Separation and Purification Technology 154 (2015) 149153

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Separation and Purification Technology

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

Comparative decolorization of dyes in textile wastewater

using biological and chemical treatment
Huma Hayat, Qaisar Mahmood , Arshid Pervez, Zulfiqar Ahmad Bhatti, Shams Ali Baig
Department of Environmental Sciences, COMSATS Institute of Information Technology, Abbottabad 22060, Pakistan

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

Article history: Textile wastewater (TW) is one of the most hazardous wastewaters for the environment when discharged
Received 6 July 2015 without any proper treatment. A comparative study was conducted to investigate the removal efficiency
Received in revised form 4 August 2015 of color, chemical oxygen demand (COD) and turbidity from real textile industry wastewater using
Accepted 20 September 2015
anaerobic IC reactor and Fentons process with and without pH adjustment. Color, COD and turbidity
Available online 25 September 2015
removal efficiencies have been studied for 25%, 50%, 75% and 100% textile wastewater. Results
demonstrated that a maximum color removal efficiency (>92%) was recorded in Fentons process at
Keywords:
pH 3 for 100% sample. However, maximum COD removal efficiency of 87% was observed in IC reactor
Decolorization
Mineralization
for 100% sample. Thus, Fentons reagent at pH 3 was found highly effective for color removal and IC
Textile wastewater reactor observed to be efficient for COD removal. Furthermore, Fentons process without pH adjustment
Fentons reagent was found higher turbidity removal efficiency as compared to other treatments. Findings from this
Biological reactor suggested that the selective treatment process could be highly promising for the decolorization of textile
wastewater and can also be practically implementable.
! 2015 Elsevier B.V. All rights reserved.

1. Introduction and reduction, electrochemical precipitation have been employed

Large amount of water used in textile dyeing processes is one of
the leading generators of liquid pollutants. The quantity of textile
wastewater has been increasing along with the growing demand
of textile products [6]. Textile wastewater is characterized by high
chemical oxygen demand (COD), biological oxygen demand (BOD),
alkalinity and total dissolved solids (TDS). The dyes are stable and
difficult to degrade due to their complex aromatic structure and
synthetic origin [24,15,16,22].
Textile industry effluents are complex, containing synthetic
dyes, dispersants, bases, acids, detergents, salts, oxidants, surfac-
tants, inhibitory compounds, grease and oil, toxicants, many other
compounds salts depending on the particular textile process such
as scouring, bleaching, dyeing, printing and finishing. Discharge
of the colored effluent into streams and rivers results in the deple-
tion of dissolved oxygen, causing anoxic conditions that are lethal
to aquatic organisms [11,10,8,9,15,23,25]. In addition, textile
industry effluent usually contains 0.60.8 g/L dye, but the pollution
is due to the durability of the dyes [8].
Various physical, chemical and biological methods such as
adsorption, photolysis, chemical precipitation, chemical oxidation
Corresponding author.
E-mail address: mahmoodzju@gmail.com (Q. Mahmood).
for the removal of dyes from wastewater [24,16,23]. However,
these technologies are usually not effective in color removal, or
are expensive and less adaptable to wide range of dye containing
wastewaters [11,10,24]. Generally, dye degradation means
decolorization and mineralization of dye in textile wastewater.
Decolorization represents destruction of chromophore group of
the dye molecule; likewise degradation of organic compounds into
CO2 and H2O is called mineralization [26]. The levels of
decolorization and biodegradation by many investigators is
determined by measuring the percentage of mineralization by
BOD total organic carbon (TOC) and COD removal ratio by measur-
ing the initial and final content [23]. Recently, Fenton reaction was
efficiently utilized in wastewater treatment process for the
removal of many hazardous organics from wastewater [7,27].
The traditionally accepted Fenton mechanism is represented by
following equations [13].
Anaerobic treatment presents more attractive alternative as
they can be developed as a renewable and clean energy sources.
The anaerobic treatment is best suited for handling load
fluctuations, high BOD wastewater and low energy requirement
as no oxygen has to be supplied and it also has potential for energy
production [25]. Fentons oxidation has been used for treating
different types of industry wastes containing toxic organic
compounds such as formaldehyde, dyestuff, phenol, and can be

