Microchemical Journal 85 (2007) 234 – 238

www.elsevier.com/locate/microc

Analysis of BTEX, PAHs and metals in the oilfield

produced water in the State of Sergipe, Brazil
Haroldo S. Dórea ⁎, José R.L. Bispo, Kennedy A.S. Aragão, Bruno B. Cunha, Sandro Navickiene,
José P.H. Alves, Luciane P.C. Romão, Carlos A.B. Garcia
Chemistry Department, Federal University of Sergipe, 49100-000, São Cristóvão, SE, Brazil
Received 3 February 2006; received in revised form 22 February 2006; accepted 1 June 2006
Available online 12 July 2006

Abstract

During oil and gas exploitation, large amounts of produced water are generated. This water has to be analyzed with relation to the chemical
composition to deduce the environmental impact of its discharge after a treatment process. Therefore, a study was carried out to evaluate preliminarily the
BTEX (benzene, toluene, ethylbenzene and xylenes), polycyclic aromatic hydrocarbons (PAHs) and metals contents in produced water samples taken
from effluents of the Bonsucesso treatment plant located in the city of Carmópolis, the most important oil and gas producer in the State of Sergipe, North-
east of Brazil. Three methods were optimized to determine the target compounds. Polycyclic aromatic hydrocarbons were determined by gas
chromatography with mass spectrometric detection (GC/MS), volatile aromatic hydrocarbons (BTEX) by gas chromatography with photoionization
detector (GC/PID) and metals were analyzed by flame atomic absorption spectrometry (FAAS). The results showed that concentrations of the target
compounds in these samples ranged from 96.7 to 1397 μg L− 1 for BTEX, from 0.9 to 10.3 μg L− 1 for PAHs and from 0.003 to 4540 mg L− 1 for metals.
© 2006 Elsevier B.V. All rights reserved.

Keywords: Purge and trap GC/PID; GC/MS; FAAS; Produced water; PAHs; BTEX; Metals

1. Introduction largest terrestrial petroleum production field and the fourth

Petroleum exploitation began 1961 in the State of Sergipe in
the city of Riachuelo, with activities of which extended rapidly
to other regions. The State of Sergipe is the third biggest petro-
leum producer in the Northeast region of Brazil. This activity is
very important to the local economy, being responsible for 40%
of gross regional domestic product. Today, petroleum produc-
tion is undertaken in both onshore and offshore operations [1].
Petroleum exploration and production in the Sergipe/Alagoas
region produces approximately 8500 m3 of crude oil per day,
5000 m3 of natural gas per day and 33,000 m3 of water per day.
Approximately 85% of this produced water is extracted in the
terrestrial platforms and is sent to the Bonsucesso treatment plant
located in the city of Carmópolis. The State of Sergipe is Brazil's
⁎ Corresponding author. Universidade Federal de Sergipe, CCET-Departa-
mento de Quimica, Av. Marechal Rondon, s/n. Jardim Rosa Elze CEP 49100-
000 Sao Cristovao/SERGIPE, Brazil. Tel.: +55 79 3212 6654; fax: +55 79 3212
6681.
E-mail address: hdorea@ufs.br (H.S. Dórea).
0026-265X/$ - see front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.microc.2006.06.002
biggest producer in the world, with an estimated production of
3600 m3 of crude oil per day and 28000 m3 of water per day.
A part of this water is re-injected into wells to extend the
production lifetime of the oilfield and the rest used to dissolve
salts generated by the Vale do Rio Doce Company, being sub-
sequently discharged to subsurface waters after treatment.
