151e156

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Journal of Environmental Management

j o u r n a l h o m e p a g e : w w w. e l s e v i e r. c o m / l o c a t e / j e n v m a n

Research article

Removal optimization of heavy metals from effluent of sludge

dewatering process in oil and gas well drilling by nanofiltration
Mostafa Hedayatipour a, Neemat Jaafarzadeh b, *
, Mehdi Ahmadmoazzam b, c

a
Department of Chemical Engineering, Mahshahr Branch, Islamic Azad University, Mahshahr, Iran
b
Department of Environmental Health Engineering, Ahvaz Jundishapur University of Medical Sciences, Ahvaz, Iran
c
Student Research Committee, Ahvaz Jundishapur University of Medical Sciences, Ahvaz, Iran

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

Article history: Oil and gas well drilling industries discharge large volumes of contaminated wastewater produced
Received 30 March 2017 during oil and gas exploration process. In this study, the effect of different operational variables,
Received in revised form including temperature, pH and transmembrane pressure on process performance of a commercially
24 July 2017
available nanofiltration membrane (JCM-1812-50N, USA) for removing Ba, Ni, Cr, NaCl and TDS from
Accepted 26 July 2017
produced wastewater by dewatering unit of an oil and gas well drilling industry was evaluated. In op-
Available online 4 August
2017 timum experimental conditions (T ¼ 25 C, P ¼ 170 psi and pH ¼ 4) resulted from Thaguchi method,
85.3,
Keywords:
Nanofiltration 77.4, 58.5, 79.6 and 56.3% removal efficiencies were achieved for Ba, Ni, Cr, NaCl and TDS, respectively.
Heavy metal Also, results from a comparison of the Schuller and Wilcox diagrams revealed that the effluent of the
Thaguchi method membrane system is usable for drinking water, irrigating and agriculture purposes. Moreover, the pro-
Well drilling industry cess effluent quality showed a scaling feature, according to Langelier saturation index and illustrated that
Wastewater the necessary proceedings should be taken to prevent scaling for industrial application. The nano-
treatment
filtration membrane process with an acceptable recovery rate of 47.17% represented a good
performance in the wastewater treatment.

1. Introduction
Oil and gas well drilling industries generate large volumes of
solid and liquid waste materials. One of the most principal prob-
lems relating to these industries is pollution caused by discharge of
drilling wastes into the soil and water resources (Saint-Fort and
Ashtani, 2014). Loss of plants and animals ecosystems, rivers and
also pollution of groundwater resources, due to the salt marsh
creation around the drilling land is one of the main
environmental problems of these industries (Bakke et al., 2013;
Bamberger and Oswald, 2012). Drilling waste includes drilling
cutting, drilling fluid, consuming water, cement and oil and
lubricants used in machines (Fakhru'l-Razi et al., 2009;
Oreshkin et al., 2015). The produced water during dewatering of
drilling waste is a large waste stream generated in oil and gas well
drilling industries. There are lots of contaminants in drilling
wastes including heavy metals (chromium, nickel, cadmium,
arsenic, barium, mercury, vanadium,
* Corresponding author. Ahvaz Jundishapur University of Medical Sciences,
Golestan Avenue, 61357-15794, Ahvaz, Iran.
E-mail address: Jaafarzadeh-n@ajums.ac.ir (N. Jaafarzadeh).
http://dx.doi.org/10.1016/j.jenvman.2017.07.070
0301-4797/© 2017 Elsevier Ltd. All rights
reserved.
iron, etc.), as well as high levels of soluble salts, grease, petroleum
hydrocarbons, which caused great environmental concerns (Bakke
et al., 2013; Fakhru'l-Razi et al., 2009; Hu et al., 2012). Therefore,
treatment and reuse of the produced wastewater in oil and gas
well drilling industries, using a cost-effective and
environmental- friendly approach is essential for sustainable
industrial develop- ment (Coday et al., 2014).
Heavy metals and the inorganic pollutants may cause either
environmental or health problems, if discharged in surface and
subsurface water resources, even at very low concentrations
(Esmaeili et al., 2014; Gherasim and Mikula sek, 2014; Ong et
al.,
2013). Removal of heavy metals from aqueous solution has been
considered as an important issue in water pollution control
(Diagomanolin et al., 2004). Until now, a wide number of remedi-
ation techniques have been applied for removal and recovery of
heavy metals from aqueous solutions including chemical precipi-
tation (Gonzalez-Munoz et al., 2006), ion exchange (Dabrowski
et al., 2004), electrochemical methods (Parga et al., 2005), coagu-
lation and flocculation (Johnson et al., 2008), adsorption on
various sorbents (Aguado et al., 2009) and membrane filtration
(Farooq et al., 2010; Wang et al., 2010). Nowadays, membrane
processes have been considered in the removal of heavy
152 M. Hedayatipour et al. / Journal of Environmental Management 203 (2017)
151e156