http://dx.doi.org/10.1016/j.seppur.2015.09.025
1383-5866/! 2015 Elsevier B.V. All rights reserved.
150 H. Hayat et al. / Separation and Purification Technology 154 (2015) 149153
used for wastewaters, contaminated soils and sludges, toxicity
reduction, organic pollutant destruction, BOD/COD removal and
color and odor removal [28,6,22]. It has been successfully used to
detoxify, decolorize and to enhance the biodegradability of textile
wastewater and dyes [20,1,21].
In this study, an attempt has been made to compare anaerobic
(i.e. IC reactor) and oxidation (i.e. Fentons oxidation) processes for
the removal of dye pollution. Decolorization and mineralization
efficiency of treatments has been investigated in terms of color
and COD removal. Thus, the aims of this study were to investigate
the decolorization efficiency of textile wastewater using anaerobic
inner loop reactor and Fenton process and to compare the
efficiency of anaerobic process and Fenton process in treating real
textile wastewater.
2. Materials and methods
2.1. Wastewater collection
Raw textile wastewater sample was taken from a textile
finishing industry located in Rawalpindi (Koh-i-Noor textile Mills),
Pakistan, where reactive dyes are being used to color cotton fabric.
The samples were used after dilution to 25%, 50%, 75% and in full
concentration (100%). The reactor was operated at HRT of 24 h at
room temperature. Sampling cans were rinsed and cleaned with
distilled water and then washed with sample during sample
collection. Ambient pH, TDS, conductivity and DO and turbidity
were measured using portable digital meters. The samples were
delivered to the laboratory within a day of being taken and
analyszed within 1 day. The samples were kept at 4 "C without
any chemicals addition. Physico-chemical characteristics of
wastewater are given in Table 1.
2.2. Experimental setup
The laboratorial-scale experiments were involved two types of
treatment processes (a) biological treatment of the industrial
wastewater using IC reactor, (b) chemical oxidation using Fentons
reagent with and without pH 3 adjustments of samples.
2.2.1. Startup of inner loop reactor
Raw textile industry wastewater was treated in a pilot scale IC
reactor (diameter 12 cm, total height 160 cm, total tank capacity of
3.5 L). The reactor was provided with conical bottom of 20 cm
length and a feed inlet pipe of 1.5 cm diameter avoid chocking
during operation. An outlet weir was provided at the top
(1.51 m), which is connected to an outlet gutter and outlet pipe
to the effluent collection tank. The reactor had ports for sampling,
feeding, effluent and gas collection. The peristaltic pump was used
for pumping of influent into the reactor. The reactor was operated
during summer when room temperature was around 35 3 "C, so
thermostat was not operated to save the energy.
Table 1
Characteristics of the sample wastewater used in this study.
Parameter Unit Concentration
pH 7.7 0.115
DO mg/L 0.3 0
Temperature "C 25.7 0
Conductivity ls 145 1.01
Turbidity NTU 188.6 0.57
Total solids mg/L 1731.6 8
Total dissolved solids mg/L 86.7 0.28
Total suspended solids mg/L 1697 7
COD mg/L 1132.6 2.5
The sludge used in the IC reactor was taken from anaerobic
digester degrading industry wastewater. During the startup, the
reactor was fed with tap water containing 400 mg/L dextrose as
the carbon source. To gradually expose the microbial community
with the inhibitory organic compounds an acclimation period
was necessary, allowing the development of enzyme producing
agents that are essential to induce biodegradation of dye interme-
diates. Measurement of COD reduction was used to assess stabi-
lization of reactor. It has taken almost 30 days to have steady
state COD reduction. Then the reactor was fed with effluent.
2.2.2. Fentons oxidation
All the tests were performed in 250 mL glass beakers containing
100 mL sample. The calculated amount of ferrous sulfate powder
and hydrogen peroxide (35% w/w) dose were added into the sam-
ple. The solution was stirred for 30 min using jar test apparatus.
After 30 min of settling supernatant was collected, caustic soda
was added to cease the reaction and been analyzed for color
(kmax), COD, pH, temperature, DO, conductivity, turbidity, TS,
TDS, TSS and heavy metals. PAM was not added in the reaction
mixture so save the operational cost. The dose of Fentons reagent
for each dilution is given in Table 2.
2.3. Analytical procedures
The pH of the solutions and samples was monitored by using
digital pH Meter (Jenway model 520). EC of the samples was deter-
mined by using conductivity meter (Jenway model 470) as lS. COD
was analyzed using a colorimetric method after digestion of the
samples in a COD digester (model TR320, Merck Spectroquant),
according to standard method [2]. The spectrum was taken with
UVVis Spectrophotometer (IRMeCO UVVis, U2020). Turbidity
of the samples was measured by using Turbidimeter (Eutech,
TN-100). Dissolved oxygen of the samples was determined by
using DO meter (Jenway, 970).
Sample stirring for Fentons oxidation was performed using Jar
test apparatus. Heavy metals were measured by using Atomic
absorption Spectroscopy (Perkin Elmer Model 920). Total solids
were determined by following the standard method described [2].
Color was measured using UV/Vis spectrophotometer from 190
to 1100 nm wavelengths; the absorbance values of supernatants
were measured. All the experiments were carried out in 4 mL
quartz cuvette. COD removal efficiency of samples is calculated
using formula (Eq. (1))
C0 ! Ct
" 100 1
C0
where C0 is the initial concentration of COD of the textile
wastewater, and Ct is the concentration of COD at the corresponding
time (t).
Table 2
Dose of Fentons reagent for different dilutions.
Sample Dose
pH 3 pH 78
25% 1:25* 1:25*
50% 1:25* 1:25*
75% 1:25* 1:25*
100% 1:25* 1:25*
*
The ratios mean 1 part ferrous sulfate and 25 parts H2O2.
 H. Hayat et al. / Separation and Purification Technology 154 (2015) 149153 151