The production of oil and gas is usually accompanied by the
production of water. This produced water consists of formation
water, which is water naturally present in the reservoir, flood-
water previously injected into the formation and condensed
water, as a result of gas production [2]. Hence, produced water
is a by-product of the oil and gas exploitation and production
processes in terrestrial or offshore platforms. Large volumes of
this produced water are often generated because many oil
deposits reside in or around groundwater aquifers [3]. During
the lifetime of the oilfield, the amount of water may range from
seven to ten times the amount of oil produced [4]. The chemical
composition of this wastewater is dependent upon the
geological formation. It may contain various toxic compounds
of natural origin such as volatile aromatic fractions of the oil,
 H.S. Dórea et al. / Microchemical Journal 85 (2007) 234–238
including BTEX, polycyclic aromatic hydrocarbons (PAHs),
organic acids, phenols and alkylated phenols, metals, radio-
nuclides and a very high salt concentration.
Some studies have been described in the literature on chemical
characterization of produced water from offshore oilfield plat-
forms in China, Norway, Austria and the United States [5–10]. In
Brazil, limited monitoring has been carried out on naturally-
occurring compounds such as organic acids, phenols, metals,
PAHs and BTEX in produced water. Among them, there are
studies on the evaluation of different technologies for oilfield
wastewater treatments from the Campos Basin, State of Rio de
Janeiro [11,12]. However, there is a general lack of data on the
chemical composition of produced water from oilfields in the
State of Sergipe. The chemical composition of produced water is
field-dependent. So, the field-specific detailed chemical charac-
terization of produced water from each oilfield or platform is
necessary in order to predict the fate and effects of the produced
water discharged to the environment.
Taking into account the above considerations and considering
that, to date, no data on chemical composition of the oilfield
produced water in the State of Sergipe have been reported in the
literature, this paper provides a preliminary evaluation of the levels
of BTEX, PAHs and metals in the effluent of produced water from
the Bonsucesso treatment plant located in the city of Carmopólis,
State of Sergipe. This treatment station receives produced water
from a number of different petroleum production units.
2. Experimental
2.1. Chemicals and materials
Dichloromethane, acetonitrile and n-hexane were nanograde
(Mallinckrodt Baker, Paris, KY, USA). Certified standards of
BTEX (benzene, toluene, ethylbenzene and m-xylene, o-xylene
and p-xylene) were purchased from ChemService at concentra-
tion of 2000 μg mL− 1 in methanol (West Chest, PA, USA).
Intermediate solutions were prepared by diluting the standard
mixture at concentrations of 5 and 50 μg mL− 1 in methanol. The
deionized water used for preparing working solutions was puri-
fied by a Millipore (Bedford, MA, USA) Milli-Q water purifica-
tion system. Certified standards of the 12 PAHs were purchased
from AccuStandard (New Haven, CT, USA): naphthalene,
acenaphthene, phenanthrene, anthracene, fluoranthene, pyrene,
benzo[a]anthracene, chrysene, benzo[a] pyrene, perylene, benzo
[e] pyrene, benzo[g,h,i] perylene. The stock solutions of the PAH
were prepared in acetonitrile at 100 μg mL− 1 and stored at
−18 °C. The working standard solutions were prepared by diluting
the stock solutions in dichloromethane as required. All standards
were at least 99% pure. All stock solutions of metals (1000 μg
mL− 1) were stored in nitric acid-washed polyethylene bottles.
Analytical grade anhydrous sodium sulfate and silica-gel 60 (70–
230 mesh) were supplied from Merck (Darmstadt, Germany).
2.2. Sampling
Produced water samples were collected from the Bonsucesso
treatment station located in the city of Carmópolis (State of
235
Sergipe, Brazil). For PAHs, the volumes were 1 L in amber
glass bottles pretreated with acetone and methanol. For BTEX,
50 mL bottles were filled to capacity to avoid any headspace.
After filling with water, the bottles were sealed with Teflon-
lined screw caps and transported on the same day to the labo-
ratory under refrigerated conditions. In the laboratory, samples
were preserved at a temperature of 4 °C, and then diluted for
further analysis of BTEX. For metal analysis, samples were
collected in 1 L acid-washed polyethylene bottles. After filling
with water, the bottles were sealed with Teflon-lined screw caps
and transported on the same day to the laboratory under refrig-
erated conditions. In the laboratory, samples were preserved at a
temperature of 4 °C before utilization.
