Journal of Colloid and Interface Science 434 (2014) 5964

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Journal of Colloid and Interface Science

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Removal of peruorooctane sulfonate (PFOS) and peruorooctanoate

(PFOA) from water by coagulation: Mechanisms and inuencing factors
Yueping Bao a, Junfeng Niu a,, Zesheng Xu a, Ding Gao a, Jianghong Shi a, Xiaomin Sun b, Qingguo Huang c
a

State Key Laboratory of Water Environment Simulation, School of Environment, Beijing Normal University, Beijing 100875, PR China
Environment Research Institute, Shandong University, Jinan 250100, PR China
c
College of Agricultural and Environmental Sciences, Department of Crop and Soil Sciences, University of Georgia, Grifn, GA 30223, United States
b

a r t i c l e

i n f o

Article history:
Received 8 May 2014
Accepted 25 July 2014
Available online 10 August 2014
Keywords:
PFOS
PFOA
Coagulation
Mechanism
Natural organic matter

a b s t r a c t
In this study, alum (Al2(SO4)318H2O), ferric chloride (FeCl36H2O) and polyaluminium chloride (PACl)
were used to remove peruorooctane sulfonate (PFOS) and peruorooctanoate (PFOA) from water. The
inuencing factors, including pH and natural organic matter (NOM), were investigated. A positive correlation was found between the size of the ocs and the removal efciency of PFOX (X = S and A). The
removal ratios of PFOS and PFOA were 32% and 12%, respectively, when 50 mg/L of FeCl36H2O was
added as the coagulant at the initial pH. Coagulation achieved high removal ratios for PFOX under acidic
conditions (47.6% and 94.7% for PFOA and PFOS at pH 4, respectively). In addition, increasing NOM concentrations decreased the removal rates of PFOX because of the existence of competitive adsorption
between NOM molecules and PFOX on the surface of the coagulants and ocs. The combination of adsorption by powdered activated carbon (PAC) and coagulation increased the removal ratios up to >90% for
PFOX at the initial concentration of 1 mg/L, implying that the adsorption enhanced coagulation. Meantime, the experiments with natural water showed that coagulation is a feasible method to remove PFOS
and PFOA from surface water.
2014 Elsevier Inc. All rights reserved.

1. Introduction
Peruorooctane sulfonate (PFOS) and peruorooctanoate
(PFOA) are typical peruorinated compounds (PFCs) that have been
used in many industries including surfactants and re retardants
for decades [1,2]. Due to their high-energy carbonuorine bond
(CAF, 116 kcal/mol) and low reactivity [3], these compounds are
persistent in the natural environment and have been widely
observed in sediments, sludge, municipal wastewater, drinking
water and even human blood throughout the world [4,5]. Although
several considerable advancements have been made in order to
understand the environmental fate and toxicity of these compounds, challenges still remain because of their particular chemical
properties [6]. In addition, PFOS was categorized as one of the new
persistent organic pollutants in the Stockholm Convention in 2009
[7]. While PFOA has been used as an additive in the production of
uoropolymers for years and is still produced and used in many
industries [8]. In contrast to other persistent organic pollutants
(POPs), PFOS and PFOA have higher water solubility (680 mg/L
for PFOS in pure water and 3400 mg/L for PFOA) [9,10], and they
Corresponding author. Fax: +86 10 58807612.
E-mail address: junfengn@bnu.edu.cn (J. Niu).
http://dx.doi.org/10.1016/j.jcis.2014.07.041
0021-9797/ 2014 Elsevier Inc. All rights reserved.

