAS concen-
between PFOPA and PFDPA (r = 0.964, p < 0.05), and 6:2 diPAP and 8:2 trations in D1(June 2016) to D2 (November 2016) and D4 (May 2017)
diPAP (r = 0.979, p < 0.05). to D3 (January 2017) in Plant B. Overall, the levels of PFASs in 2017
On average, PFBA, PFBS, and PFPeA were abundant in the leachates were lower than in 2016, which could have been related to improve-
from the MSW incineration plants (Fig. 2). In a recent study by Wang ments in MSW management in China, as well changes in MSW compo-
et al. (2020), PFBA was found to be the dominant PFASs at transfer sta- nents that accompanied economic development.
tions and incineration plants, indicating the shift to short chain alterna- A higher content of short chain PFASs was consistent with the fact
tives after restrictions on PFOS and the voluntary phase out of PFOA that short chain PFASs have higher aqueous solubility and lower
after the Stockholm Convention (Harrad et al., 2019a, 2019b). Due to sediment-water partition coefficients than long chain PFASs (Fuertes
the variability in MSWs, the extremely high PFAS levels in Plant A et al., 2017). High concentrations of PFBS could be attributed to the in-
(June 2016) could have been accidental since the MSW was mixed creasing use of sulphonamides, which have been demonstrated to
with more industrial waste containing PFASs. In addition, May and form PFBS and short chain PFCAs (D'eon et al., 2006; Fuertes et al.,
June are the rainy months in Guangdong Province. Under the influence 2017). As a replacement used in paper and textile applications, methyl
perfluorobutane sulfonamidoethanol (Me-FBSE) can degrade to methyl
perfluorobutane sulfonamidoacetic acid (Me-FBSAA), which is the most

Fig. 1. The levels of different types of PFASs (Short chain PFCAs, Long chain PFCAs, PFSAs, Fig. 2. The concentrations of different kinds of observed PFASs (PFBA, PFPeA, PFHxA,
PFPAs, and diPAPs) in leachate from three MSW incineration plants. PFHpA, PFOA, PFBS, and PFHxS) in the leachate from MSW incineration plants.

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S. Liu, S. Zhao, Z. Liang et al. Science of the Total Environment 795 (2021) 148468

abundant sulphonamide in leachate and a precursor of PFBS (Huset

et al., 2011).
The physical-chemical properties, including pH, electrical conductiv-
ity (EC), total suspend solids (TSS), total organic carbon (TOC), and
leachate temperature are other possible factors that could influence
the leaching of PFASs from MSW (Benskin et al., 2012; Gallen et al.,
2016). Remarkably, the individual PFASs congeners (PFBA, PFPA, and
PFHxA) were found to increase with increasing pH, but there were no
obvious correlations between the PFCAs and PFSAs and the physical-
chemical properties of the leachate. Different studies have shown that
the correlations between EC and PFAS concentrations can be either pos-
itive or negative, and that TOC is weakly correlated with PFAS concen-
tration (Hamid et al., 2018). In the present study, large particles were
removed from the leachate prior to extraction using centrifugation,
which potentially could have led to a lower value than the actual PFAS
amounts. In general, the physical-chemical properties of leachate can af-
fect the content of PFASs by altering the adsorption behavior and mobil-
ity of PFASs. An investigation that compares PFAS concentrations and
temperature should be conducted in the future, which would be helpful
in explaining the differences between months.