2.3. Sample preparation
The samples for PAHs and BTEX analyses were not filtered.
Before metal analysis, the samples were filtered through a
0.45 μm Millipore filter. Determination of ammonia was made
using the indophenol blue reaction, while the azide-Winkler
method and electrical conductivity were used to measure dis-
solved oxygen and salinity, respectively.
2.4. Apparatus
2.4.1. Purge and trap conditions
A Tekmar–Dohrmann velocity XPT purge-and-trap (Mason,
Ohio, USA) was used to pre-concentrate the BTEX in produced
water. The P and T unit consists of a 5 mL stripping vessel. No
cryogen was needed for BTEX trapping, using Tenax TA as
adsorbent trap. The water sample was purged with helium
(99.995% purity) at 40 mL min− 1 during 11 min at 26 °C. The
volatiles were thermally desorbed (180 °C, 4 min), and transferred
to the GC/PID-FID via a transfer line heated to 100 °C. After
desorption, the trap was cleaned by heating at 200 °C for 8 min.
2.4.2. GC/PID-FID conditions
A Shimadzu 17A gas chromatograph (Kyoto, Japan) equipped
with photoionization (PID) and flame ionization (FID) detectors
and a split/splitless injector was used for quantification of BTEX.
A fused-silica megabore column, DB-624 (6% cyanopropyl-
phenyl–94% dimethylpolysiloxane; 75 m × 0.53 mm I.D.,
3 μm), supplied by J and W Scientific (Folsom, CA, USA),
was employed, with helium (purity 99.995%) as carrier gas at a
flow-rate of 10 mL min− 1 . The column temperature was
programmed as follows: 30 °C for 1 min, increasing to 100 °C
at 5 °C min− 1 and directly to 220 °C at 8 °C min− 1 then holding for
5 min. The injection port and detector were operated at 180 and
220 °C, respectively. The PID system was operated with a 10 eV
bulb and at an intensity of 1 mA.
2.4.3. Flame atomic absorption spectrometric conditions
A Shimadzu (Kyoto, Japan) AA-6800 flame atomic
absorption spectrophotometer equipped with BCG-D2 back-
ground correction was used for determining the metals. The
instrumental adjustments were determined according to the
recommendations of the manufacturer.
236 H.S. Dórea et al. / Microchemical Journal 85 (2007) 234–238
2.4.4. GC/MS conditions
A Shimadzu system consisting of a QP-5050A mass spec-
trometer equipped with a GC-17A gas chromatograph with a
split/splitless injector was used for the quantification and
confirmation of the polycyclic aromatic hydrocarbons. A fused-
silica column, DB-5 ms (5% phenyl-95% dimethylpolysilox-
ane; 30 m × 0.25 mm I.D., 0.25 μm), supplied by J and W
Scientific (Folsom, CA, USA), was employed with helium
(purity 99.995%) as carrier gas at flow-rate of 1.5 mL min- 1.
The column temperature was programmed as follows: 40 °C for
1 min, increasing to 160 °C at 25 °C min- 1 and directly to
300 °C at 5 °C min- 1 and holding for 6 min. The solvent delay
was 5 min. The injector port was maintained at 250 °C and 1 μL
volume was injected in splitless mode (1.0 min). The data were
acquired and processed by the Shimadzu Class 5000 software.
The effluent from the GC column was transferred via a transfer
line held at 280 °C and fed into a 70 eV electron impact
ionization source held at 280 °C. The analysis was performed in
the selected ion monitoring (SIM) mode.
2.5. Methods
2.5.1. Procedure for BTEX analysis
An analytical aliquot of 5 mL of produced water with 10 μL
of α, α, α-trifluorotoluene (surrogate) was transferred to the P
and T port without air bubbles. The sample was purged with
helium and the volatiles were trapped on the Tenax adsorbent
and thermally desorbed into the GC/PID system.