are easy to transport into the aquatic environment, resulting in

acute and chronic toxicity to aquatic organisms [10]. The physicochemical properties of PFOS and PFOA are shown in Table S1. In our
previous study, the toxicity effects of PFOS and PFOA on Brachionus
calyciorus (B. calyciorus) were tested, and the results displayed
the changes of B. calyciorus both at the single level and at the population level when they were exposed to PFOS and PFOA [11].
Other studies showed that PFOS and PFOA had been found in the
blood of virtually all Americans tested during the last decade
[12], and higher serum levels of PFOS and PFOA were associated
with a higher prevalence of hyperuricemia [13]; at the same time,
they were related to current disease in the U.S. general adult population [14]. Therefore, it was necessary to develop reliable and
effective methods for the removal of PFOS and PFOA from aqueous
environments.
In previous studies, PFOS and PFOA were reported to be resistant to oxidation [5,1517]. Some researchers studied the adsorption behaviors of PFOS and PFOA on different adsorbents [1822],
indicating that physicochemical treatments played an important
role on the removal of these compounds. Conventional physicochemical technologies, such as adsorption [2326], membrane ltration [9,27,28] and sonochemistry [2931], have been conrmed
to be effective for PFOS and PFOA removal at a relatively high

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Y. Bao et al. / Journal of Colloid and Interface Science 434 (2014) 5964

concentration (tens to hundreds mg/L) in wastewater. However,

these technologies are not effective and economic for lower concentrations of PFOS and PFOA in surface water. Therefore, it is still
meaningful to nd an effective method for the removal of PFOS and
PFOA with relatively low concentrations.
Coagulation has been widely employed in drinking water and
wastewater treatment processes for removing various particulates
and natural organic matter (NOM) [32,33]. The process of coagulation is inuenced by the source of water and the nature of the
organic constituents existing in the water (including suspended,
colloidal and dissolved organic matter). Coagulation by adding
hydrolyzing chemicals, such as alum and iron salts, mainly
involves: (i) destabilization of small suspended and colloidal particulate matter; (ii) adsorption or reaction of portions of the colloidal and dissolved NOM to particles; and (iii) creation of occulent
particles that sweep through the water to be treated, enmeshing
small suspended, colloidal, and dissolved material as they settle.
In prior study, PFOA was reported to be removed up to 90% from
water by polyaluminium chloride (PACl, Al2O3 = 29%). In the coagulation process, PFOA was adsorbed on the particles in water at the
rst step, which was the crucial one, and then removed via the
removal of suspended solids (SS) [34]. However, in other literature,
the removal of PFOS and PFOA by coagulation was veried by the
adsorption onto the freshly formed ne Al hydroxide ocs during
the initial stage of coagulation [35]. Until now, the removal mechanism for PFOS and PFOA in water has not been fully understood.
Thus, it is necessary to examine the effects of different coagulants
in removing PFOS and PFOA from water. The different inuencing
factors such as pH and NOM are also needed to be investigated
to interpret the removal mechanism of peruorinated compounds
from water by coagulation.
In this study, the removal abilities of different coagulants for
PFOS and PFOA, including alum (Al2(SO4)318H2O), PACl and ferric
chloride (FeCl36H2O), were investigated. The aims of this present
study were: (i) to investigate the effect of inuencing factors,
including pH and NOM; (ii) to explore the removal efciency of
PFOS and PFOA in natural water and the combined coagulation
with powdered activated carbon (PAC); and (iii) to interpret the
removal mechanisms between peruorinated compounds and
coagulants.