3. Results 100 (a)

90
Glucose was fed to IC reactor during start up which was organic 80

% Color removal
substrate for the anaerobic heterotrophs present in the reactor. The 70
COD removal efficiency during start up period was in range of 60
7095%. During last seven days, the removal efficiency remained 50
40
above 90% which was considered as success of start up. Table 3 pre-
30
sent the characteristics of raw wastewater and its various dilutions.
20
It is evident from the Table that the raw wastewater contained high
10
TS, alkaline pH, lower DO, higher COD and excessive turbidity
0
levels. 25% 50% 75% 100%
Wastewater samples
3.1. Color removal efficiency
100 (b)
Anaerobic IC reactor has been used for the decolorization of 90
textile wastewater. The sample was used in % solutions in order 80

% Color removal
70
to acclimatize microbes grown within. Fig. 1ac presents color
60
removal efficiency of IC reactor, Fentons reagent without and with
50
pH adjustments. Maximum color removal efficiency was shown for 40
25% sample and minimum for 100% sample and color removal effi- 30
ciency of IC reactor for 25%, 50%, 75% and 100% sample was 82%, 20
29.2%, 62% and 19%, respectively. However, Fentons reagent has 10
been used to compare the decolorization of textile wastewater. 0
25% 50% 75% 100%
Color removal efficiency using Fentons process without pH adjust-
ment for 25%, 50%, 75% and 100% sample was 74%, 77.3%, 37% and Wastewater samples
88.8%, respectively. Fenton reagent found to be quite effective for
color removal without pH adjustment as compare to IC reactor. 100 (c)
In addition, color removal efficiency of Fentons process with pH 90
adjustment for 25%, 50%, 75% and 100% sample was 83%, 81.9%, 80
% Color removal