3.2. PFASs in fly ash and bottom ash Fig. 3. The levels of different types of PFASs (Short chain PFCAs, Long chain PFCAs, PFSAs,
PFPAs, and diPAPs) in fly ash and bottom ash from three MSW incineration plants.
The concentrations of PFASs in fly ash collected from Plant A (mean
33.4 ng/g), Plant B (4.02 ng/g), and Plant C (12.7 ng/g) were in the
ranges of 7.14–87.6 ng/g (n = 6), 1.55–7.19 ng/g (n = 7), and from Plant B and C were slightly higher than those in the fly ash,
1.46–58.6 ng/g (n = 7), respectively (Table 1). The total PFAS concen- while the PFASs concentration in the fly ash from Plant A was approxi-
trations in bottom ash samples collected from Plant A, Plant B, and mately two times higher than the bottom ash.
Plant C were 3.35–77.4 ng/g (n = 8), 3.92–23.4 ng/g (n = 7), and According to the TGA research of Xiao et al. (2020), PFSAs become
3.12–67.3 ng/g (n = 9), respectively. In the fly ash, PFOS (mean more thermally stable than PFCAs with increasing perfluorinated
15.0 ng/g, range 2.93–55.4 ng/g) was the most abundant PFASs in carbons (CF2), and decomposition of PFCAs requires higher tempera-
Plant A, followed by PFBS (mean 11.6 ng/g, range 0.0720–41.7 ng/g), ture. This can explain the high content of PFSAs in both the fly ash and
PFBA (mean 4.00 ng/g, range 1.25–8.42 ng/g) and PFOA (mean bottom ash in Plants A and B. With respect to Plant C, the short chain
1.90 ng/g, range 0.875–5.55 ng/g) (Table 2). PFOS (8.89 ng/g) was also PFBA (mean contribution 66.3%) was the most abundant PFAS, followed
the predominant PFAS in Plant C, followed by PFBA (4.71 ng/g) and by PFOS (7.19%). Compared to fly ash, bottom ash contained a non-
PFOA (1.18 ng/g). In addition, the PFAS concentrations in Plant B were negligible amount of PFPAs, especially in Plant B (42%), which illus-
found to be in the following order: PFBA (1.68 ng/g) > PFOS (1.55 ng/ trated that the MSWs collected in Plant B had high concentrations of
g) > PFOA (1.18 ng/g). With regard to bottom ash, PFOS was the pre- PFPAs. Some applications of PFPAs include cleaning products and fume
dominant PFAS with mean concentrations of 24.3 ng/g and 10.9 ng/g suppression in metal plating. A previous study proposed that diPAPs
in Plant A and B, respectively, while Plant C had the highest concentra- (mean concentration 7637 ng/g) represented 98% of the PFASs in indoor
tion of PFBA (15.4 ng/g). Compared with Plant A, which had high con- dust, but the levels of PFPAs were three orders of magnitude lower than
centrations of PFHxA, PFBA, PFBS, and PFOA, Plant B and C had high diPAPs (De Silva et al., 2012). In addition, the adsorption of PFPAs (resis-
concentrations of PFDPA. tant to heat) on organic matter increases with increasing perfluoroalkyl
The total concentration of PFASs showed the trend of Plant A > Plant chain length, which can explain the relatively high concentration of
C > Plant B in fly ash and Plant C > Plant A > Plant B in bottom ash, PFDPA in the bottom ash (Wang et al., 2016).
which was different from the leachate. Except for the nature of the The contents of the predominant PFASs in the fly ash (PFBA, PFHxA,
MSWs, the type of the incinerator and the combustion conditions, PFHpA, PFOA, PFBS, PFHxS, and PFOS) and bottom ash (PFBA, PFPeA,
such as time and temperature, were significant factors that influence PFHxA, PFHpA, PFOA, PFBS, PFHxS, and PFOS) on the different dates
the nature of fly ash and bottom ash, which have been shown to be cor- are shown in Figs. 4 and 5. Compared with bottom ash, the primary
related to the levels of PFAS (Dugenest et al., 1999). The Higgs grate fur- types of PFASs in fly ash from the different plants were more stable
nace of Belgium was used in Plant B and had good incineration and consisted of PFBA, PFOA, and PFOS. Except for D4, PFBS was the
efficiency, which could explain the lowest concentration of PFASs in most abundant PFAS in Plant A, and PFBA was the predominant PFAS
both the fly ash and bottom ash in Plant B. The pH of bottom ash was in Plant B and C, other than on D2. The highest concentrations of the
greater than 11.5 under high temperature in the incinerator, which major PFASs in the fly ash and bottom ash from Plant C occurred on
had an effect on PFAS extraction efficiency (Shen et al., 2010). In addi- D2 and D3, respectively. Compared with Plants B and C, the major
tion, the pH and organic matter content of bottom ash varied in MSW PFAS contents of the bottom ash in Plant A exhibited little change
compositions and incineration conditions, and their effects on the among dates. In general, the concentration of the major PFASs in Plant
PFASs in ashes require further study. C was higher than that in Plant A, which was inconsistent with previous
In the fly ash of the three incineration plants, short chain PFCAs and findings in leachate. This indicates that the variety of MSWs had a larger
PFSAs accounted for greater than 80% PFASs, and PFSAs were the pre- effect on the smaller MSWs treatment capacity of the plants. Therefore,
dominant portions in Plants A (mean contribution 80%), B (48%), and the incineration treatment efficiency of Plant C, with the smallest treat-
C (72%) (Fig. 3). In the bottom ash, except for the PFSAs (57%), short ment capacity, was more unstable. This resulted in large fluctuations in
chain PFCAs attributed to 35% of the PFASs in Plant A. In addition, the concentrations of PFASs. In addition, the contributions of other
short chain PFCAs comprised 45% of PFASs in Plant B and 86% in Plant PFASs, other than the major PFASs in Plant A, were greater.
C. In addition, PFSAs (26%) and PFPAs (24%) were also important pro- Molecular decomposition via thermal destruction and sequential
portions of the PFASs in Plant B. The PFAS levels in the bottom ash defluorination are two mechanisms involved in the destruction of

