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Bulletin of EnvironmentalContamination and Toxicology ISSN 0007-4861Volume 94Number 1 Bull Environ Contam Toxicol (2015)94:34-40DOI 10.1007/s00128-014-1419-y

Perfluoroalkyl Substances in Daling RiverAdjacent to Fluorine Industrial Parks:Implication from Industrial Emission

Jing Meng, Tieyu Wang, Pei Wang,Zhaoyun Zhu, Qifeng Li & Yonglong Lu

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Perfluoroalkyl Substances in Daling River Adjacent to FluorineIndustrial Parks: Implication from Industrial Emission

Jing Meng • Tieyu Wang • Pei Wang •

Zhaoyun Zhu • Qifeng Li • Yonglong Lu

Received: 13 May 2014 / Accepted: 3 November 2014 / Published online: 25 November 2014

� Springer Science+Business Media New York 2014

Abstract The pollution level and source of perfluoroalkyl

substances (PFASs) in mainstream and tributary of Daling

River in northeast China were investigated in present study.

Concentrations of PFASs in surface water and sediment

ranged from 4.6 to 3,410 ng/L and from 0.08 to 2.6 ng/g

dry weight, respectively. The lowest levels of PFASs were

found in vicinity of a drinking water source located in

upstream of Daling River. Xihe tributary, which is adjacent

to two local fluorine industrial parks, contained the highest

level of PFASs. Short-chain PFASs, including perfluorob-

utanoic acid and perfluorobutane sulfonate, were of higher

levels due to their emerging as alternative products for

perfluorooctane sulfonate. High level of perfluorooctanoic

acid was also found in Daling River. Based on these

results, it can be concluded that the relatively severe pol-

lutions of Xihe tributary were caused by long-term devel-

opment of the two local fluorine industry parks.

Keywords PFASs � Historical deposition � Sediment

core � Partition � Fluorine industrial park

Perfluoroalkyl substances (PFASs) have been widely used in

both industrial and domestic products since 1950s (OECD

2002). Several PFASs are toxic bioaccumulative organic

pollutants. In 2009, perfluorooctane sulfonate (PFOS) and

related compounds were listed under Stockholm convention

on persistent organic pollutants and called for restriction on

manufacture and application worldwide (UNEP 2009).

China began large-scale production of PFOS since 2003 and

the total output of PFOS is about 230 t/a in past several years

(Xie et al. 2013). In recent years, the fluoropolymer industry

has been using C4 PFASs, including fluorobutanesulfonate

(PFBS) and perfluorobutanoic acid (PFBA), to replace PFOS

and perfluorooctanoic acid (PFOA). All these PFASs have

been widespread with the industrial wastes (Oliaei et al.

2013; Wang et al. 2013).

Fluorine industrial enterprises in China are mainly located

in Liaoning, Zhejiang, Jiangsu and Shandong provinces

(Chen et al. 2009). Daling River is the largest river in west

Liaoning Province and flows into Liaodong Bay of Bohai

Sea. Two local fluorine industrial parks are located next to

Daling River, producing and applying PFASs. Previous

studies showed that the river has been contaminated with

PFASs (Bao et al. 2011; Liu et al. 2009; Wang et al. 2013).

The local fluorine chemical industry has been under long-

term development and caused the pollution of Daling River.

However, the studies related to pollution history of PFASs in

the river are still scarce. Vertical profile of residues in sedi-

ment core has been used as historical records of the pollution

and related anthropogenic activities. The objectives of this

study were to evaluate the pollution level of PFASs in Daling

River, assess environmental fate and potential sources for

regional urban and industrial development. This investiga-

tion will provide scientific information for future fluorine

industry management and water remediation.