63% and 92.5%, respectively (Fig. 1c). The results demonstrated 70

that the Fentons process with pH adjustment was found highly 60
50
effective for the removal of color in textile wastewater.
40
30
3.2. COD removal efficiency 20
10
Fig 2ac presents COD removal efficiency of IC anaerobic 0
reactor, with and without pH adjustments using Fentons reagent. 25% 50% 75% 100%
In IC anaerobic reactor the removal efficiency of COD in 25%, 50%, Wastewater samples
75% and 100% sample after treatment with IC reactor was 76.8%,
60.1%, 69.6% and 87%, respectively (Fig. 2a). COD removal efficiency Fig. 1. Color removal efficiency of (a) anaerobic IC reactor, (b) Fentons reagent and
(c) Fentons reagent with pH 3 for all samples.
of Fentons reagent with pH adjustment in 25%, 50%, 75% and 100%
sample was 28.8%, 89%, 40.4% and 28%, respectively (Fig. 2b).
Fenton reagent found to be effective for COD removal except for
50% sample. However, the findings were quite surprising in treat- was 26.6%, 21.2%, 33% and 26%, respectively (Fig. 2c). Thus, the
ment without pH adjustment. COD removal efficiency of Fentons findings revealed that the IC reactor was found comparatively
reagent without pH adjustment in 25%, 50%, 75% and 100% sample higher COD removal efficiency as compared to other treatments.

Table 3
Parameters determined for each sample dilution solutions before treatment.

Parameters Dilution
25% 50% 75% 100%
pH 7.23 0.047 6.89 0 7.08 0.008 7.80 0.11
DO (mg/L) 2.73 0.094 0.103 0.004 0.3 0 0.3 0
TS (mg/L) 506.3 5.79 884.3 2.05 1444.6 7.58 1731.6 8
TSS (mg/L) 697 6.16 812.5 2.05 1225.9 5.78 1697 7
TDS (mg/L) 26.0 0.047 51.8 0 80.3 0.047 86.7 0.28
Conductivity (ls) 58.3 0.047 79.6 0 114 0.1 145 1.01
COD (mg/L) 282.9 0.69 560.5 4.74 851.6 2.49 1132.6 2.5
Turbidity (NTU) 47.25 0.04 86.6 0.47 180 1.63 188.6 0.57
Temperature ("C) 23.4 0 25.2 0 25 0 25.7 0.05
Manganese (mg/L) 0.003 0.001 0.08 0 0.009 0.015 0.012 0.02
Lead (mg/L) 0.092 0.04 0.210 0.001 0.266 0.02 0.385 0.01
Chromium (mg/L) 2.61 0.001 3.45 0.004 4.80 0.01 6.45 0.03
Zinc (mg/L) 0.024 0.002 0.485 0 0.631 0.02 0.085 0.03
Nickel (mg/L) 0.021 0.001 0.043 0.002 0.063 0.02 0.086 0.01
152 H. Hayat et al. / Separation and Purification Technology 154 (2015) 149153

100 100
(a) (a)
90 90
80 80

%Turbidity removal
% COD removal

70 70
60 60
50
50
40
40
30
30
20
20
10
0 10
25% 50% 75% 100% 0
25% 50% 75% 100%
Wastewater samples
Wastewater samples
100
(b) 100
90 (b)
98
80
96
% COD removal

70

%Turbidity removal
60 94
50 92
40 90
30 88
20 86
10 84
0 82
25% 50% 75% 100%
80
Wastewater samples 25% 50% 75% 100%
Wastewater samples
100
(c)
90 100
80 (c)
90
% COD removal

70
80
60
%Turbidity removal

50 70
40 60
30 50
20 40
10 30
0
25% 50% 75% 100% 20
10
Wastewater samples
0
Fig. 2. COD removal efficiency of (a) anaerobic IC reactor, (b) Fentons reagent and 25% 50% 75% 100%
(c) Fentons reagent with pH 3 for all samples for all samples. Wastewater samples

Fig. 3. Turbidity and color removal efficiency of (a) IC reactor, (b) Fenton reagent at
3.3. Turbidity removal efficiency pH 3, and (c) Fenton reagent without pH adjustment.