a negligible effect on the adsorption of PFOS and PFOA in our previous study. Meanwhile, 1.0 mmol/L NaHCO3 and 1.0 mmol/L NaCl
were added to provide alkalinity and ionic strength [35]. A given
amount of PFOS or PFOA was added into the synthetic water, and
the mixture was stirred for 30 min before the coagulation experiments. The synthetic water containing PFOS or PFOA was used to
conduct the coagulation experiments, including the effects of coagulant dose (1100 mg/L), solution pH (49), concentration of HA or
FA (050 mg/L) and PAC (01000 mg/L), on the removal of PFOS or
PFOA and turbidity. To investigate the effect of PAC, different
amounts (01000 mg/L) of PAC were added into the synthetic
water, and the mixture was stirred for 30 min to allow PFOX to
adsorb on the PAC and reach the sorption equilibrium. During
the coagulation experiments, the changes of pH values, as well as
the turbidity, were measured in each of the batch experiments.
Coagulation experiments were performed in 500 mL plastic
beakers on a conventional jar test apparatus. The coagulants were
added into each 500 mL solution with an initial concentration of
1.0 mg/L PFOS or PFOA to study the removal efciency. Before
coagulation, the mixture was stirred for 30 min to examine the
adsorption of the plastic beaker. The jar test procedures consisted
of a 30 s rapid mix (300 rpm), a 15 min slow mix (50 rpm), and a
15 min settling period. The obtained supernatants were collected
for PFOS and PFOA determination, as well as the changes of pH
and turbidity.
2.3. Characterization
The FA used in the experiments was characterized by Fourier
transform infrared spectroscopy (FT-IR, Nexus 670, Nicolet, USA),
and the main functional groups were determined. The ocs formed
in the coagulation were characterized by transmission electron
microscopy (TEM, H600, Hitachi, Japan), and the particle sizes of
the ocs were measured by a particle size analyzer (S3500, Microtrac, USA). The surface area of PAC used in the experiment was
measured with a surface area analyzer (Quadrasorb SI, Quantachrome, USA) as 1280 m2/g with the use of nitrogen, and its point
of zero charge (pHpzc) was determined to be pH 7.8, according to
the method reported before [36,37]. The pH values and turbidity
changes were recorded by a microprocessor pH meter (pH 211,
EUTECH Co, USA) and a turbidimeter (WGZ-1B, Xinrui, China).

2. Experimental section
2.4. Analytical method of PFOS and PFOA
2.1. Materials
All chemicals used in the experiments were of reagent grade or
higher and were used as received without further purication.
PFOS and PFOA were supplied by SigmaAldrich Chemical Co.
Humic acid (HA), fulvic acid (FA), kaolinite clay, sodium hydroxide
(NaOH), ammonium acetate (CH3COONH4), and other chemicals,
such as Al2(SO4)318H2O, FeCl36H2O and PACl, were obtained from
Sinopharm (Beijing, China). The pH values were adjusted by adding
HCl (5%, v/v) and NaOH (5%, m/m). A stock solution of HA was prepared by adding 2.5 g HA into 250 mL 0.1 mmol/L of NaOH solution, whereas FA was dissolved directly into deionized (DI) water.
All solutions used in our experiments were prepared with deionized (DI) water supplied by a Milli-Q Gradient-A 10 Millipore
(resistance of 18.25 MX).

After the coagulation process, 1.0 mL of PFOS solution taken

from the supernatant was diluted with 1.0 mL methanol
(v/v = 1:1). The mixture was then ltered with a 0.2 lm inorganic
membrane lter, whereas the sample of PFOA was directly ltered
with a 0.2 lm inorganic membrane lter without dilution [21]. The
concentrations of PFOS and PFOA were measured by a high performance liquid chromatography coupled with a triple-stage quadrupole mass spectrometer (HPLC-MS/MS, API 3200, Applied
Biosystems, USA). The HPLC separation was performed with a HPLC
BEH C18 column (2.1  50 mm, 1.7 lm) at 40 C. The mobile
phases were composed of methanol and 10 mmol/L CH3COONH4.
The total analysis time was 7 min, and the ow rate was set at
0.8 mL/min. The details of the analytical method can be found in
our previous study [38].

2.2. Jar tests

3. Results and discussion

Coagulation of PFOS and PFOA was performed in a series of jar

tests at different initial pHs and concentrations of HA or FA. Unless
otherwise specied, the synthetic water was prepared by adding
kaolinite clay (10 mg/L) for turbidity, which was proven to have

3.1. Removal of PFOS and PFOA by coagulation

As ferric or aluminum ions are added into the water, a number
of parallel and sequential reactions occur. Initially, when a salt of

Y. Bao et al. / Journal of Colloid and Interface Science 434 (2014) 5964

61

Al (III) and Fe (III) are added into water, they will dissociate to yield
trivalent Al3+ and Fe3+, as given below:
3

Al2 SO4 3 2Al

FeCl3 Fe

3SO2
4

3Cl

The trivalent ions of Al3+ and Fe3+ then hydrate to form the
3+
aquometal complexes Al(H2O)3+
6 and Fe(H2O)6 . Soon afterward,
these aquometal complexes pass through a series of hydrolytic
reactions, as shown in Eqs. (3) and (4). These subsequent reactions
give rise to the formation of a variety of soluble mononuclear (one
aluminum or iron ion) and polynuclear (several aluminum or iron
ions) species, as illustrated in the research of Letterman [39].