Materials and Methods

The sampling sites cover Xihe tributary and mainstream of

Daling River. Seven surface water samples and corresponding

J. Meng � T. Wang (&) � P. Wang � Z. Zhu � Q. Li � Y. Lu

State Key Lab of Urban and Regional Ecology, Research Center

for Eco-Environmental Sciences, Chinese Academy of Sciences,

Beijing 100085, China

e-mail: wangty@rcees.ac.cn

J. Meng � P. Wang � Z. Zhu � Q. Li

University of Chinese Academy of Sciences, Beijing 100049,

China

123

Bull Environ Contam Toxicol (2015) 94:34–40

DOI 10.1007/s00128-014-1419-y

Author's personal copy

sediment cores were collected from this watershed in October

2011. Sediment cores were collected using a Beeker sediment

sampler at*3 m off the riverbanks. The sampler was cleaned

with methanol and Milli-Q water before each sampling. Each

sediment core was sliced into 2 cm intervals to the depth of

30 cm sections and 105 sub-samples were prepared totally,

and then stored in polypropylene (PP) bottles to transport to

the laboratory. Subsequently the samples were freeze-dried,

passed through a 2 mm mesh sieve, and stored at 4�C in pre-

cleaned glass jars before used. Corresponding surface water

samples (1.5 L) were collected 20–30 cm below water sur-

face with PP bottles. All of the, 105 sediments and 7 surface

water samples were analyzed for PFASs in laboratory.

Water sample was extracted with a solid phase extrac-

tion (SPE) cartridge as previously reported with minor

modification and optimization (Wang et al. 2011). The

cartridge was preconditioned with 4 mL of 0.1 % ammonia

in methanol, 4 mL methanol and 4 mL Milli-Q water. Five

hundred milliliter water sample was loaded into the car-

tridge. The cartridge was washed with 20 mL Milli-Q

water, 4 mL of 25 mM sodium acetate, allowed to run dry,

and eluted with 4 mL methanol and 4 mL of 0.1 %

ammonia in methanol. The eluents were collected, com-

bined, and concentrated to 1 mL under a gentle stream of

high purity nitrogen and then filtered through a 0.2 lm

nylon filter into a 1.5 mL auto-sampler vial fitted with PP

cap for HPLC analysis. Sediment samples were extracted

as the previously reported (Wang et al. 2011). Briefly,

2 mL Milli-Q water was added to 2.5 g sediment. Each

sample was spiked with 1 mL of 0.5 M tetrabutylammo-

nium hydrogensulfate (TBAHS) and 2 mL of 25 mM

sodium acetate under vortexing. Subsequently, the sedi-

ment was extracted with 5 mL of methyl tert-butyl ether

(MTBE) and the supernatant was collected. The extraction

was repeated twice, and the sediment was then washed with

15 mL MTBE. The supernatants were combined, dried

under a gentle stream of high purity nitrogen and redis-

solved in 1 mL methanol. The 1 mL elution was trans-

ferred to 50 mL PP tube, brought to 50 mL with Milli-Q

water and extracted with the SPE cartridge as described

above for the water sample.

All PFASs were analyzed using an Agilent HP 1200 high

performance liquid chromatography system equipped with

an Applied Biosystems SCIEX 3000 tandem mass spec-

trometer (HPLC–MS/MS). MS was operated in negative

electrospray ionization (ESI) mode. The analytes were

separated on C18 analytical column using methanol as a

mobile phase and 2 mM ammonium acetate as an ionization

aid. Chromatograms were recorded with MS detection in

multiple reaction monitoring (MRM) mode and at least two

transitions of per-analyte were monitored when possible.

The optimal settings for collision energies and declustering

potential were determined for the transitions of each analyte.

Field blanks (n = 3) and transport blanks (n = 3) were

included during field sampling. Procedural blanks (n = 7)

were prepared to check for potential contamination. All

blanks were below the limit of detection (LOD), where

LOD was defined as three times of signal-to-noise ratio

(S/N). The limit of quantification (LOQ) was set as five

times of S/N. Matrixes spiked with a standard solution

were analyzed to determine the recovery of each target

PFAS. All the matrix spike recoveries (MSRs) ranged from

86 % ± 4 % to 113 % ± 5 % for water samples and ran-

ged from 86 % ± 6 % to 119 % ± 4 % for sediment. The

LODs, LOQs and MSRs for all target PFASs were sum-

marized (Table 1). All concentrations lower than the LOQs

were reported as half of the LOQs, and those lower than

LODs were reported as zero.

