Science of the Total Environment 637–638 (2018) 1358–1362

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Science of the Total Environment

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

Short Communication

Priority substances and emerging pollutants in urban rivers in Ukraine:

Occurrence, fluxes and loading to transboundary European
Union watersheds
Y. Vystavna a,b,⁎, Z. Frkova a,f, H. Celle-Jeanton c, D. Diadin b, F. Huneau d,e, M. Steinmann c, N. Crini c, C. Loup c
a
Biology Centre of the Czech Academy of Sciences, Institute of Hydrobiology, Na Sádkách 7, 37005 České Budějovice, Czech Republic
b
Department of Environmental Engineering and Management, O.M. Beketov National University of Urban Economy in Kharkiv, 17, Marshal Bazhanov Street, Kharkiv 61002, Ukraine
c
Université Bourgogne Franche-Comté, Laboratoire Chrono-Environnement, CNRS, UMR 6249, 16 route de Gray, F-25030 Besançon, France
d
Université de Corse Pascal Paoli, Laboratoire d'Hydrogéologie, Campus Grimaldi, BP 52, F-20250 Corte, France
e
CNRS, UMR 6134 SPE, BP 52, F-20250 Corte, France
f
Biology Centre of the Czech Academy of Sciences, Institute of Soil Biology, Na Sádkách 7, 37005 České Budějovice, Czech Republic

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

• Priority substances and emerging pol-

lutants in urban waters in Ukraine ex-
ceed EU standards.
• Loading of priority substances from
Ukrainian cities into EU rivers can be
over 2 t a−1.
• Chemicals banned in the EU can reach EU
water resources from this transboundary
country.
• Transboundary water management is
needed to fulfil EU water quality
standards.

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

Article history: The occurrence and fluxes of 18 priority substances and emerging pollutants listed in the European Union Water
Received 23 February 2018 Framework Directive and a Watch List (trace metals (Cd, Pb and Ni), nonylphenols, octylphenols, 8 polyaromatic
Received in revised form 5 May 2018 hydrocarbons, 4 dioxin-like polychlorinated biphenyls and diclofenac) were investigated in a Ukrainian city and
Accepted 7 May 2018
the mass discharge loads of these compounds into EU-transboundary watersheds were estimated. Fluxes of
Available online xxxx
chemicals were calculated per capita and per area of the Ukrainian urban territory and used to estimate mass
Editor: Kevin V. Thomas loading of priority and emerging concern compounds from Lviv, Uzhorod and Chernivtsi (West Ukraine) to
neighbouring EU-transboundary rivers. The highest loading was found for trace metals (1.15 t a−1), diclofenac
Keywords: (0.7 t a−1) and nonylphenols (0.4 t a−1). Transboundary water contamination must be considered in order to
Emerging pollutants successfully manage water resources in a manner that fulfils the requirements of EU environmental quality
Water framework directive standards.
Diclofenac © 2018 Elsevier B.V. All rights reserved.
Transboundary water
PAH
PCB

1. Introduction
⁎ Corresponding author at: Biology Centre of the Czech Academy of Sciences, Institute of
Hydrobiology, Na Sádkách 7, 37005 České Budějovice, Czech Republic. The European Union (EU) water legislation, the Water Framework
E-mail addresses: yuliya.vystavna@hbu.cas.cz, (Y. Vystavna),
zuzana.frkova@hbu.cas.cz, (Z. Frkova), helene.jeanton@univ-fcomte.fr, (H. Celle-Jeanton),
Directive (WFD, 2000/60/EC) aims to achieve and maintain good chem-
huneau@univ-corte.fr, (F. Huneau), marc.steinmann@univ-fcomte.fr, (M. Steinmann), ical and ecological status of surface water and groundwater. Environ-
nadia.crini@univ-fcomte.fr, (N. Crini), christophe.loup@univ-fcomte.fr (C. Loup). mental quality standards (EQS) based on annual average (AA-EQS)

https://doi.org/10.1016/j.scitotenv.2018.05.095
0048-9697/© 2018 Elsevier B.V. All rights reserved.
 Y. Vystavna et al. / Science of the Total Environment 637–638 (2018) 1358–1362 1359