Fig. 3ac presents turbidity removal efficiency of anaerobic IC

reactor, with and without pH adjustments using Fentons reagent.
Turbidity removal efficiency of IC reactor for 25%, 50%, 75% and
100% sample was 70%, 55%, 82.3% and 36.4%, respectively
(Fig. 3a). However, turbidity removal efficiency using Fentons pro-
cess with pH adjustment for 25%, 50%, 75% and 100% was 92.6%,
93.4%, 90.8% and 93.4%, respectively, which was found to be higher
as compared to IC reactor. But the turbidity removal efficiency of
Fentons process without pH adjustment for 25%, 50%, 75% and
100% sample was 87.9%, 72%, 73%, 94.3%, respectively (Fig. 3c).
As result Fentons process without pH adjustment was found
higher turbidity removal efficiency as compared to other
treatments.
4. Discussion
The present study was conducted to investigate the decoloriza-
tion and mineralization efficiency of anaerobic biological IC reactor
and Fentons reagent as a chemical treatment with and without pH
adjustments. The purpose of running different concentrations of
sample was to acclimatize the anaerobes to wastewater character-
istics and gradually exposing them to high concentrations. In the
past several physicochemical methods have been employed for
the removal of dyes from textile wastewater effluent [23]. How-
ever, enzymatic or microbial degradation and decolorization is an
eco-friendly cost-competitive option that could help reduce water
consumption compared to physicochemical treatment methods.
Biological treatment was found to be quite effective; however,
most of the organic matter in the effluent is toxic and or not so
biodegradable, so biological treatment alone is not efficient [4].
Consequently, the tighter international regulations and increased
public concern challenged the textile industry to explore and go
for new alternatives to minimize environmental problems associ-
ated with dye containing wastewater.
It is well established that the oxidation processes can be suc-
cessfully used for the remediation of contaminated surface, ground
and industrial wastewaters containing non-biodegradable organic
pollutants [28,3,5,12]. Fenton oxidation is one of the powerful
advanced oxidation processes. Fenton Oxidation mechanism is
based on the generation of hydroxyl radicals as a result of the
 H. Hayat et al. / Separation and Purification Technology 154 (2015) 149153
reaction of hydrogen peroxide with ferrous ions a catalyst under
acidic conditions [22].
The Fenton reaction has significant advantages such as a short
reaction time respective to all other advanced oxidation processes,
reagents are cheap and non-toxic; there is no complexity in
carrying on the reaction [5,14]. Although Fentons reagent can
decolorize the dye wastewater, it has its own limitations as the
high reagent costs, generation of aromatic amines and production
of sludge which needs safe disposal [17,28,22]. Many investigators
have reported that Fentons reagent is effective for partial
degradation and complete color removal of complex organic
matter [17,10].
Color and COD removal efficiency of anaerobic IC reactor has
been studied in the present study. Maximum color removal of
82% for 25% sample while minimum was 19% for 100% sample
was recorded. Therefore, IC was found not too effective for color
removal except for 25% sample (Fig. 1a). Dye concentration may
play a role in the color removal process. The applied dye concentra-
tions in several studies largely exceed the 10250 mg/L range in
textile effluents. High dye concentrations negatively affect the
anaerobic color removal efficiency, either by causing toxicity for
microbes or by exceeding the reactors dye reduction capacity
[18]. Studies investigating the effect of different dye concentra-
tions usually reported higher net color removal efficiencies at
lower dye concentrations [29].
In this study, Fentons reagent with and without pH adjustment
was used for the removal of color and COD. Fentons reagent was
found to be highly efficient in terms of color removal with
minimum efficiency not less than 63.5%. However, COD removal
efficiency was in the range of 21.233% demonstrating a poor
response for COD removal. Other studies also revealed that Fenton
process along with oxidation and coagulation was effective for the
removal of color rather than COD. But a photo-Fenton process was
found to be more effective (>98%) for decolorization [19].
5. Conclusions
A comparative study using two removal processes (IC reactor
and Fentons reagent with and without pH adjustment) for the
removal of color, COD and turbidity removal from a real textile
industry wastewater was evaluated in this study. Color removal
efficiency in Fentons process with and without pH adjustment
was found to be highly efficient. However, minimum color removal
efficiency was shown by anaerobic IC reactor in comparison to
other treatments. In all cases maximum COD removal efficiency
was shown by anaerobic IC reactor in comparison to other
treatments. It was found that Fentons reagent with pH 3 is best
for color removal and IC reactor for COD removal. Furthermore,
findings from this suggested that the selective treatment process
could be more effective for the removal of targeted pollutants from
textile wastewater.
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