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Separation and Purification Technology 131 (2014) 79–83

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Separation and Purification Technology


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

Short Communication

Efficient treatment of domestic wastewater by electrochemical oxidation


process using bored doped diamond anode
Rimeh Daghrir a,1, Patrick Drogui b,⇑, Joel Tshibangu b,2
a
Centre des Technologies de l’Eau (CTE), 696, Avenue Sainte-Croix, Montréal, QC H4L 3Y2, Canada
b
Institut National de la Recherche Scientifique, Centre Eau, Terre et Environnement, 490 rue de la Couronne, Québec, QC G1K 9A9, Canada

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

Article history: Domestic wastewaters (DWW) contain varied and high amounts of organic matter which are difficult to
Received 5 November 2013 oxidize biologically or chemically. The discharge of such effluents is undesirable and can cause excessive
Received in revised form 13 April 2014 oxygen demand in the receiving water. In order to produce an effluent suitable for stream discharge,
Accepted 30 April 2014
electrochemical techniques have been explored at the laboratory pilot scale for organic compound
Available online 9 May 2014
removal from DWW. Electrolysis of DWW was carried out using rectangular electrolytic cell containing
two circular electrodes (anode and cathode). A preliminary voltametric study was carried out using
Keywords:
different anode materials (Ti/BDD, Ti/IrO2 and Ti/IrO2–RuO2). The Ti/BDD electrode was found to be
Electrochemical oxidation process
Domestic wastewater
the most effective electrode for DWW treatment. Electrochemical oxidation process using Ti/BDD elec-
Boron-doped diamond trode at the anode and a-C at the cathode with a current density imposed of 26.53 mA/cm2 ensures
Nanostructured amorphous carbon the removal efficiencies of 78.2%, 70% and 89.5% of COD, TOC and color, respectively. DWW could be oxi-
dized by both direct anodic electrochemical oxidation (by means of OH) and indirect electrochemical
oxidation via mediators, such as hydrogen peroxide generated by cathodic reduction. Both actions (direct
and indirect effects) lead to the formation of powerful oxidizing agents capable of oxidizing refractory
organic compounds.
Ó 2014 Elsevier B.V. All rights reserved.

1. Introduction producing hydroxyl radicals (E(OH/H2O) = 2.80 V vs. SHE). Hydro-


xyl radicals are very powerful oxidants capable of oxidizing a wide
Domestic wastewater (DWW) generated from isolated range of organic compounds [4,5]. The Electrooxidation (EO) pro-
communities and industries are complex mixture of organics, cess has been found to be a promising environmental remediation
inorganic and microbial pollutants [1]. Their exposure and accu- technology to remove organic pollutants [7–9]. The interest of
mulation in the aquatic environment lead to adverse effects using EO is based on its capability of reacting on pollutants by
towards human life and cause eutrophication of surface waters using both direct and indirect effect of electrical current [9–11].
and transmission of waterborne diseases [2,3]. Therefore, the Direct oxidation may be achieved through mineralization with
major concern is to treat the wastewater before discharge into hydroxyl radicals (OH) produced at the electrode surface by
the aquatic environment. The stricter restrictions imposed by dimensionally stable anodes (DSA) having high oxygen overvolt-
new legislations have caused extensive effort to focus on the devel- age, such as IrO2, PbO2 and boron doped diamond (BDD), among
opment of alternative and effective treatment processes in order to others [12–14]. In fact, OH radicals are exclusively generated on
remove organic pollutants from decentralized wastewaters. the anode electrodes from the oxidation of water (Eq. (1)) and
Nowadays, electrochemical advanced oxidation processes have organic compounds can be completely transformed or degraded
been proposed and identified as an attractive option for wastewa- by reacting with adsorbed OH radicals (Eq. (2)) [15–17]. As
ters treatment [4–6]. Electrochemical advanced oxidation reported by previous research works [17,18], the electrochemical
processes are environmentally friendly technologies capable of oxidation process using BDD as anode is highly potent to provide
more rapid destruction of pollutants and total mineralization of
the organic loading with high current efficiencies. Compared to
⇑ Corresponding author. Tel.: +1 (418) 654 3119; fax: +1 (418) 654 2600. the other DSA, BDD has received a great attention due to its inert
E-mail addresses: rdaghrir@cteau.com (R. Daghrir), patrick.drogui@ete.inrs.ca (P.
surface with low adsorption properties, its remarkable corrosion
Drogui), joetshiba@yahoo.fr (J. Tshibangu).
1
Tel.: +1 514 747 2782; fax: +1 514 747 2783.
stability even in acidic media and its high oxygen evolution
2
Tel.: +1 (418) 654 2530; fax: +1 (418) 654 2600. over-potential [10,19].