and maximum allowable (MAC-EQS) concentrations were defined so Supplementary information, SI) crossing a large Ukrainian city (Kharkiv
far for 45 priority group of substances that represent a significant risk city; 1,439,039 inhabitants, 308 km2 area) (Fig. 1), in May 2016. Sam-
for the aquatic environment and thereby human health (Directive pling of diclofenac was done using the POCIS passive samplers and com-
2013/39/EU). Subsequently, the EU Watch List was established on mon- posite grab water samples (n = 3) were taken for the rest of targeted
itoring other potentially harmful substances (Decision 2015/495/EC). compounds. Cadmium (Cd), lead (Pb) and nickel (Ni) in water samples
While an awareness regarding the occurrence and distribution of prior- were analyzed by inductively coupled plasma mass spectrometry. Ex-
ity and emerging concern substances in EU catchments is developing tracts of polyaromatic hydrocarbons (PAH, i.e. anthracene, fluoran-
(Rodrigo, 2017; Sousa et al., 2018), there is still a gap in our knowledge thene, naphthalene, benzo(a)pyrene, benzo(b)fluoranthene, benzo(k)
on the spreading of these contaminants in transboundary waters, in- fluoranthene, benzo(g,h,i)perylene and indeno(1,2,3,-cd)pyrene) and
cluding those restricted and forbidden in the EU (Sousa et al., 2018; dioxin-like polychlorinated biphenyls (PCBs, i.e. PCB 77 as 3,3′,4,4′-
OECD, 2011). Eastern EU countries (Hungary, Poland, Romania and the T4CB, PCB 118 as 2,3′,4,4′,5-P5CB, PCB 126 as 3,3′,4,4′,5-P5CB, PCB 169
Slovak Republic) share large water basins (Bug and Danube) with as 3,3′,4,4′,5,5′-H6CB) were analyzed by gas chromatography tandem
Ukraine. Despite the development of legislative initiatives on the use mass spectrometry. Diclofenac, 4-nonylphenol (NPEO2, representative
of transboundary waters (Convention, 1994; Water Code of Ukraine, of nonylphenols) and 4-(1,1′,3,3′-tetramethylbutyl)-phenol (OPEO1,
1995; Agreement, 2014), only limited data exist on priority substances representative of octylphenols) in extracts were analyzed by liquid
and compounds of emerging concern in Ukraine/EU transboundary wa- chromatography tandem mass spectrometry. The detailed information
ters (Macklin et al., 2003; Sousa et al., 2018). Considering that the ma- on water sampling and analysis is in the SI. The fluxes of priority sub-
jority of these chemicals originate from urban areas and enter the stances (WFD, 2000/60/EC): Cd, Pb, Ni, PAHs, PCBs, NPEO2, OPEO1,
aquatic environment mainly via urban runoff (Delhomme et al., 2008), and diclofenac (EU Watch List) were calculated per capita and per
and/or domestic and industrial wastewaters (Sousa et al., 2018), a spe- area of the Kharkiv city. Mixed pre-treated at industrial sites (15% of
cial focus should be addressed towards urban catchments (Tiedeken total influents) and raw domestic wastewaters (85% of total influents)
et al., 2017). The occurrence and fluxes of 18 priority substances and of the Kharkiv city are processed in a conventional wastewater treat-
emerging pollutants listed in the European Union Water Framework Di- ment plant (WWTP; ca. 550,000 m3 d−1) via mechanical and biological
rective and a Watch List (trace metals (cadmium, lead and nickel), 8 treatment and discharged into the Lopan River downstream of the city
polyaromatic hydrocarbons, 4 dioxin-like polychlorinated biphenyls, centre (Fig. 1). Upstream of the WWTP, urban runoff enters the river
nonylphenols, octylphenols, and diclofenac) were investigated in a without treatment. Specific fluxes of targeted compounds were esti-
Ukrainian city and the mass discharge loads of these compounds into mated based on concentrations, water flow rates, urban area, number
EU-transboundary watersheds of the Baltic and Black Seas were of served by urban sewage population and expressed in a gram per
estimated. capita per year (g ca−1 a−1) for fluxes from WWTP and in a gram per
square km of the urban area per year (g km−2 a−1) for urban runoff.
2. Materials and methods These fluxes were used to approximate annual mass loading in a kilo-
gram (kg a−1) and tons per year (t a−1) of studied compounds from
Water sampling was performed in the Lopan River (the Seversky other cities in Ukraine including Lviv, Uzhorod and Chernivtsi, all of
Donets watershed, average discharge is 1 m3 s−1; detailed in the which discharge treated wastewaters into EU-transboundary rivers

Fig. 1. Location of study areas and sampling sites in Ukraine.