Results and Discussion

Thirteen PFASs were detected in surface water and corre-

sponding sediments in seven sampling sites (Table 2). The

concentrations of PFASs in the surface water of Daling

River ranged from 4.6 to 3,410 ng/L. It is clear that con-

centrations of PFASs from Daling River, especially at site

P2, were at high levels. PFBA and PFBS were the pre-

dominant PFASs with concentrations in ranges of

1.1–960 ng/L and 1.4–2,280 ng/L, respectively. Concentra-

tions of short-chain PFASs, such as PFBA and PFBS, from

Daling River were higher than the corresponding PFASs

from other Chinese rivers, such as Liaohe River (PFBS, not

detected, abbreviated as nd), Haihe River (PFBS

0.41–1.79 ng/L), Pearl River (PFBS \0.03–3.4 ng/L) and

Yangtze River (PFBS\0.005–2.1 ng/L) (So et al. 2007; Pan

et al. 2011; Yang et al. 2011). The concentration of PFOA

ranged between 0.63 and 280 ng/L. The level of PFOS

contamination was relatively low in the surface water, with

concentrations in the range of 0.80–8.7 ng/L. According to

water quality criteria, the contaminations of PFOA, PFBS

and PFOS in the surface water of Daling River are all under

the related criteria maximum concentration (CMC) and

criteria continuous concentration (CCC) for the protection of

aquatic organisms (Fig. 1) (Giesy et al. 2010). Thus, the

PFASs in the surface water may not induce the acute or

chronic toxicity to aquatic organisms. However, concentra-

tions of PFBS in five water samples were higher than the

Avian Wildlife Values (AWV) (17 ng/L), indicating that

PFBS has caused potential adverse effects on some wildlife

at the top of food chain, such as birds. The concentrations of

PFOS in all seven sampling sites were lower than the AWV

(47 ng/L) and may not lead to harmful effects.

PFASs were detected in seven surface sediments with

concentrations ranging between 0.08 and 2.6 ng/g dry

weight (dw). The concentrations of most PFASs in surface

Bull Environ Contam Toxicol (2015) 94:34–40 35

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sediments of Xihe River (P1 and P2) were significantly

higher than those of the mainstream of Daling River (P3–

P7). Along the mainstream of Daling River, the concen-

trations of PFASs in the upstream sediment (P3 and P4)

were lower than those in the downstream sediment (P5, P6

and P7). PFBA and PFBS were the dominant PFASs in

surface sediments of this river system, with concentrations

in ranges of nd-0.80 and nd-1.0 ng/g dw, which was con-

sistent with the results of surface water analysis. The

highest concentrations of PFBA and PFBS were both

observed at site P1, which is different from the reported

data for the major rivers in China. It has been reported that

PFOA and PFOS are dominant PFASs in most rivers in

China, generally (Bao et al. 2010; Li et al. 2011). The high

levels of PFBS and PFBA contamination in Xihe River are

attributed to the fluorine parks next to it, which produces

PFBS related products. In addition, concentrations of

PFOA and PFOS were in the ranges of 0.02–0.55 and nd-

0.47 ng/g dw, respectively. The highest concentration of

PFOS in surface sediment was detected at sampling site P2.