http://dx.doi.org/10.1016/j.seppur.2014.04.048
1383-5866/Ó 2014 Elsevier B.V. All rights reserved.
80 R. Daghrir et al. / Separation and Purification Technology 131 (2014) 79–83

M þ H2 O ! Mð OHÞ þ Hþ þ e Þ ð1Þ -


+

Mð OHÞ þ organics ! M þ oxidation products ð2Þ
Furthermore, indirect oxidation can be achieved through elec-
trochemical generation of a mediator in solution such as H2O2
[20,21]. Hydrogen peroxide (H2O2) (1.77 V) electrochemically gen-
erated at the cathode is an environmentally metastable molecule (3)
with high disinfecting and oxidizing properties able to convert (6) (1)
toxic organics to a less harmful products [20,22]. (7)
In this context, it could be interesting to explore at the labora-
tory scale the electrochemical oxidation process in order to remove
organic pollutants from domestic wastewater (DWW). The DWW
(4) (5)
was an effluent provided from a tank (septic tank) and collected
after bio-filtration treatment of wastewater from isolated resi-
dences. The main objective of this study is to develop an electro- (2)
chemical oxidation process using boron doped diamond at the
anode and to evaluate its performance in treating domestic
wastewaters.
Fig. 1. Schematic diagram of the experimental setup: (1) PVC tank, (2) peristaltic
recycling pump, (3) electrolytic reactor, (4) anode, (5) cathode, (6) in let, (7) out let.
2. Materials and methods