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S. Liu, S. Zhao, Z. Liang et al. Science of the Total Environment 795 (2021) 148468

Although short chain PFASs (PFBA or PFBS) were predominant in bot-

tom ash, generation from long chain PFASs was not found in thermal
treatment (Xiao et al., 2020). The thermal behavior of PFASs should be
further studied under model incinerator conditions to determine
whether intermediate substances (including short chain PFASs) will
be produced.
To specify the thermal behaviors of PFASs, a TGA-DSC was per-
formed on PFOA (one of the most common PFASs) and 8:2 FTOH
(Fig. 6). Two similar endothermic peaks occurred in the DSC profiles.
The endothermic peak that occurred at approximately 50 °C indicated
that changes were occurring in the chemicals, while the TG profiles
showed that there were no weight changes at approximately 50 °C.
These findings indicated that PFOA and 8:2 FTOH could liquefy first at
approximately 50 °C. The second endothermic peak that occurred at
approximately 130 °C was accompanied with significant weight
loss, which could illustrate that PFOA and 8:2 FTOH vaporized or
decomposed to the gas phase near 130 °C. These results were consistent
with previous studies, which proved that gasification of PFOA occurred
near 100–150 °C (Xiao et al., 2020). Based on the observed results, it can
be concluded that most PFOA and 8:2 FTOH would decompose during
the MSW incineration process.
Fig. 4. The concentrations of different kinds of observed he concentrations of different
kinds of observed PFASs (PFBA, PFHxA, PFHpA, PFOA, PFBS, PFHxS, and PFOS) in the fly 3.3. Flux estimations
ash from MSW incineration plants.

The average concentrations of perfluoroalkyl carboxylic acids

PFASs (Horst et al., 2020). Therefore, incineration treatment is an appro- (PFCAs), perfluoroalkyl sulfonic acids (PFSAs), and the sum of all
priate way to remove PFASs from MSWs. The results from Solo-Gabriele PFASs in leachates from incineration Plant A-C were calculated based
et al. (2020) showed a significant negative correlation (R2 = 0.92, p = on the daily disposal capacities of the incineration plants. The annual
0.008) between the PFAS levels in the leachates from MSW ash and in- production of leachate collected from the three target MSW incineration
cineration temperature. The concentration of PFBS in ash incinerated at plants were estimated to be approximately 937,200 t (Plant A), 231,000
815 °C was 5 ng/mL, which was higher than that incinerated at 842.5 °C
(0.35 ng/mL). The formation of PFCAs from the thermolysis of precursor
fluoropolymers was found, and the volatile precursors, such as FTOHs
and FOSA/FOSEs, were transformed to PFCAs or PFSAs (Rayne and
Forest, 2009; Haug et al., 2011). The associations between PFASs in fly
ash and bottom ash were explored using Spearman Rank correlations
(Tables S4, 5). Significant correlations (p < 0.05) were found between
PFBS and PFCAs (PFHxA, PFHpA, and PFOA), as well PFOS and short
chain PFSAs (PFBS, PFHxS, and PFHpS), which may indicate the decom-
position of PFOS to low chain PFSAs. However, correlations within the
PFCAs were less frequent. In bottom ash, PFHxS was significantly corre-
lated with PFCAs, and PFBS was negatively correlated with PFBA.