essence to, their good performance, simplicity and easy to scale up Table 2
Operational flows and variables under the 16 test conditions of the Taguchi L16
and control, no changing in phases, high operational efficiency, 3
(4 )
environmental-friendly and energy-saving (Zhu et al., 2014). orthogonal array.
1
However, micro filtration (MF) and ultra filtration (UF) have low Test condition Variable Operational flow (L min )
rejection potential and little potential to remove heavy metals T ( C) P (psi) pH Qin (avg) Qout (avg)
(Muthukrishnan and Guha, 2006). Application of reverse osmosis
1 20 110 2 0.97 0.12
(RO) has been limited in wastewater treatment zones, because of 2 20 130 4 1.2 0.2
the lower discharge, high pressure need and higher energy con- 3 20 150 6 1.36 0.31
sumption, despite the high performance (Murthy and Chaudhari, 4 20 170 8 1.38 0.44
2008). Nanofiltration (NF) which uses membranes with very 5 25 110 4 1 0.14
6 25 130 2 1.29 0.39
small pores (<1 nm) and requires operating pressures in the 7 25 150 8 1.32 0.37
10e50 bar range has been used as a growing technology for the 8 25 170 6 1.4 0.49
removal of heavy metals in water and wastewater treatment, due 9 30 110 6 1.1 0.11
to the high performance and low power consumption (Gherasim 10 30 130 8 1.22 0.28
11 30 150 2 1.36 0.43
and Mikul a sek, 2014). Also, NF has higher rejections to
12 30 170 4 1.43 0.55
multivalent heavy metal ions than UF membranes, because of its 13 35 110 8 1.15 0.17
unique sep- aration mechanisms (size exclusion and Donnan 14 35 130 6 1.33 0.31
exclusion) (Maher et al., 2014). NF is an energy-saving process in 15 35 150 4 1.29 0.44
comparison with RO membranes, because of its much lower 16 35 170 2 1.5 0.48