33 2
32
H2 O
OH2
H2 O
OH
6
7
6
7

4 H2 O Al=Fe OH2 5 4 H2 O Al=Fe OH2 5 H

H2 O
OH2
H2 O
OH2
3

Fig. 2. Effect of the coagulants on the removal of PFOS and PFOA. Initial
concentrations of PFOS and PFOA: 1 mg/L; initial pH values: 8.54 and 8.56 for
PFOS and PFOA, respectively; initial turbidity: 9.5 NTU; alkalinity: 1 mM NaHCO3;
ion strength: 1 mM NaCl.

in the solution. This result was related with the sizes of ocs produced by different coagulants, suggesting that the removal efciency was inuenced by the size of ocs (see Figs. S1 and S2 of
the Supporting Information).

In the case of aluminum; the dashed lines are used to

denote an unknown sequence of reactions:

3.2. Effect of pH

Because the pKa values of PFOS and PFOA are around 3.27 and
2.8 [40,41], respectively, both were lower than the pH values
adopted in the current study. Therefore, PFOS and PFOA mainly
existed in the deprotonated forms in all of the experimental conditions. These anions could be easily adsorbed onto the positive surface of the coagulants and the ocs via electrostatic attraction and
removed with the formed precipitate. Some detailed mechanisms
related to the removal of PFOS and PFOA contain the following:
(i) binding of monomeric cationic species to anionic sites of the
organic molecules; (ii) binding of polymeric cationic species; (iii)
adsorption on the ocs, which were supercially positively
charged; and (iv) enmeshment in a precipitate (Fig. 1).
The effect of coagulant dose on the removal of PFOS and PFOA
by coagulation is shown in Fig. 2. The concentrations of PFOS and
PFOA in water decreased with the increasing coagulant dose from
1 to 100 mg/L, and Al2(SO4)318H2O had a slight effect on the
removal of PFOS and PFOA. As shown in Fig. 2, the removal ratios
of PFOS and PFOA are at their maxima when FeCl36H2O was added

Among all of the factors involved in the coagulation process, pH

is one of the most important factors because it can inuence all of
the hydrolysis equilibria that arise and is sensitive to the addition
of metallic cations.
The effect of pH on the removal of PFOX by FeCl36H2O coagulant is presented in Fig. 3. For PFOS and PFOA, the removal rates
would increase with the decrease of pH. As the pH decreases, the
ocs are positively charged, inducing the electrostatic attraction
with the anionic PFOS and PFOA species. In addition, coagulation
achieved a higher removal ratio for PFOS than PFOA under the conditions at pH 4 and 7, suggesting the favorable sorption process of
PFOS on ocs. Because PFOS and PFOA have similar ranges of ACF2A chain length, the distinctly different degrees of adsorption
capacity are presumably due to the different functional groups of
PFOS and PFOA. This result was in accordance with the adsorption
behaviors of PFOS and PFOA on aluminum in a previous study [21].
According to Pearsons concept of hard and soft acids and bases,

Fig. 1. Schematic diagram of the coagulation mechanisms of PFOS and PFOA: (i)
binding of monomeric cationic species to anionic sites of the organic molecules; (ii)
binding of polymeric cationic species; (iii) adsorption on the ocs which were
supercially positive charged; (iv) enmeshment in a precipitate.

Fig. 3. Effect of the coagulation pH on the removal of PFOS and PFOA by the
addition of 50 mg/L of ferric chloride. Initial concentrations of PFOS and PFOA:
1 mg/L; initial turbidity: 9.5 NTU; alkalinity: 1 mM NaHCO3; ion strength: 1 mM
NaCl.