1360 Y. Vystavna et al. / Science of the Total Environment 637–638 (2018) 1358–1362

(Fig. 1). The employed approach is based on the assumption that Ukrai- Similar to EU rivers (Nagy et al., 2013; Sousa et al., 2018), naphthalene
nian cities have identical wastewater treatment (type of facilities, re- was the dominant component of PAHs in the Lopan River. This could
moval efficiency) and socio-economic (connection to sewerage, be attributed to its use as a precursor in the production of phthalic anhy-
industrial profile, consumption patterns) conditions (Report, 2015). dride, an important material with various industrial applications
(Azpíroz et al., 2008; Liu et al., 2017). Concentrations of Σ4 PCBs were
3. Results and discussion from 201.8 to 210.6 ng L−1 (Table 1). Low variation and a homogeneous
distribution in our sites suggest that PCBs originate from the atmo-
3.1. Occurrence and concentration sphere rather than a point source (Rossi et al., 2004; McKee et al.,
2017), perhaps deriving from the incineration of PCB-containing wastes
Our results show that among 17 priority substances and diclofenac, or evaporation from waste disposal sites (UNEP, 2016). In urban waste-
which were examined, 14 of them were detected in the Lopan River water, some PCBs may be discharged alongside effluents from the pro-
and were associated with urban runoff and treated wastewater efflu- duction of electrical goods, where they are used as dielectric and heat
ents (Table 1). Concentrations of several PAHs, i.e. fluoranthene, benzo exchange fluids, as additives in paint, carbonless copy paper, and plas-
(k)fluoranthene and indeno(1,2,3,-cd)pyrene and PCB 118 were less tics (UNEP, 2016). Contamination of the Lopan River was comparable
than the limit of the detection (LOD) in all sampled sites (Table 1). to urban and industrial sites in Europe where ΣPCBs are often higher
Trace metals concentration was from 17 to 50 ng L−1 for Cd, from 70 than 100 ng L−1 (Rossi et al., 2004; McKee et al., 2017). Downstream
to 150 ng L−1 for Pb and from 2060 to 5620 ng L−1 for Ni (Table 1). of the WWTP, concentrations of nonylphenol, octylphenol and
The presence of Ni and Pb in the Lopan River is mainly associated with diclofenac were notably higher than upstream and ranged from 50 to
insufficiently pre-treated industrial wastewaters, households (con- 2110 ng L−1 for NPEO2, from b10 to 110 ng L−1 for OPEO1 and from 4
struction, diet, washing, etc.) and incomplete removal of these sub- to 3560 ng L−1 for diclofenac. Measured concentrations exceeded the
stances in WWTPs, but also with traffic activity and atmospheric AA-EQS value by 36-fold for diclofenac and 7-fold for the nonylphenol.
deposition from fossil fuel burning (Vystavna et al., 2012b, 2013). The The NPEO2 concentration was also higher than the MAC-EQS value
Ukrainian EQS (Water Code of Ukraine, 1995), established for the stud- (Table 1) and was much higher (2110 ng L−1) than in many EU rivers
ied trace metals only, were not exceeded (Table 1). Concentrations of where concentration are usually b800 ng L−1 (Rocha et al., 2015; Loos
PAHs varied between compounds with a maximum of 67 ng L−1 for et al., 2007; Sousa et al., 2018). The OPEO1 concentration in the Lopan
naphthalene and Σ8 PAHs was from 13.9 to 81.2 ng L−1 (Table 1). River was close to the levels found in many EU rivers, being
Benzo(a)pyrene concentration was higher upstream (4.5 ng L−1) than b500 ng L−1 (Quednow and Püttmann, 2008; Sousa et al., 2018). This re-
downstream WWTP (2.9 ng L−1) and higher than the AA-EQS at three duction of nonylphenols and octylphenols in EU rivers has been ob-
sites (Table 1). Benzo(a)pyrene was dominance over benzo(g,h,i) served since 2005 due improved legislation that placed restrictions on
perylene (2.7-fold) and lower than the LOD level of indeno(1,2,3,-cd) use, emissions and losses of nonylphenols and the related ethoxylates
pyrene and fluoranthene indicated that PAHs have a pyrogenic origin, in the environment (Directive 2003/53/EC; Loos et al., 2007; Rusconi
mainly from coal combustion (Gevao et al., 1998; Delhomme et al., et al., 2015). Additionally, the presence of nonylphenols in the city cen-
2008; Launay et al., 2016). According to our results, concentrations of tre and upstream of Kharkiv city sites indicates their atmospheric origin
PAHs in the Lopan River were close to those observed in EU rivers. For (Björklund et al., 2009) and/or upstream contributions from agricultural
instance, the Σ8 PAHs detected downstream of the WWTP land and sub-urban influents. Diclofenac concentration downstream of
(81.2 ng L−1) is similar to that found in the Raba River, Hungary (aver- the WWTP in the Lopan River was higher than previously measured in
age Σ8 PAHs is 60.2 ± 41 ng L−1; Nagy et al., 2013) and the Odra River, many EU rivers with a concentration of generally b500 ng L−1 (maxi-
Czech Republic (average Σ17 PAHs is 172 ng L−1; Blahova et al., 2014). mum is 1500 ng L−1; Vieno and Sillanpaa, 2014). This may be explained