2.1. Sampling and characterization of DWW 40-70 (Aca Tmetrix, Mississauga, ON, Canada) with a maximum
current rating of 70 A at an open circuit potential of 40 V. All exper-
The domestic wastewaters (DWW) used throughout this study iments were carried out at room temperature (25 ± 0.1 °C). For all
was an effluent provided from Riviere du Loup community domes- tests, a total volume of 1.0 L was used.
tic wastewater treatment plant (WTP, Riviere du Loup, Quebec,
Canada). It is a conventional WTP having a primary treatment
(septic tank) of wastewater providing from isolated residences fol- 2.4. Experimental procedure
lowed by a bio-filtration process. The effluents were sampled at the
outlet of the bio-filtration unit. Samples were collected and stored A preliminary voltammetric study was performed with a three-
in polypropylene bottles and kept at 4 °C until use. The treated- electrode Voltalab 80 system (Radiometer analytical) equipped
effluent had an initial content of COD of 79.17 ± 4 mg/L, TOC of with a rotating working electrode (CVT 101, Radiometer analyti-
19.9 ± 0.8 mg/L, color of 100 ± 4 TCU, turbidity of 11.4 ± 0.3 NTU, cal). It included a potentiostat/galvanostat (Tacussel 20V/1A PGP
pH of 7 ± 0.03 and conductivity of 941.7 ± 10 ls/cm. 201). The reference electrode was a saturated calomel (Hg/Hg2Cl2/
KCl) electrode (Tacussel XM 110), while the auxiliary electrode was
2.2. Electrolytic cell platinum (Taccusel Pt XM 140). The materials used as working
electrode were titanium coated with bored doped diamond (Ti/
The electrolytic cell used was made of PVC material with a BDD, 11 mm diameter), titanium coated with iridium oxide (Ti/
dimension of 17 cm (depth)  5 cm (width)  15 cm (length). The IrO2, 11 mm diameter) and titanium coated with iridium-ruthe-
electrochemical cell was comprised of one anode and one cathode nium dioxide (Ti/IrO2–RuO2, 11 mm diameter). Linear voltammet-
electrodes in the form of expanded metal, each having a solid sur- ric measurements were conducted in a 0.1 M Na2SO4 electrolyte
face area of 65 cm2 and a void surface area of 45 cm2. The circular solution to identify the best electrodes. Subsequently, the treat-
anode electrode (12 cm of diameter  0.1 cm thick) was either ment of DWW using electrochemical oxidation process was oper-
made of titanium coated with boron doped diamond (Ti/BDD), ated under different operating parameters such as electrodes
whereas the circular cathode electrode was made of titanium materials (Ti/BDD; and Ti/IrO2–RuO2) and current density (from
coated with amorphous carbon (Ti/a-C) (12 cm of diame- 4.42 mA/cm2 to 26.5 mA/cm2) in order to determine the best con-
ter  0.1 cm thick). The magnetron-sputtering technique was used ditions (reduce cost and increase effectiveness). Experiments were
to coat deployed titanium grid substrates with nanostructured carried out over 120 min of electrolysis times. Owing to the high
amorphous carbon (a-C) films. The inter-electrode gap was conductivity, the treatment of DWW by electrochemical oxidation
1.0 cm in the electrolytic cell. The electrodes were vertically process was performed without adding Na2SO4. During these
installed on a perforated Plexiglas plate at 2 cm from the bottom assays, the effectiveness of the electrochemical oxidation process
of the cell. was evaluated by simultaneously measuring the residual concen-
tration of COD, TOC and color. Energy consumption of each test
was also determined. To verify the effectiveness and the reproduc-
2.3. Experimental setup
ibility of the electrochemical oxidation process, the measurement
of all parameters were repeated in triplicate.
The tests were carried out in a closed loop as depicted schemat-
ically in Fig. 1. A 2.0 L of PVC tank (1), a peristaltic recycling pump
(2) and the electrolytic cell (3) constitute the loop. All the essays 2.5. Analytical technique
were conducted in batch recirculation mode with a flow of effluent
entering the bottom of the cell. A recycle flow rate of 120 mL/min The pH was determined using a pH-meter (Fisher Acumet
was maintained using a peristaltic recycling pump (Master flex, model 915) equipped with a double junction Cole-Palmer electrode
Model 77200-50, USA). The electrochemical cell was operated with Ag/AgCl reference cell. A conductivity meter (Oakton Model
under galvanostatic conditions, with a current intensity (from 510) was used to determine the ionic conductivity of the effluent.
0.5 A to 3 A) imposed during 120 min of treatment period. Current Turbidity (in nephelometric units, NTU) was measured using a
intensity was imposed by means of DC power supply Xantrex XFR turbidimeter Hach 2100 AN. Chemical oxygen demand (COD)
R. Daghrir et al. / Separation and Purification Technology 131 (2014) 79–83 81