2.5.2. Procedure for polycyclic aromatic hydrocarbon analysis
An analytical aliquot of 1000 mL of produced water sample
was placed in a separating funnel. 30 mL of n-hexane were
added and the mixture was extracted for 20 min in a manual
shaker. The residue was re-extracted with another 2 × 30 mL of
n-hexane. The extract was concentrated using a rotary
evaporator (35 °C) and was transferred to at chromatographic
column filled with 0.5 g of silica-gel (200–325 mesh) and 5 g of
anhydrous sodium sulfate. The PAHs were eluted with 20 mL of
n-hexane:dichloromethane (70:30, v/v) mixture and evaporated
to nearly 0.1 mL under a gentle stream of nitrogen. The residue
was dissolved in dichloromethane (1 mL) and an aliquot (1 μL)
was analyzed by GC/MS.
2.5.3. Procedure for heavy metal analysis
After the metals had been extracted from the matrix using the
ammonium pyrrolidine dithiocarbamate (APDC) in methyl
isobutyl ketone (MIBK) method [13], the metals were measured
in the organic phase by FAAS.
3. Results and discussion
3.1. General comments
This study reports on results obtained from a survey of
wastewater from the Bonsucesso produced water treatment
plant for the levels of BTEX, PAHs and metals in the effluent.
This treatment plant was selected because it contributes a
high percentage of the total amount of produced water dis-
charged into subsurface waters from the oilfields of the State
of Sergipe.
3.2. BTEX analysis
The above described extraction procedure was developed on
the basis of EPA method 524.2 (purgeable organic compounds
by the PT technique) [14]. To find the extraction conditions
providing the highest yields of BTEX from the produced water
and to validate the method for the simultaneous determination
of these analytes, some parameters of the purge and trap system
and of the chromatograph were optimized: Purge and desorption
times and temperatures; transfer line and column temperatures;
detector selection (PID or FID). The m-and p-xylenes were not
separated and were determined together.
After the definition of the analytical conditions for the PT-
GC/PID-FID, a study of comparison was performed between the
two gas chromatographic detection systems (PID and FID) to
find the detector providing the highest sensitivity using standard
solutions at 4 ng mL− 1. Considering the results, PID showed
higher sensitivity ranging from 5.6 (for the ethylbenzene) to 7.2
(for the m + p-xylenes) times greater than FID. Hence, PID was
chosen for determining BTEX in produced water.
Recovery assays were done in triplicate by spiking produced
water samples at two levels (4 and 40 μg L− 1). The mean
recoveries obtained with spiked samples at the 4 μg L− 1 level
ranged from 105.5% to 138.6%, with relative standard devia-
tions (RSD) between 10% and 19.8%, while at 40 μg L− 1
recoveries ranged from 99.9% to 104.3%, with RSD between
1.2% and 3.5%. Surrogate standard was added to each extraction
to control any losses during the analysis procedures. Addition-
ally, each analytical sequence included quality control standards
and blanks to check noise and background levels, possible
carryover effects and to cover small retention time variations.
Six point (average of three injections) calibrations (based on
peak areas) were obtained over the concentration range of
interest (2–200 μg L− 1 for m + p-xylenes and 1–100 ng mL− 1
for other species). Calibration curve correlation coefficients
were higher than 0.9998 in all cases. The analytical calibration
curves were used for quantification purposes using the external
standards procedure. The limits of detection (LODs) were verified
by analyzing the BTEX mixture at 0.5 μg L− 1. LODs ranged from
0.06 μg L− 1 for xylenes to 0.12 μg L− 1 for benzene, while the
limits of quantification (LOQs) ranged from 0.21 μg L− 1 for
xylenes to 0.41 μg L− 1 for benzene.
3.3. Polycyclic aromatic hydrocarbon analysis
The liquid–liquid extraction procedure described above was
developed on the basis of the EPA 3510 and 8270C methods
[15,16] and the Reddy and Quinn procedure [17]. The pro-
cedures given in these sources were modified and further im-
proved for produced water analysis. Positive identification of
the total PAHs was achieved first by mass spectral identification
and then by acquisition of standard PAHs and comparison with
unknown GC retention times.