operating pressure (Zhu et al., 2014). However, the adverse and

destructive effects of dril- ling waste discharge can be reduced
with simple and low-cost proceedings. The application of a
membrane unit in waste man- agement system is one of these
proceedings. The effluent of the dewatering unit which contains
high concentrations of environ- mental contaminants can be
applied as a feed of the membrane unit. To the best of our
knowledge, no research has been conducted on the feasibility of
using nanofiltration membrane technology for wastewater
treatment of sludge dewatering process in oil and gas well
drilling industries. Therefore, this research was aimed at the
performance evaluation of NF process in removing three important
heavy metals; Ni, Cr and Ba, as well as NaCl and TDS from effluent
of dewatering process in oil and gas well drilling industries
in different operating conditions and also process optimization
using the Taguchi method.
2. Materials and methods
2.1. Set-up and operation of membrane
system
The experiment was performed in a lab-scale nanofiltration
membrane system. The system was operated in continuous mode
with the constant return and both permeate and reject streams
were returned to the feed tank in order to keep the concentration
constant in each step. NF module was equipped with a spiral
membrane made in the USA. The characteristics of the applied
membrane are illustrated in Table 1.
Samples were collected from the effluent of a sludge
dewatering unit of a waste management system situated close to
the drilling rigs in one of the Iranian south west oil fields close
to Ahvaz city. The Samples were gathered at different days and
times, mixed together and then a specific amount of them was
sent to the lab- oratory for using in the membrane filtration
process. At each stage,
Table 1
Characteristics of the NF membrane used.
Membrane structural parameters
Material Polyamide
Module Spiral
Maximum operating temperature 40 C
Maximum operating pressure 300 psi
pH operating range
2e11
Maximum operating flow 7.6 L min
1 literature. Sixteen test conditions were designed according to the
Active surface 0.32 m
2 L16 (4 ) orthogonal array. The experiments were repeated twice
Model number JCM-1812-50N
500 ml of the membrane effluent was taken and used for analysis.
Important parameters including temperature, transmembrane
pressure and pH were considered as the operational variables.
The operating range for each parameter was selected based on
the membrane operating range and preliminary studies. In order
to prevent clogging the membrane was washed using 1M HCl
solution and then neutralization was done using 1 N NaOH
solution after membrane rinsing.
2.2. Analytical methods
All chemicals used in this study were of analytical grade and
purchased from Merck (Germany). pH was measured by a
portable pH-meter (Hanna, Romania). TDS and EC measurements
were done using a portable TDS/EC-meter (Hach, USA).
Concentrations of metals were measured using a flame
atomic absorption with detection limit of about 0.5 mg/L
(Analytic jena-5 FL, Germany). Anions were measured
according to procedures described in standard methods for
examination of water and wastewater (Eaton et al., 2005). All
experiments were repeated twice and the mean values were
reported.
2.3. Design of study with Taguchi method
The Taguchi method was used to find the optimum experi-
mental factors affecting the experiment (Taguchi et al., 2005).
This method is a combination of the statistical and
computational methods which has been widely applied in
experimental studies. The most important characteristic of this
method is its economical nature for testing the complex
processes. The minimum number of experiments is used to study
all levels of operational variables and separating the effects of
simultaneous changes of operational var- iables along with
process optimization are possible. In Taguchi method, S/N ratio
can be used to express the impact of each vari- able, where N is
the mixing factor and is an expression of the dif- ficulty in
controlling the evaluated variable and S is the signal factor and
shows the simple control of the evaluated variable (Yang and
Tarng, 1998). In this study, Qualitek-4 software was used to
design experiments, according to Taguchi method. Three control
factors with four levels were selected, based on the available
3
to
calculate the experimental error and S/N ratio. Also the tests were
 M. Hedayatipour et al. / Journal of Environmental Management 203 (2017) 153
151e156

illustrates the experimental conditions and variables with the
corresponding levels.
2.4. Data analysis
There are two methods for analyzing the experimental data
namely analysis of variance (ANOVA) and signal to noise ratio
(S/N). The signal to noise ratio is used where the amount of S/N
shows the dispersion around a certain value and that how the
responses have been changed in several tests. The purpose of
ANOVA is to inves- tigate which of operational variables are
important if their effect is significant compared to error (Wilcox,
2003). The signal to noise ratio was calculated using equation (1)
and in this case, a higher S/N ratio shows better results.
1 Xni
S=Ni ¼ 10 log 1 (1)
ni i¼1 yi2
where, n represents the number of test repeats and y indicates the
test responses.
2.5. Determination of recovery and rejection rates
The rejection rate was calculated using equation (2):
3.1. Effect of transmembrane
pressure
The effect of transmembrane pressure on the performance of NF
is depicted in Fig. 1 (a) as S/N ratio variations. Pressure increasing
to
170 psi in all cases caused an increase in the removal rate and
also proved that pressure is a decisive factor in the removal of
all pa- rameters. This phenomenon could be due to enhancement
in the solvent passage which is derived from increasing pressure
and as a result, increase in solutes rejection (Al-Rashdi et al.,
2013; Gherasim and Mikula sek, 2014). Results from a similar
study showed that Ni rejection increased from 72 to 97%,
when the pressure witnessed an increasing trend from 4 to 20
bar (Murthy and Chaudhari, 2008). The removal rate was almost
constant for the pressure higher than 150 psi and TDS removal
rate also showed a slight decreasing trend from 150 to 170 psi. This
observation could be due to the increase in concentration
polarization and membrane fouling. One of the reasons for
increasing fouling by the elevated pressure is compressing
membrane surface in high pressure. High pressure can also
import particles into the membrane and lead to membrane
clogging (Gherasim and Mikula sek, 2014; Maher et al.,
2014). A similar study reported that the rejection of metal ions
slightly increased with the operating pressure, and slightly
decreased with increasing the metal concentration in the feed
3.2. Effect of temperature