The concentrations of PFOS in other six samples were

relatively lower than 0.10 ng/g dw. PFBA, PFOA, PFBS

Table 1 Quality assurance of 13 target PFASs including limit of detection (LOD), limit of quantification (LOQ) and matrix spike recovery

(MSR) for water and sediment

Water Sediment

LOD (ng/L) LOQ (ng/L) MSR (%) LOD (ng/g) LOQ (ng/g) MSR (%)

Perfluorobutanoic acid (C4, PFBA) 0.13 0.63 86 ± 4 0.020 0.10 100 ± 5

Perfluoropentanoic acid (C5, PFPeA) 0.05 0.15 95 ± 5 0.010 0.03 104 ± 3

Perfluorohexanoic acid (C6, PFHxA) 0.04 0.15 98 ± 1 0.004 0.02 110 ± 3

Perfluoroheptanoic acid (C7, PFHpA) 0.06 0.15 105 ± 2 0.006 0.02 96 ± 6

Perfluorooctanoic acid (C8, PFOA) 0.05 0.19 102 ± 3 0.002 0.01 100 ± 11

Perfluorononanoic acid (C9, PFNA) 0.06 0.13 105 ± 4 0.002 0.01 109 ± 2

Perfluorodecanoic acid (C10, PFDA) 0.05 0.15 112 ± 4 0.004 0.02 103 ± 7

Perfluoroundecanoic acid (C11, PFUdA) 0.03 0.08 113 ± 5 0.008 0.02 90 ± 4

Perfluorododecanoic acid (C12, PFDoA) 0.05 0.13 98 ± 4 0.004 0.01 89 ± 4

Perfluorobutane sulfonate (C4, PFBS) 0.03 0.09 109 ± 7 0.004 0.01 119 ± 4

Perfluorohexane sulfonate (C6, PFHxS) 0.01 0.06 118 ± 4 0.004 0.01 114 ± 8

Perfluorooctane sulfonate (C8, PFOS) 0.03 0.10 109 ± 5 0.004 0.01 117 ± 2

Perfluorodecane sulfonate (C10, PFDS) 0.03 0.06 105 ± 8 0.010 0.03 86 ± 6

Table 2 Concentrations of PFASs in water and surface sediment from the Daling River

Analyte Water (ng/L) Sediment (ng/g dw)

P1 P2 P3 P4 P5 P6 P7 P1 P2 P3 P4 P5 P6 P7

PFBA 962 763 1.5 1.0 308 192 266 0.80 0.64 (0.07)a 0.14 0.22 0.13 0.19

PFPeA 47 31 \0.05b 0.64 21 14 21 0.06 0.06 \0.01 (0.02) (0.02) (0.02) (0.01)

PFHxA 15 37 0.27 \0.04 60 13 22 0.03 0.02 (0.01) 0.02 0.05 0.03 0.02

PFHpA 3.5 7.6 0.18 \0.06 3.6 2.9 3.8 0.02 (0.01) \0.006 (0.01) (0.01) 0.03 (0.01)

PFOA 103 284 1.2 0.63 101 83 132 0.55 0.41 0.02 0.33 0.16 0.11 0.14

PFNA 0.81 1.5 0.22 0.14 2.8 1.8 2.8 0.06 0.04 (0.01) (0.01) 0.07 0.03 0.03

PFDA 0.29 0.44 0.17 \0.05 0.40 0.33 0.39 0.03 (0.02) (0.01) \0.003 0.09 0.03 0.02

PFUdA 0.13 (0.05) 0.17 \0.03 \0.03 \0.03 \0.03 (0.01) (0.01) (0.01) (0.01) 0.08 0.03 (0.02)

PFDoA (0.09) (0.07) \0.05 \0.05 0.19 \0.05 \0.05 0.02 0.01 (0.01) (0.01) 0.03 0.01 \0.004

PFBS 1,825 2,276 7.8 1.4 652 341 600 1.00 0.89 0.03 (0.01) 0.20 0.07 0.15

PFHxS 1.6 3.8 \0.01 \0.01 0.58 0.27 0.94 0.04 0.06 0.02 0.01 0.01 0.01 0.02

PFOS 1.4 8.7 0.8 1.4 5.0 2.7 4.8 0.04 0.47 \0.004 0.01 0.04 0.08 0.05

PFDS 0.18 \0.03 \0.03 \0.03 0.74 \0.03 \0.03 (0.02) \0.01 0.05 \0.01 \0.01 0.06 (0.01)

PFASs 2,960 3,413 13 4.6 1,155 650 1,054 2.66 2.64 0.21 0.55 0.98 0.63 0.65

a Value in bracket means concentrations between LOD and LOQb Value less than LOD

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and PFOS accounted for 47–91 % of total PFASs. Based

on these results, it can be concluded that relatively higher

PFASs was deposited in sediments from Daling Watershed.