Fig. 5. The concentrations of different kinds of observed PFASs (PFBA, PFPeA, PFHxA, Fig. 6. The thermogravimetric analysis−differential thermal analysis (TGA–DTA) profiles
PFHpA, PFOA, PFBS, PFHxS, and PFOS) in the bottom ash from MSW incineration plants. of PFOA and 8:2 FTOH.

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S. Liu, S. Zhao, Z. Liang et al. Science of the Total Environment 795 (2021) 148468

t (Plant B), and 41,500 t (Plant C). Based on the fact that the yields of fly the fate and transport of PFASs in WWTP-treated leachates and the ther-
ash and bottom ash were 3 wt% and 25 wt% of the municipal wastes, re- mal behavior of PFASs in MSW incineration plants should be studied.
spectively, the production of fly ash and bottom ash could also be calcu- From an engineering perspective, techniques to remove PFASs in leach-
lated. Thus, the annual discharges of PFCAs, PFSAs, and PFASs from the ate and to destroy PFASs in incinerator should be developed.
leachate, fly ash and bottom ash for each plant could be estimated and
are shown in Table 3. CRediT authorship contribution statement
The total average quantities of PFASs discharged from the leachates
in the three plants were estimated to be approximately 384 kg/y Shanshan Liu: Methodology, Writing-original draft;
(Plant A), 47.3 kg/y (Plant B), and 2.82 kg/y (Plant C). The estimations Shiyi Zhao: Investigation, Methodology;
of PFASs in the U.S. municipal landfill (Lang et al., 2017) and the Zhihong Liang: Conceptualization, Visualization;
Canada landfill (Li et al., 2012) leachates were 563–638 kg/y and Feiyun Sun: Polishing;
66,000 kg/y, respectively, which were higher than those found in our Fei Wang: Validation, Writing-review & editing;
study. There were 70 PFASs found in their leachates, and the leachates Da Chen: Supervision.
contained large amounts of fluorotelomer carboxylic acid (FTCA) that
had existed for a long period of time in that landfill location (Lang Declaration of competing interest
et al., 2017). In addition, our results were much higher than the reported
landfill leachate in Norwegian (17 kg/y) (Knutsen et al., 2019), Canada The authors declare that they have no known competing financial
(16 kg/y) (Benskin et al., 2012), and Germany (0.049 kg/y) (Busch interests or personal relationships that could have appeared to influ-
et al., 2010). The differences may be attributed to the different leaching ence the work reported in this paper.
time of the MSWs from the incineration plants and landfills. The landfill
leachates are typically collected at stable leaching stage after a long Acknowledgements
leaching time, and most PFASs have already leached out during the ini-
tial fast leaching stage. In contrast, leachate from MSW incineration This research was supported by the National Natural Science
plants is a short-term (typically 5 days in the present study) leachate Foundation of China (Project No. 21637001) and the Guangdong
with high levels of PFASs. Furthermore, production of leachates from (China) Innovative and Entrepreneurial Research Team Program (No.
different waste treatment plants should also be considered. Compared 2016ZT06N258). It was also partially supported by the Fundamental
with the variety of factors that affect landfill leachate, leachate from Research Funds for the Central Universities (No. 21617454) and the
MSW incineration plants is primarily influenced by MSW types. Shenzhen Science and Technology Funding Project [Grant No.
The amounts of PFASs in the fly ash (Plant A: 1.390 kg/y, Plant B: JCYJ20170816102318538].
0.0915 kg/y, and Plant C: 0.0650 kg/y) and bottom ash (Plant A:
5.45 kg/y, Plant B: 1.96 kg/y, and Plant C: 0.724 kg/y) were significantly Appendix A. Supplementary data
less than those in the leachates. Low contents of PFASs in the fly ash and
bottom ash indicated that incineration destroyed most of the PFASs Supplementary data to this article can be found online at https://doi.
under high temperatures, with some residues still captured by fly ash org/10.1016/j.scitotenv.2021.148468.
or remaining in the bottom ash due to uncompleted incineration,
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