% Rejection ¼ 1 Cp 100 (2) The water temperature is an important parameter in NF mem-

CF
where, Cp and CF are permeate concentration and feed concentra-
tion respectively. And recovery rate is defined as follows:
% Recovery ¼ Qp 100
QF
where Qp and QF are permeate flow and feed flow rates in L min
1 TDS was at 20 C and their removal rate was reduced at higher
respectively.
3. Results and discussion
The performance of the NF process for removal of heavy metals
(Ba, Cr and Ni), NaCl and TDS under different test conditions
based on the Taguchi method is shown in Table 3. According to
the ob- tained data, the study was divided into two separate
steps. In the first step, the optimum experimental conditions
were determined for individual removal of each parameter
and simultaneous removal of all parameters. In the second step,
the NF performance was evaluated in the optimum
experimental conditions of maximum removal for NaCl (as the
priority parameter) for simul- taneous removal of all parameters.
Also, the NF effluent quality for reuse goals was determined using
the Wilcox and Schuller diagram and Langelier saturation index.
brane operation which significantly affects the membrane flux and
removal efficiency. Fig. 1 (b) shows the influence of different tem-
peratures on removal rate of all parameters. It is observed
that
increasing temperature did not lead to the enhancement of the
(3) removal rate for all parameters. Ni was the only parameter which
showed an increase in its removal rate with increasing the tem-
perature from 20 to 35 C. The maximum removal rate for Ba and
temperatures. The optimum temperature for NaCl and Cr was
observed at 25 C and higher temperature showed a negative
effect on their removal rates. This possibly can be attributed to
the fact that the high temperature can lead to increasing the
membrane pore size (especially polymeric membranes) and
which will cause reduction of the membrane resistance against
the transition of soluble components and also decreasing the
removal rate (Tsuru et al., 2000). Furthermore, membrane
fouling increases with increasing temperature, because of the
influence of higher tem- perature on deposition of materials on
the surface and membrane pores.
3.3. Effect of pH
The influence of pH on membrane performance was studied at
four pH levels. The removal rate of NaCl and Ba was almost
constant until the solution pH was 4. While, by increasing solution
pH from 4

Table 3
Parameters removal rate (%) under different test
conditions.
a
Removal (%) Test conditions

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16

NaCl 61 57.4 59.5 48.2 67.4 60.2 48.9 70.5 51.8 37.7 55.8 58.1 41.5 55.8 59.2 63.4
Ba 78.3 81.5 68.8 54.2 82.1 67.05 57.8 65.4 66 44.4 66.3 80 52.4 67.5 83.7 75
Cr 23.7 29.8 56.7 77.8 32.3 27.5 78.4 55.4 49.3 64.8 28.5 37.7 78.9 42.5 31 26.4
Ni 37.8 63.2 62.3 75.2 51.6 43.3 65.5 79.05 68.05 83.2 49.2 80.3 71.1 78.1 75.6 58.6
TDS 39 43.7 47 41.9 33.6 42 39 43.4 33.9 28.9 50.2 48.4 29.8 33.7 45.6 46.2
a
See Table 2 for test conditions.
154 M. Hedayatipour et al. / Journal of Environmental Management 203 (2017)
151e156

38 38
(a) (b)
36
36
S/N ratio

34

S/N ratio
34
32 NaCl Ba
Cr Ni 32
30
NaCl Ba Cr
TDS
Ni TDS
28 30
110 130 150 170 20 25 30 35
Pressure Temperature

39 (c)

37

35
S/N ratio

33

31

29 NaCl Ba Cr
Ni TDS
27
2 4 6 8
pH

Fig. 1. The effect of pressure (a), temperature (b) and pH (c) on the removal rate of all parameters at all levels as S/N ratio.