 H.S. Dórea et al. / Microchemical Journal 85 (2007) 234–238 237

Table 1 3.5. Real produced water samples

Concentrations of PAHs and BTEX in produced water collected from the
Bonsucesso treatment plant, State of Sergipe
The developed methods were applied to the determination of
Compound Concentration (μg L− 1) target compounds in produced water samples collected from the
Range Average⁎ Bonsucesso treatment plant effluent. Target compounds levels
Minimum Maximum above the detection limits were found. Tables 1 and 2 contain a
Naphthalene 9.9 10.7 10.3 summary of the occurrence and concentrations of target com-
Acenaphthene 1.6 2.4 2.0 pounds in produced water samples. These data reflect mainly
Phenanthrene 2.2 2.4 2.3 the presence, at the highest concentration, of BTEX, although
Anthracene 0.8 1.7 1.3 the presence of PAHs was also detected. Individual PAH
Fluoranthene 2.7 6.2 4.4 concentrations ranged from 0.9 to 10.3 μg L− 1, with total PAHs
Pyrene 0.9 1.0 0.9
Benzo[a]anthracene 1.6 1.9 1.7 of 37.4 μg L−1. In earlier work, UV-fluorescence was used to
Chrysene 5.9 9.9 7.9 determine PAHs in seawater from different coastal areas in
Perylene 1.6 2.6 2.1 Brazil, with a range from <0.04 to 52.43 μg L− 1 [20]. Utvik
Benzo[e] pyrene 2.4 2.6 2.5 et al [18] evaluated concentrations of produced water originated
Benzo[g,h,i] perylene 0.9 3.1 2.0
PAHs in the marine environment of the North Sea. Measurable
Benzene 1291 1511 1397
Toluene 1167 1357 1263
concentrations of PAHs in produced water included a notable
Ethylbenzene 136 158 148 proportion of alkylated PAHs, in addition to the parent PAH
m + p-xylenes 194 242 216 compounds, from the Norwegian Brage field, North Sea, with a
o-xylene 89 103 96 total range from 0.2 to 350 μg L−1. Discharged PAHs were
⁎ n = 3 replicates. readily diluted by receiving waters, so that PAH concentrations
in the ocean typically reach near background levels a short
distance from the discharge point. In addition, processes such as
Five point calibrations were performed at 10, 15, 20, 25 evaporation, sedimentation, adsorption, chemical oxidation,
and 50 μg L− 1. The regression coefficients show good linear- photo-oxidation and biodegradation contribute to lowering PAH
ities in the concentration range under consideration, allowing concentrations in the surrounding seawater. The total PAHs
quantification of these compounds by the method of external evaluated at that site were in the range of 0.002–0.01 μg L− 1 for
standardization. the non-impacted locations.
The LODs were defined as a response three times the There is scarce information available on the concentration
average height of the blank baseline noise and the LOQs were levels of PAHs in produced water from Brazilian oilfields,
defined as a response ten times the average height of the blank however the levels recorded in this study for the PAHs in pro-
baseline noise. So, the results were between 5 and 15 μg L− 1 for duced water are higher than those found in some other locations,
LOD and between 15 and 40 μg L− 1 for LOQ. such as Western Xiamen Bay in China (0.106–0.945 μg L− 1 in
The herein reported results are based on an unfortified sub-surface marine water) or the Baltic Sea and the Seine River
sample and three samples fortified with 1.0 μg L− 1 of each
PAH. All experiments showed mean recoveries in the range
from 62.1% to 113.6%, except for the phenanthrene, for which
Table 2
recoveries exceeded 120%. Relative standard deviations were
Concentrations of metals, and hardness, salinity and density of produced water
between 14.3% and 29.5%. collected from the Bonsucesso treatment plant, State of Sergipe, and from the
North Sea
3.4. Heavy metal analysis Parameter Carmópolis, Sergipe (mg L− 1) North Sea⁎⁎
(mg L− 1)
Range⁎
The predominant inorganic components associated with
produced waters are dissolved salts, which many times exceed Minimum Maximum Average