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Y. Bao et al. / Journal of Colloid and Interface Science 434 (2014) 5964

Fig. 4. Effect of FA on the removal of PFOS and PFOA by the addition of 50 mg/L of
ferric chloride. Initial concentrations of PFOS and PFOA: 1 mg/L; initial turbidity:
9.5 NTU; alkalinity: 1 mM NaHCO3; ion strength: 1 mM NaCl.

the carboxylate group is a soft base, whereas the sulfonate group is

a relatively hard one. Because the ocs produced in the experiments were oxides, which belong to hard acids, the hard base is
more easily adsorbed on the oxide surfaces. Another reason for this
phenomenon is the difference in the molecular size, which is a sign
of being more hydrophilic or hydrophobic. In addition, changes in
the pH and turbidity were observed. The experimental results
showed that the coagulation process has a signicant effect on
the removal of turbidity (see Table S2 of the Supporting
Information).

3.3. Effect of NOM

In natural environment, NOM can interact with organic contaminants through various binding and adsorption interactions, which
has a considerable effect on the migration and transformation of
organic pollutants [22,4245]. The effect of organic matter on the
partitioning of PFOS and PFOA to clay particles was reported in
the literature, which suggested that organic matter could inuence
the sorption behavior of PFOS and PFOA through hydrophobic and
electrostatic interactions [46]. As one of signicant portions of
NOM in the environment, humic acid (HA) and fulvic acid (FA),
which mainly arise from microbial degradation of plants and animals, are ubiquitous in natural waters. Consequently, it is essential
to analyze the effects of HA/FA on the removal of PFOS and PFOA in
aqueous solution by coagulation. In the experiments, different concentrations (050 mg/L) of dissolved HA/FA were added into the

reaction liquid to investigate the potential effect of HA and FA on

the removal of PFOS and PFOA by coagulation. FA was characterized by FT-IR (Fig. S3), and the results in the experiments showed
that the addition of HA had a more signicant effect on the removal
of PFOS than PFOA (see Fig. S4 of the Supporting Information). High
NOM concentrations made the coagulation system stable, whereas
the PFOS and PFOA removal rates dropped at the high concentrations of FA (Fig. 4). When a low concentration of FA (2 mg/L) was
added into the solution, the removal rate increased slightly
because of the adsorption of PFOS and PFOA on the FA via hydrophobic interaction. Previous studies indicated that hydrophobic
partitioning was mainly responsible for PFOS sorption on the
organic fraction in natural sediments [47], and the sorption of
PFOA on sludge was due to its partitioning from the aqueous phase
to the biosolids during the sorption process [26]. However, because
of the steric hindrance effect of the FA molecule, as well as
the competitive adsorption between FA molecules and pollutants,
the removal rate would have a downtrend with the increasing concentration of FA. Similar results were also observed in the HA
experiments. Another reason for this phenomenon is that HA/FA
would be negatively charged in water due to the dissociation of
the functional groups (i.e., ACOOH, AOH, AC@O), enhancing the
electrostatic repulsion between them and the negatively charged
pollutants in water. When the metal ions (Al3+ and Fe3+) were
added into the water, HA/FA bonded with the metal ions (Al3+
and Fe3+), and the ocs produced in the coagulation decreased with
the decrease of free ions.
Supplementary experiments were conducted to investigate the
efciency of coagulation in the surface water, and the results indicated that the coagulation process has an effective application in
actual water to some extent (see Fig. S5 of the Supporting Information). Due to the low concentration of particles in actual water (low
turbidity), the removal ratios of PFOS and PFOA in actual surface
water were 9.6% and 14.3%, respectively, which were slightly
lower than that in the synthetic water. The removal efciency
depends on the sizes of ocs produced in the experiments
(FeCl36H2O > PACl  Al2(SO4)318H2O). However, different from
the results of synthetic water, the removal of PFOA was higher than
that of PFOS in the actual surface water.
3.4. Enhanced coagulation by PAC
Carbon materials have been used to remove PFOS and PFOA
from water due to their economy and effectiveness [18,19,22]. It
has been reported that peruorinated compounds could be effectively removed by granular activated carbon (GAC) [26,48].
Because PAC has a signicantly higher adsorption rate and capacity
for both PFOS and PFOA in comparison with GAC, PAC may be a

Fig. 5. Distribution of PFOS and PFOA in solid and aqueous phases after 30 min sorption by adding PAC. Initial concentrations of PFOS and PFOA: 1 mg/L; initial turbidity: 9.5
NTU; alkalinity: 1 mM NaHCO3; ion strength: 1 mM NaCl.