to 8, a decrease was happened in NaCl and Ba removal (Fig. 1 (c)).
In
addition, increasing the solution pH decreased the TDS removal
rate at all levels. The solubility of metals depends on the pH and
the rate of solubility also has a direct relationship with the
molecular mass (Paugam et al., 2004). As shown in Fig. 1 (c) the
removal rate of Cr and Ni was increased with increasing the pH
from 2 to 8. This can be due that in high pH values, Cr and Ni
may precipitate and thus are more removed. Also, when the
hydroxyl ions (OH ) in- crease in alkaline pH, the accumulation
of negative charge at the membrane surface may increase and
cause increased ion electro- static repulsion (Wang et al., 2007).
Muthukrishnan et al. found that the separation of Cr in
nanofiltration process mainly depends on the pH and the
concentration of the chromium solution. Their re- sults showed
that the rejection was increased from 84 to 99.7% by changing the
solution pH from acidic to alkaline (Muthukrishnan and Guha,
3.4. Determination of the optimum experimental conditions
The optimum experimental conditions for each parameter were
selected, according to the results of the S/N ratio from the Taguchi
method (Fig. 1) and ANOVA (Table 4) for all variables. Then, the
experiments were carried out in optimum experimental conditions
of all variables, and the removal rate was obtained for each
parameter. Since, the optimal experimental condition is that NaCl
has the least concentration (for environmental problems caused
by NaCl in high concentration), therefore, the optimum
experimental conditions for NaCl removal were considered as
the optimum experimental conditions for removal of all
parameters. Table 5 shows the removal rates obtained in
optimum experimental con- ditions for each parameter (test
condition 1 to 5), the removal rate in optimum experimental
conditions for NaCl removal (test
condition 1) and for all parameters. As shown in Table 4, pH is the
most important variable in the removal of all parameters,
therefore it was observed that the removal rate of Cr and Ni
showed a decreasing trend from 81.3 to 58.5% and 89.5 to 77.4%,
respectively in optimum experimental conditions for removal of
each parameter and all parameters. Other studies have also
emphasized on this point that the NF performance is influenced
by operating variables pH, temperature and transmembrane
pressure, and therefore determination of optimum experimental
conditions should be considered (Al-Rashdi et al., 2013; Go€ nder
et al., 2010; Maher et al.,
3.5. Nanofiltration performance evaluation
Separation process in NF membrane is based on the screening
mechanism and also different reactions such as Donnan potential,
adsorption and excretion of ions through the membrane which
can be effective in removal of various ions. These reactions
depend on the properties of the influent and membrane structure.
Since most of the membranes have negative charge,
interactions between membrane and solution play an important
role in separating the substances and minerals, especially heavy
metals, from solution (Zhu et al., 2014). Table 6 shows the
concentration of the measured parameters in the feed and
permeate of NF process and their removal rate in optimum
experimental conditions. The maximum removal rate among the
heavy metals was observed for Ba (85.3%) and the removal rate
was 77.4 and 58.5% for Ni and Cr respectively, in the optimum
experimental conditions selected based on the maximum
removal of NaCl. One of the reasons that leads to removal
rates lower than 90e100% was high feed concentration. One
effect of high feed concentration is greater solution ionic in-
tensity that influences the removal efficiency of heavy metals by
 M. Hedayatipour et al. / Journal of Environmental Management 203 (2017) 155
151e156
Table 5

Error
Results from the tests in optimum conditions based on the S/N ratios from the

0.91
0.15

4.98
Taguchi method.

e
e
6
b a
Test conditions Parameter Variables Removal (%)

15.63

15.17
34.03

32.68
5.21
pH
T ( C) P (psi) pH (A) (B)

3
1 NaCl 25 170 4 79.6 79.6

P (psi)

25.65

25.19
55.85

54.27
2 Ba 20 170 4 88 85.3

8.55
3 Cr 25 170 8 81.3 58.5

3
4 Ni 35 170 8 89.5 77.4
5 TDS 20 150 2 57.9 56.3
T ( C)

4.21

3.75
9.18

8.09
TDS

1.4
a
(A) Shows the removal rates in optimum conditions for each parameter and
3

(B) shows the removal rates in optimum conditions of NaCl removal (test
condition 1) for all parameters.
Error

0.76
0.12

3.02
b
See Table 2 for test conditions.
e
e
6
40.83
13.61

40.45
106.5

63.74

Table 6
pH

Characteristics of the feed and permeate of the NF in the optimum conditions.

a
P (psi)

Parameter Feed Permeate Removal (%)

30.63
11.74

11.36
3.91

17.9

Ca 1642 100 93.9

3

Mg 362.5 40 88.9
K 132.3 6.7 94.9
T ( C)