Table 1
Concentration and environmental quality standards of target compounds (average ± standard deviationa, exceeding EQS is in bold), ng L−1.

Substance Upstream City centre Downstream WWTP European Union Ukraine EQS

AA-EQS MAC-EQS

Cd 18 ± 3 17 ± 3 50 ± 3 90 600 5000
Pb 70 ± 5 80 ± 5 150 ± 5 1200 14,000 100,000
Ni 2060 ± 120 2200 ± 100 5620 ± 200 4000 34,000 10,000
Naphthalene b33 b33 67 ± 0 2000 130,000 n/a
Anthracene 9.4 ± 0.4 12.1 ± 0.5 11.3 ± 0.4 100 100 n/a
Fluoranthene b4 b4 b4 6.3 120 n/a
Benzo(a)pyrene 4.5 ± 0.1 4.1 ± 0.1 2.9 ± 0.1 0.17 270 n/a
Benzo(b)fluoranthene b1.3 2.6 ± 0.1 b1.3 n/a 17 n/a
Benzo(k)fluoranthene b8.9 b8.9 b8.9 n/a
Benzo(g,h,i)perylene b0.4 1.5 ± 0.0 b0.4 n/a 8.2 n/a
Indeno(1,2,3,-cd)pyrene b0.9 b0.9 b0.9 n/a
Σ8 PAHs 13.9 ± 0.3 20.3 ± 0.3 81.2 ± 1 n/a n/a
PCB 77 77.6 ± 1 76.9 ± 0.3 77.7 ± 2 n/a n/a
PCB 118 b0.20 b0.20 b0.20 n/a n/a
PCB 126 79.4 ± 1.9 78.4 ± 0.5 81.2 ± 5 n/a n/a
PCB 169 48.8 ± 3.4 46.5 ± 2.1 51.7 ± 10.1 n/a n/a
Σ4 PCBs 205.8 ± 6.4 201.8 ± 2.9 210.6 ± 17.1 n/a n/a
NPEO2 (nonylphenol) 50 ± 1 220 ± 8 2110 ± 10 300 2000 n/a
OPEO1 (octylphenol) b10 10 ± 0 110 ± 10 100 n/a n/a
Diclofenac 4 ± 0.1 98 ± 2 3560 ± 10 100b n/a n/a

n/a refers to that data are not available; LOD–limit of detection.

a
Standard deviation refers analytical variance.
b
Water quality limit.
 Y. Vystavna et al. / Science of the Total Environment 637–638 (2018) 1358–1362 1361

Table 2
Specific fluxes and annual mass loading (ML) of target compounds into rivers.

Chemicals Specific Specific Kharkiv, Lviv, estimated ML, Uzhorod, estimated Chernivtsi, Sum of three
fluxes from fluxes ML, kg kg a−1 ML, kg a−1 estimated ML, kg transboundary cities,
wastewater from a−1 a−1 estimated ML, kg a−1
effluents, g urban
ca−1 a−1 runoff, g
km−2 a−1