Y. Bao et al. / Journal of Colloid and Interface Science 434 (2014) 5964

63

Fig. 6. Removal of PFOS and PFOA by adsorption and coagulation. Initial concentrations of PFOS and PFOA: 1 mg/L; initial turbidity: 9.5 NTU; alkalinity: 1 mM NaHCO3; ion
strength: 1 mM NaCl; coagulant: 50 mg/L ferric chloride.

more promising adsorbent for PFOS and PFOA removal [22,49]. It is

of great importance to investigate the behavior of coagulation on
the existence of PAC for the removal of PFOS and PFOA in water.
Previous studies reported that the removal ratio of PFOA can be
enhanced by the addition of PAC before coagulation and the
adsorption of PFOA on the PAC plays an important role in the
removal processes [34]. The combined effect of adsorption and
coagulation was further examined in the present study.
As shown in Fig. 5, the amount of PFOS and PFOA in water
decreased with the increase of the amount of PAC, indicating that
most PFOS and PFOA molecules were able to be adsorbed on the
PAC in water. In the experiments, PAC exhibited higher adsorption
efciency for PFOA than PFOS, which was in correspondence with
previous study [49]. Based on the adsorption behaviors and the
characteristics of adsorbents and adsorbates, electrostatic interaction and hydrophobic interaction were deduced to be involved in
the adsorption behaviors.
After the sorption equilibrium, the mixture was used to investigate the behavior of coagulation. The effects of PAC dose on the
removal of PFOS and PFOA in water after the adsorption and coagulation are shown in Fig. 6. The addition of PAC signicantly
increased the removal rates (>90%) of PFOS and PFOA in water by
coagulation. Most PFOS and PFOA molecules were removed in
the coagulation via the produced precipitate because PFOS and
PFOA could be adsorbed on the surface of PAC. In all of the experiments, the turbidities after coagulation were lower than 0.5 (the
initial turbidities of PFOS and PFOA were 9.5 and 9.6, respectively).
4. Conclusions
Coagulation is an effective method to remove PFOX (X = S and
A) from water, and the removal was achieved by adsorption onto
the surface of coagulants and ocs via electrostatic interaction.
Under the conditions of 10 mg/L kaolinite clay for turbidity,
1 mmol/L NaHCO3 for alkalinity and 1 mmol/L NaCl as ionic
strength, the removal ratio of PFOS (32%) was higher than that
of PFOA (12%) at a FeCl36H2O dose of 50 mg/L. Coagulation
resulted in higher removal ratios of PFOS and PFOA in acidic conditions, suggesting the favorable sorption process of PFOS and PFOA
on ocs. In the experiments, the distinctly different degrees of
adsorption capacity for PFOS and PFOA were presumably due to
the different functional groups and molecular sizes. Meanwhile,
FA at low concentrations can enhance the removal of PFOS and
PFOA by coagulation because of adsorption on FA via hydrophobic
interactions. However, when the concentration of FA increased, the
removal ratios of PFOS and PFOA decreased because of the steric
hindrance effect of FA molecules and the competitive adsorption.
In addition, the combination of PAC adsorption and coagulation

resulted in the removal ratios of PFOS and PFOA > 90%, indicating
that the adsorption enhanced coagulation. The experiments with
surface water demonstrated that coagulation can be applied to
remove PFOS and PFOA in surface water to some extent.
Acknowledgments
This work was supported by the National Science Foundation
for Innovative Research Group of China (No. 51121003), the
National Natural Science Foundation of China (No. 51378065)
and the Fundamental Research Funds for the Central Universities
(No. 2012LZD03).
Appendix A. Supplementary material
Supplementary data associated with this article can be found, in
the online version, at http://dx.doi.org/10.1016/j.jcis.2014.07.041.
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