26.37

15.33
10.11
3.37

9.73

Na 14,864 205.6 98.6

Ni

Cle 18,650 203 98.9

SO42e 4479 380.7 91.5
Error

3.79
0.46

3.24

HCO3e 480.5 214 55.5

e
e
6

NO3e 6.4 2.1 67.1

Ba 209 30.7 85.3
199.4
64.81
139.1

Ni 6.2 1.4 77.4

94.5
193
pH

Cr 5.3 2.2 58.5

3

NaCl 14,180 2892 79.6

TDS 61,500 26,870 56.3
P (psi)

5.83
1.94

4.43
4.17

2.17

TH 2074 389.1 81.2

3

EC 14,311 1680 88.3

b
Q 1.4 0.66 47.17
T ( C)

1.02
0.34
0.73

a 1
All parameters are based on mg/l unless EC (mm/cm) and Q (L min ).
Cr

0
0

b
This value shows the recovery rate calculated by Eq. (3).
Error

0.35
0.59

2.19
e
e
6

osmotic pressure effect and decreases the removal rate

(Gherasim
208.08
37.03
12.34

36.58
90.74

and Mikula sek, 2014).

pH

3.6. Process effluent quality

P (psi)

1.02
6.77

2.53

The quality of NF effluent for its application in agricultural and

1.2
0.4
3

drinking water perspectives was categorized by the Wilcox and

Schoeller diagram. Findings of Wilcox diagram showed the C3S1
T ( C)

11.34
2.01
0.67

1.84
4.53

type for the effluent which implies that there is no limitation for
Ba

its use in agriculture for irrigation purposes. A similar study

showed that the treated drainage water using nanofiltration was
Error

0.33
0.55

2.65

considered
e
e
6

as a suitable source for irrigation and agricultural perspectives

22.16

21.99
132.3

when classified according to Wilcox diagram (Abid et al., 2013).

7.38

69.7
pH

Moreover, Schoeller diagram illustrated that the effluent was

acceptable as a drinking water source. Furthermore, the NF
P (psi)

17.09

effluent quality demonstrated a scaling feature, according to

2.86
0.94

2.69
8.54

Langelier saturation index, and showed that necessary

3

proceedings should be taken to prevent scaling for industrial

T ( C)

36.99
NaCl

6.19
2.06

6.02
19.1

4. Conclusion
ANOVA results for all parameters.

The principal objective of this research was determination of

Participation percentage

the
Degrees of freedom

optimum experimental conditions based on the removal priority

Sum of squares

of NaCl, metal ions and TDS. Therefore, the optimum

Least-squares

experimental conditions for removal of NaCl was selected as

Parameter

Variance
Variable

optimal conditions for all parameters. The results for

F-ratio
Table 4

simultaneous
conditions (T ¼removal
25 C, Punder
¼ 170these conditions
psi and pH ¼ 4) for all parameters
resulted from
the
Thaguchi method, the maximum removal efficiencies of 85.3%
156 M. Hedayatipour et al. / Journal of Environmental Management 203 (2017)
151e156
observed for Ba. Furthermore, 77.4, 58.5, 79.6 and 56.3% removal
efficiency were obtained for Ni, Cr, NaCl and TDS, respectively.
The findings of comparison between Schuller and Wilcox
diagrams showed that the effluent of membrane system is
applicable for drinking water, irrigating and agriculture
objectives. Moreover, the process effluent quality showed a
scaling feature, according to Langelier saturation index and
showed that necessary proceedings have to be taken to prevent
scaling for industrial usages. Also, ac- cording to the obtained
recovery rate of 47.17%, that is almost equal to half of the feed
flow, it can be concluded that NF process illus- trated a good
performance in the wastewater treatment. Since water transfer
to onshore rig is practically difficult and expensive, NF process
can be a useful approach for reusing the effluent of sludge
dewatering process in order to reduce the operational costs and
water supply. Also, regarding the high quality of NF effluent, the
environmental problems and soil and water pollution caused by
discharging effluent can be prevented.
Acknowledgments
The present paper is prepared from MSc thesis in Chemical
Engineering: Environmental Engineering. This research did not
receive any specific grant from funding agencies in the public,
commercial, or not-for-profit sectors.
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