determination was measured based on APHA (1999) and a reading To evaluate the effect of the anode material on the electrochem-
spectrophotometer UV 0811 M136 (Varian, Australia). Total ical oxidation of DWW, additional experiments were carried out
organic carbon (TOC) measurements were performed using a Shi- using Ti/a-C as cathode, at 26.53 mA/cm2 of current density and
madzu TOC 5000A analyzer (Shimadzu Scientific Instruments Inc) during 120 min of treatment time. Only two anode electrodes
equipped with an autosampler. The measurements of color con- materials (Ti/BDD and Ti/IrO2–RuO2) were respectively used. The
centrations were carried out according to a standard method results are summarized in Fig. 3. Higher removals of COD
(MA. 103-Col. 2.0) based on the color scale using platinum-cobalt (80.9%), TOC (69.4%) and color (87.4%) have been recorded using
[23]. For that, a stock solution of platinum-cobalt reagent was Ti/BDD at the anode. By comparison, 57.4% (COD), 40.6% (TOC)
firstly prepared by dissolving 1.25 g of K2PtCl6 and 1 g of CoCl2- and 73.9% (color) were respectively removed using Ti/IrO2–RuO2.
6H2O in 1 L of distilled water. According to this method, such a The comparison between Ti/BDD and Ti/IrO2–RuO2 anode elec-
stock solution corresponds to 500 true color units (TCU). From this trodes showed that Ti/BDD was 1.5 times more effective than Ti/
stock solution, different standard solutions (5, 10 20, 75 and 100 IrO2–RuO2 for DWW treatment. In fact, the nature of the electrode
TCU) were prepared by dilution. A calibration curve of known color material strongly influences both the selectivity and the efficiency
concentration (absorbance vs. true color unit (TCU)) was used to of the direct oxidation process. Several authors argue that, direct
calculate the residual color concentration in treated and untreated oxidation by Ti/IrO2–RuO2 anodes (active electrode) occurs
effluents. The absorption peak was measured at the wavelength of through the formation of higher oxide M-Ox+1 in the lattice rather
400 nm using a spectrophotometer Carry UV 50 (Varian Canada, than hydroxyl radicals owing to a higher adsorption enthalpy of
Mississauga, Canada). the M-OH, M being the anode electrode [9,30,31]. By comparison,
using Ti/BDD anode electrode, hydroxyl radicals play an important
role due to the weak interaction between the hydroxyl and the
2.6. Economic aspect
electrode surface. As reported in previous research [17,32], the
Ti/BDD anode has a higher oxidation power and a great ability to
Evaluation of operation costs related to the electrochemical oxi-
produce active radicals from the electrochemical oxidation of
dation treatment process included energy consumption. The
water than the Ti/IrO2–RuO2. This was one of the reason for which
energy consumed was estimated at a cost of 0.06 US$/kW h, which
Ti/BDD anode electrode was more effective for DWW treatment
corresponds to the cost in the province of Quebec (Canada). The
compared to Ti/IrO2–RuO2.
total cost was evaluated in terms of U.S. dollars spent per cubic
meter of treated solution (US$/m3).
3.2. Influence of the current density on DWW treatment

3. Results and discussions The oxidation power of the electrochemical cell was expected to
strongly depend on the applied current [10,33]. To find the best
3.1. Influence of anode material on DWW treatment operating conditions for the treatment of DWW by the electro-
chemical oxidation process, a series of experiments were carried
It is well-know that the type of anode material can greatly influ- out using different current densities ranging from 4.42 mA/cm2
ence electrochemical oxidation processes [24,25]. This can be to 26.5 mA/cm2 during 120 min of electrolysis time. The changes
attributed to the different crystalline natures of electrodes that cat- in COD, TOC and color as a function of current density are shown
alyze the reaction of the electrochemical oxidation [26,27]. Thus, in Fig. 4. The percentage of COD degradation passed from 41.1%
prior to galvanostatic study, linear voltametric (LV) was investi- to 78.2% while the current density increased from 4.42 mA/cm2
gated at a sweep rate of 5 mV/s. According to LV curves (Fig. 2), to 26.5 mA/cm2. By comparison, 89.5% of color was removed for
it can be seen that Ti/IrO2 and Ti/IrO2–RuO2 anodes had compara- a current density imposed of 26.5 mA/cm2. In our experimental
tively oxygen evolution potential (0.9 V and 1.0 V), whereas the conditions, the percentage of color removal was higher than those
oxygen evolution on Ti/BDD appeared at 2.5 V. The use of anode recorded for COD and TOC using either Ti/IrO2–RuO2 or Ti/BDD
materials with a high oxygen evolution is required for organic anode material (see Figs. 3 and 4). As the current density increased,
compound oxidation because on such electrodes oxygen formation the treated effluent became more and more limpid. Likewise, as the
does not easily take place [28,29]. Considering this assumption, Ti/ current density increased, the depurative efficiency also increased
BDD seemed to be the best electrode for DWW treatment. in term of removal of DOC and TOC, respectively. It is believed that