Cd 0.010 1.6 10.5 6.7 0.9 2.0 9.6

Pb 0.029 9.2 30.9 20.4 2.9 6.5 29.8
Ni 1.105 239.6 1175.7 762.5 108.2 236.1 1107
Naphthalene 0.013 2.0 14.2 9.1 1.3 2.8 13.2
Anthracene 0.002 1.5 2.2 1.6 0.2 0.6 2.4
Benzo(a)pyrene 0.001 0.4 0.5 0.4 0.1 0.1 0.6
Benzo(b)fluoranthene n/d 0.5 0.16 0.1 0.01 0.1 0.21
Benzo(g,h,i)perylene n/d 0.3 0.09 0.04 0.01 0.03 0.08
Σ8 PAHs 0.016 4.7 17.15 11.24 1.62 3.63 16.5
PCB 77 0.014 7.8 14.7 10.1 1.5 3.5 15.1
PCB 126 0.014 7.9 15.4 10.6 1.6 3.6 15.8
PCB 169 0.009 4.5 9.9 6.7 1.0 2.3 10.0
∑4 PCBs 0.037 20.2 40.0 27.4 4.1 9.4 40.9
NPEO2 (nonylphenol) 0.436 39.9 464.2 294.1 41.2 87.4 422.7
OPEO1 (octylphenol) 0.023 2.0 24.1 15.2 2.1 4.5 21.8
Diclofenac 0.738 19.7 785.8 491.7 68.4 142.8 702.9
Total amount 2.395 337.1 2517.3 1629.4 229.4 492.2 2351
EU-transboundary river, n/a n/a n/a Pltva, Western Bug Uzh River, Danube Prut River, Danube Western Bug and
watershed and basin watershed, Baltic Sea watershed, Black Sea watershed, Black Sea Danube watersheds
basin basin basin

n/d refers to that the substance was not determined (bLOD); n/a refers to that data is not applicable as the study site has no transboundary waters with EU. Calculated sum of substances is
in bold.

by a higher consumption rate of diclofenac in Ukraine (~3 g cap−1a−1; and seasonal monitoring of priority and emerging concern compounds
Vystavna et al., 2012a, 2017) than in the EU (b1 g cap−1 a−1; aus der in Ukraine/EU transboundary rivers.
Beek et al., 2016).
4. Conclusions

3.2. Fluxes and loading to EU-transboundary basins Our results indicate that aquatic concentration and fluxes of trace
metals (Cd, Pb and Ni), 8 PAHs, 4 PCBs, nonylphenols, octylphenols,
Specific fluxes of Cd and Ni from wastewater effluent in Ukraine and diclofenac from Kharkiv city, Ukraine are comparable to those in
(Table 2) were higher than those reported in France: 0.49 g ca−1 a−1 EU rivers. They show that studied priority and emerging concern com-
for Cd and 0.003 g ca−1 a−1 for Ni (Deycard et al., 2014), however, pounds could enter the EU-transboundary waters from treated urban
lower for Pb: 0.12 g ca−1 a−1 (Deycard et al., 2014). But specific fluxes wastewater in West Ukraine. Given this contamination threat, im-
of nonylphenols and octylphenols from treated wastewater into the proved transboundary water management is required and should in-
Lopan River (Table 2) are lower than those observed in an urban area clude preventive measures. Without this it may be impossible to reach
in France: 0.72 g ca−1 a−1 and 0.15 g ca−1 a−1, respectively (Bergé the established EU water quality standards.
et al., 2014).
Results of the mass loading estimation revealed that over 2.4 t a−1 of
Acknowledgments
target compounds, arising from urban runoff and wastewater effluent of
three cities (Lviv, Uzhorod and Chernivtsi) in West Ukraine could enter
This research has been partly granted by the Embassy of France to
the EU-transboundary waters. Highest loadings were found for trace
Ukraine (Bourse de Court Séjour de Recherche). One author was
metals (1.15 t a−1), particularly Ni (1.1 t a−1), diclofenac (0.70 t a−1)
granted by the United Nations Educational, Scientific and Cultural Orga-
and nonylphenols (0.42 t a−1). Mass loading of Σ4 PCBs and Σ8 PAHs
nization (UNESCO Contract No. 4500282119) in the framework of
was 0.04 t a−1 and 0.02 t a−1 respectively, and comprised of mostly
UNESCO IHP Program on Emerging Pollutants in Wastewater Reuse in
naphthalene (80% of the Σ8 PAHs) (Table 2). The enrichment in trace
Developing Countries, International Initiative on Water Quality (IIWQ)
metals, particularly in Cd and Ni, PAHs, PCBs and phenolic compounds
case study “Emerging pollutants in water and wastewater of East
in natural water has been previously observed in Western Ukrainian
Ukraine: Occurrence, Fate and Regulation”.
rivers (Lebedynets et al., 2005; Stolyar et al., 2008; Lukashev, 2010)
and at sites downstream of these rivers in other EU countries (Macklin
Appendix A. Supplementary data
et al., 2003; Harrad, 2009; Mihaiescu et al., 2016). Persistent organic
chemicals are highly mobile in aquatic environments (Sousa et al.,
Supplementary data to this article can be found online at https://doi.
2018) and thus can potentially contribute to river contamination in
org/10.1016/j.scitotenv.2018.05.095.
Poland, the Slovak Republic and Romania, and should be considered in
the management of transboundary water.
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