that of seawater. For instance, the concentration of chloride ex- Pb 0.003 0.003 0.003 <0.500
ceeds the concentrations of other anionic produced water species Co 0.003 0.004 0.003 <1.00
Cu 0.001 0.001 0.001 <0.001–0.100
(for the greater part by a factor of 1000 and more). Therefore,
Fe 4310 4770 4540 4.50–6.00
while quantification of major ionic components such as chloride Mn 0.058 0.068 0.062 Not analyzed
or sodium exhibits no significant problem, it is far more chal- Ni 0.015 0.017 0.016 <0.300
lenging to monitor anions or cations occurring in produced water Zn 0.027 0.028 0.027 0.005– 35.0
at lower and especially much lower concentrations. Regarding this Cl 16,100 19,500 17,800 44,600
K 3100 4900 4000 Not analyzed
analytical task, produced water can be categorized as a complex
Na 8800 9600 9200 Not analyzed
sample and hence often forces an analytical method to operate Hardness of water, 4890 5130 5010 7000
very close of the performance limit. CaCO3
In this work, recovery assays of seven metals were done by Salinity, NaCl 31,700 4110 36,400 58,500
spiking water samples at 5 μg mL− 1. Recoveries ranged from Density, 20°C 1010 1070 1040 Not analyzed
97% for Ni to 104% for Cr. ⁎n = 3 replicates; ⁎⁎Ref. [21].
238 H.S. Dórea et al. / Microchemical Journal 85 (2007) 234–238
and Estuary (France), where values ranged from 0.0003 to
0.0005 ng L− 1 and 0.004 to 0.036 μg L− 1, respectively. How-
ever, the present concentrations are lower than found in Daya
Bay, China, (range 4.2–29.3 μg L− 1) [19].
BTEX mean levels found in our study were between 96.7
and 1397 μg L− 1. Results of these samples were given as the
sum of m- and p-xylenes, because these isomers show similar
recovery and response. These findings are of the same order of
magnitude as those reported by other authors, such as in the
effluent of produced water from platforms of two different
petroleum production units located in the Campos Basin, State
of Rio de Janeiro, Brazil (283–1855 mol L− 1 for benzene,
87.04–2224 mol L− 1 for toluene, 16.77–1220 mol L− 1 for
ethylbenzene and 67.35–5969 mol L− 1 for xylenes) [11]. For
comparison, 1318 μg L− 1 for benzene and 1065 μg L− 1 for
toluene were detected in oilfield wastewater from platforms of
the Gulf of Mexico [7], and in Norway total BTEX of 8000 μg
L− 1 was measured [5].
Metal mean levels found in our study are of the same order of
magnitude as those reported by Ray and Rainer [21].
4. Conclusions
This paper describes the evaluation of PT-GC/PID, GC–MS
and FAAS for the determination of BTEX, polycyclic aromatic
hydrocarbons and metals of environmental interest, respectively,
in produced water samples. The reliability and performance of
the analytical methods were checked by determining the detec-
tion and quantification limits, precision and accuracy. Concen-
tration levels ranged from 96.7 to 1397 μg L− 1 for BTEX, from
0.9 to 10.3 μg L− 1 for PAHs and from 0.003 to 4540 mg L− 1 for
metals, in produced water samples collected from the Bonsu-
cesso treatment station. The salinity of produced water was
about 36 g L− 1. The work was restricted to produce water
samples only from the city of Carmópolis. More detailed moni-
toring studies have to be carried out on different oil production
units, covering a wider spectrum of chemical classes, to obtain a
detailed chemical characterization of the produced water from
oilfields in the State of Sergipe.
Acknowledgements
The authors gratefully acknowledge Dr. Andrew Allen
(University of Birmingham) for his assistance with the English
in this manuscript and the Petrobras/Unseal, CNPq/PIBIC,
FAPITEC-SE/FUNTEC and the FINEP for financial support of
this study. We also would like to thank the Bonsucesso treat-
ment station located in the city of Carmópolis, State of Sergipe,
for the produced water samples.
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