Fig. 2. Linear voltammograms using different anode electrodes (Ti/IrO2, Ti/IrO2–SnO2 and Ti/BDD); electrolyte [Na2SO4] = 0.1 M; sweep rate = 5 mV s1; rotating
speed = 1000 tr min1.
82 R. Daghrir et al. / Separation and Purification Technology 131 (2014) 79–83

Fig. 3. Effect of anode materials on DWW degradation and mineralization (Ti/a-C: cathode; current density = 26.53 mA/cm2 and electrolysis time = 120 min).

Fig. 4. Effect of current density on DWW treatment (Ti/a-C: cathode; Ti/BDD: anode and electrolysis time = 120 min).

the pollutants associated with color were easier to be degraded enhancement in the degradation rate was mainly attributed to a
than the other pollutants. Indeed, the electrochemical decomposi- great electro-generation of H2O2 at the cathode and the high
tion of organic water components can be carried out using two amounts of hydroxyl radicals produced at the surface of BDD
effects: direct anodic oxidation (by means of OH) and indirect anode. Finally, electrochemical treatment cost of DWW using elec-
electrochemical oxidation via mediators, such as hydrogen perox- trooxidation process (including only energy consumption) was
ide. Such an oxidant can be electrochemically generated at the estimated to 7.98 ± 0.01 $/m3.
cathode electrode using for instance titanium coated with amor-
phous carbon (Ti/a-C). The results of H2O2 production on such a 4. Conclusion
Ti/a-C cathode material have been presented elsewhere by Daghrir
et al. [34]. The two effects (direct anodic oxidation and indirect This study investigated the treatment of DWW in batch recircu-
electrochemical oxidation) could lead to the formation of powerful lation mode using EO process. Ti/BDD (or Ti/IrO2–RuO2) and a-C are
oxidizing agents capable of simultaneously removing color, TOC the two circular electrodes used at the anode and the cathode,
and DOC. Likewise, hydrogen peroxide (H2O2) is well-known for respectively. The EO process is a feasible technology for the treat-
its decolourising properties of water. It was one on the main rea- ment of DWW characterized by high concentrations of COD TOC,
sons for which the pollutants associated with color were more sen- and color. The treatment of domestic wastewater by electro-oxida-
sitive than the other pollutants (TOC and COD) during the tion process was greatly affected by the operating conditions, such
electrochemical treatment. as type of anode and current density applied. Using Ti/BDD at the
Besides, the residual concentration of TOC recorded at the end anode and a-C at the cathode with a current density imposed of
of EO treatment was 5.9 mg TOC/L, whereas 20 mg/L was initially 26.5 mA/cm2, the removal efficiencies of COD, TOC and color
measured in the DWW. The relatively high yield of TOC removal recorded after 120 min of electrolysis time were 78.2%, 70% and
(70%) indicates that a high fraction of refractory organic matter 89.5%, respectively. Hence, the electrochemical oxidation process
was completely oxidized into water and carbon dioxide. The rela- may be a promising technology that can be used as tertiary treat-
tively high mineralization rate is mainly attributed to the hydroxyl ment to remove refractory organic compounds from DWW. How-
radical (OH) formation at the surface of Ti/BDD anode. Thereby, EO ever, it will be interesting to evaluate the efficiency and the
technique is an efficient treatment process able to upgrade water capacity of the EO process to remove microorganisms from DWW.
quality by providing high removal of refractory organic compounds
from DWW. The same trend has been also observed by Guinea Acknowledgment
et al. [4] while using electrochemical advanced process to oxidize
synthetic wastewater contaminated with salicylic acid (164 mg/ Sincere thanks are extended to the NSERC National Sciences and
L). The TOC removal efficiency passed from 61% to 84% by increas- Engineering Research Council of Canada (NSERC) for the financial
ing the applied current density (from 33 to 150 mA/cm2). This support.
R. Daghrir et al. / Separation and Purification Technology 131 (2014) 79–83 83

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