The two fluorine chemical parks (Park 1 and Park 2) have

been releasing PFASs into the surrounding environment for

several years (Wang et al. 2013).

Concentrations of PFASs in whole sediment core in P1

ranged between 0.08 and 2.7 ng/g dw (Fig. 2). The top

three layers of the sediment core contained relatively

higher amount of PFASs. The concentration of PFASs in

the following layers increased first and then decreased with

the increasing of depth. The highest concentration was

found in the layer of 20–22 cm deep. PFBA, PFOA and

PFBS are the predominant PFASs, accounting for 69 %–

95 % of the total PFASs. Concentrations of PFASs in P2 in

whole sediment core were between 0.33 and 6.4 ng/g dw

(Fig. 2). The top six layers contained higher amount of

PFASs, ranging between 2.6 and 6.4 ng/g dw. The highest

concentration of PFASs was found in the layer of

10–12 cm deep. PFBA, PFOA, PFBS and PFOS contribute

91 % to the total PFASs in P2 sediment core, therein,

PFBS and PFOS are predominant PFASs. Sampling sites of

P1 and P2 are located in the vicinity of park 1 and park 2

that were built in 2004 and 2008, respectively. The major

products of these two parks are fluoropolymer, aromatic

fluoride, surfactants, intermediates of medicine and pesti-

cides containing fluorine, which contribute directly to high

levels of PFASs in the sediment, especially in the top

layers of the sediment at P1 and P2. Currently, PFBS has

become an effective alternative product to replace PFOS in

several industrial and domestic products (Carter and Farrell

2010). Thus, high level of PFBS may be caused by the

application of these alternative techniques. The increasing

trend of PFASs in P1 and relative higher concentrations of

PFASs in P2 indicate that although concentration of PFOS

decreased, contaminations by other PFASs, mainly PFBA

and PFBS, in Daling River will become more serious with

the development of local fluorine parks. Therefore, emis-

sions of PFASs should be reduced/restricted during pro-

duction process and PFASs removal should be enhanced

during wastewater treatment.

P3 and P4 were selected in the vicinity of the Baishi

Reservoir that is located on the upstream of the Daling

River. Concentrations of PFASs in the whole sediment

cores of P3 and P4 were 0.14–0.32 and 0.14–0.55 ng/g dw,

respectively, which were obviously lower than those in

other sediment cores (Fig. 2). The average concentrations

of PFASs in whole sediment cores of P3 and P4 slightly

varied with mean values of 0.21 and 0.30 ng/g dw,

respectively. Relatively higher concentrations of PFASs at

site P4 and distinct PFASs compositions in these two sites

indicated that PFASs come from different sources.

P5, P6 and P7 sampling sites were selected on Daling

River after Xihe tributary merges into its mainstream.

Pollution levels of PFASs in the sediment cores at these

three sites are similar, with most PFAS concentrations

\1.0 ng/g dw (Fig. 2). The low levels of PFASs, espe-

cially low levels of PFBA and PFBS, in these three cores

were possibly due to the dilution of PFASs by the main-

stream, indicating major pollutants come from the Xihe

tributary. The highest concentration of PFASs (0.96 ng/g

dw) was observed in the first layer (0–2 cm) of P5 sedi-

ment, which further confirmed that fluorine industrial parks

along the upstream of Xihe tributary discharged PFASs

related pollutants directly into their surrounding environ-

ment. The variations of PFAS concentrations and compo-

sition in different layers of Xihe tributary sediment

indicated that other local industries, including electrical

applications, food processing, fine chemistry, have also

contributed to the PFASs pollution. The highest levels of

Fig. 1 Comparison of PFASs with suggested water quality criteria values for protection of aquatic organisms (n1/n2 in right figure: n1 means

concentration of PFOA, n2 means concentration of PFOS)

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PFBA and PFBS have been accumulated in the middle

layer of 12–14 cm deep in P6 and P7 sediments and

resulted in concentrations of 0.96 and 1.0 ng/g dw,

respectively. This observation indicated that these PFASs

directly come from the upstream and possibly is caused by

historical accidental discharge. PFBA and PFOS contrib-

uted to 69.4 % of the total PFASs at P6. PFBA, PFOA,

PFBS and PFOS, accounted for about 82.2 % of the total

PFASs at P7. The average level of PFASs in P7 sediment

(0.57 ng/g dw) was higher than that in P6 sediment

(0.37 ng/g dw), suggesting that PFASs from the upstream

is partially deposited in the estuarine sediment and there

were other potential local pollution sources. And because

of many oil production plants in coastal areas around

Jinzhou, fire-fighting foams partially contributed pollution

of PFOS comparing with other sites.

Relative concentrations of PFASs in the surface water

and sediments of Daling River and different potential

pollution sources are shown in Fig. 3. PFBS was the pre-

dominant PFASs composition in surface water with a

contribution of 57.48 % to the total PFASs, followed by

PFBA that accounted for 22.71 % of total PFASs. PFOA

contributed about 9.13 % to total PFASs. PFBS related

products have been produced in local fluorine chemical

parks of Daling River area. PFBS has become an alterna-

tive product for PFOS in a wide range of applications,

including textiles, leather, carpets, waxes, floor polishes

and paint/varnish. PFBA is replacing PFOS in waxes and

floor polishes (Force Technology 2004). PFOA and its salts

are used as a processing agent in the manufacture of

fluoropolymers such as polytetrafluoroethylene (PTEE)

(Prevedouros et al. 2006), one of major products in the

local fluorine chemical parks. All these contribute to the

PFASs contamination in Daling River.

The composition profiles of main detected PFASs are

not different between surface water and corresponding

sediment, indicating their PFASs contaminations are from

the same sources. However, the portions of same PFAS in

water and sediment are different. PFASs are released to

water and then adsorb to sediments. Different PFASs show

Fig. 2 Vertical profile of PFASs (ng/g) in sediment core from Daling River

38 Bull Environ Contam Toxicol (2015) 94:34–40

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different adsorption ability to sediment, resulting in the

portion variation of same PFAS in water and sediment. For

example, the proportions of PFBA in water and sediment

were at same level. The proportion of PFOA in surface

water ranged between 10.27 and 44.74 %, which was

higher than that in sediment. On the contrary, proportions

of PFBS in surface water and in sediment were 5.27 and

52.40 %. The portions of PFOS and C6 & C10 perfluoro-

alkyl sulfonic acids (PFSAs) in the three regions in sedi-

ment were generally higher, which was consistent with the

previous study that the adsorption of PFSAs to sediment is

much stronger than that of perfluoroalkyl carboxylic acids

(PFCAs) (Ahrens et al. 2009). Furthermore, longer chain

PFASs is easier to be absorbed by sediment than shorter

chain PFASs (Myers et al. 2012), but there was no related

sorption studies on PFBA and PFBS.

In general, the current findings will help researchers and

managers better understand the contaminations and indus-

trial emissions of PFASs in watershed adjacent to fluorine

industrial parks. Further detailed work with a more inten-

sive sampling effort with temporal discrimination is rec-

ommended to identify any shifts in production to shorter

chained or lesser fluorinated PFASs.

Acknowledgments This study was supported by the National Nat-

ural Science Foundation of China under Grant Nos. 41171394 and

41371488, and the Key Project of the Chinese Academy of Sciences

under Grant No. KZZD-EW-TZ-12.

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