Chemical Engineering Journal 328 (2017) 703707

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Short communication

Hexavalent chromium as a cathodic electron acceptor in a bipolar

membrane microbial fuel cell with the simultaneous treatment of
electroplating wastewater
Changman Kim a, Cho Rong Lee a, Young Eun Song a, Jinhee Heo b, Sung Mook Choi b, Dong-Ha Lim c,
Jaehoon Cho d, Chulhwan Park e, Min Jang f, Jung Rae Kim a,
a
School of Chemical and Biomolecular Engineering, Pusan National University, Busan 46241, Republic of Korea
b
Advanced Characterization & Analysis Research Group, Korea Institute of Materials Science (KIMS), Changwon 51508, Republic of Korea
c
Energy Plant R&D Group, Korea Institute of Industrial Technology, 30 Gwahaksandan 1-Ro 60 beon-gil, Gangseo-gu, Busan 46749, Republic of Korea
d
Green Process and Materials Group, Korea Institute of Industrial Technology, 89 Yangdaegiro-gil, Ipjang-myun, Cheonan-si 31056, Republic of Korea
e
Department of Chemical Engineering, Kwangwoon University, 20 Kwangwoon-Ro, Nowon-Gu, Seoul 01897, Republic of Korea
f
Department of Environmental Engineering, Kwangwoon University, 20 Kwangwoon-Ro, Nowon-Gu, Seoul 01897, Republic of Korea

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

Electroplating hexavalent chromium -

oj v [ TSGz Gj OP
wastewater was treated in the j Y v Z SGw Gj O )

cathode of MFC. Cu
O
S

A bipolar membrane MFC C

Pt
Cr
Cu

significantly improve the removal

OH - H+ Cr6+
efficiency of Cr6+. Cr3+ 20 m
Acetate

Simultaneous higher bioelectricity
CO2
was obtained from bipolar membrane OH - H+

(BPM).

The BPM supports cathodic reaction
OH - H+
without pH decrease in anodic
chamber. Bipolar membrane

The reduced chromium particles
precipitated on the cathode surface
was identified.

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

Article history: Hexavalent chromium wastewater is produced in electroplating processes and the heavy metal industry,
Received 27 May 2017 highlighting the need for an environmentally friendly treatment and the recovery of chromium. This
Received in revised form 11 July 2017 study compared the performance of microbial fuel cells implemented with a proton exchange membrane
Accepted 12 July 2017
(PEM-MFC) and a bipolar membrane (BPM-MFC) using hexavalent chromium from electroplating
Available online 13 July 2017
wastewater as the catholyte. The removal of hexavalent chromium and simultaneous bioelectricity
generation were enhanced significantly using a BPM. On the other hand, in the PEM-MFC, the lower
Keywords:
pH of the electroplating wastewater (pH 1.8) in the cathodic chamber decreased the anodic pH due to
Microbial fuel cell
Chromium wastewater
proton diffusion through the PEM, and inhibited the bioelectrochemical reaction. Scanning electron
Hexavalent chromium microscopy showed that the reduced chromium particles precipitated on the cathode carbon electrode
Bipolar membrane during the MFC operation. The precipitate was identified as amorphous chromium oxide particles by
Proton exchange membrane energy dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy.
2017 Elsevier B.V. All rights reserved.

Corresponding author at: School of Chemical and Biomolecular Engineering, Pusan National University, Busan 46241, Republic of Korea.
E-mail address: j.kim@pusan.ac.kr (J.R. Kim).

http://dx.doi.org/10.1016/j.cej.2017.07.077
1385-8947/ 2017 Elsevier B.V. All rights reserved.
704 C. Kim et al. / Chemical Engineering Journal 328 (2017) 703707
1. Introduction
Hexavalent chromium is used widely in various electroplating,
welding, and chromate painting processes owing to its higher
water solubility and spontaneous reduction to trivalent chromium,
which is plated on the metal surface. The U.S. Environmental Pro-
tection Agency has identified Cr(VI) as one of the heavy metals that
are a threat to humans, and set enforceable standards in drinking
water (i.e. <50 lg/L) and wastewater discharge (0.10.5 mg/L)
[1,2]. Electroplating wastewater is generally treated by conven-
tional processes, such as chemical precipitation, ion exchange,
membrane filtration, and chemical oxidation and/or reduction
[3,4]. These processes convert Cr(VI) to the less toxic and mobile
form of Cr(III), but most of these methods require heavy doses of
chemicals and energy-intensive processes. Recently, the biological
treatment of industrial wastewater contaminated with heavy met-
als has been highlighted as an eco-friendly and energy saving
process.
Microbial fuel cells (MFCs) have been applied to bioelectricity
recovery with simultaneous organic wastewater treatment. Vari-
ous catholytes containing metal ions, such as Cr6+, Cu2+, Ag+, and
Hg2+, have been assessed as replacements for conventional and
expensive cathode catalysts (i.e. platinum), and the oxygen reduc-
tion reaction [511]. Recent attempts have been made to use heavy
metal-containing industrial wastewater as an alternative catholyte
in MFCs [1214]. If a heavy metal ion-driven cathodic reaction
combines with an industrial wastewater treatment, the opera-
tional cost of the MFC can not only be saved, but also have added
benefit for the sustainable treatment and simultaneous recovery
of metal resources. Unfortunately, the pH of metal wastewater
from the electroplating industry is either extremely low or high
(e.g., pH 2 of electroplating chromium wastewater), which seri-
ously limits the applications of MFCs.
The oxidation-reduction potential of Cr(VI) to Cr(III) (E0 0 =
+1.33 V vs. SHE) is comparable to that of oxygen reduction
(+1.22 V vs. SHE). Therefore, the substitution of Cr-containing
wastewater as a terminal electron acceptor in the catholyte is fea-
sible, provided that the extreme pH of wastewater is implemented
appropriately in a MFC [10]. The Nernst equation shows the rela-
tionship between the proton concentration and Cr(VI) reduction
(See Supporting information 1). According to the equation, more
efficient Cr(VI) reduction is expected when the pH of the catholyte
is low. Previous reports also showed that wastewater treatment
with Cr(VI) resulted in more efficient power generation and simul-
taneous hexavalent chromium reduction in an acidic catholyte
rather than in a neutral or alkaline solution because of the suffi-
cient proton concentration [10,15]. On the other hand, a more
acidic catholyte than the anolyte can cause reversed proton trans-
ference through the ion exchange membrane, which would inhibit
the anodic bacterial community [16]. To solve the pH problem and
other inhibitive effects of acidic wastewater, Xafenias et al. applied
an augmented alkaline hexavalent chromium catholyte in a MFC
but the current generation and chromium removal efficiency were
significantly low [17].
A bipolar membrane (BPM), which laminates both a cation
exchange membrane and an anion exchange membrane, is capable
of dissociating water directly to H+ and OH. A BPM has a great
advantage in supplementing OH (in the anodic chamber) and H+
(in the cathodic chamber), particularly when the proton transfer-
ence through the membrane is insufficient. Therefore, the pH (or
ionic) imbalance, which normally develops in MFCs, can be
resolved by the application of a BPM. BPMs have been examined
frequently in MFCs and/or bioelectrochemical systems, particularly
for the application of acidic or alkali wastewater as a catholyte,
even though BPM has a relatively high polarization resistance com-
pared to the conventional ion exchange membrane [5,7,11,1820].
In this study, a bipolar membrane was implemented for the
treatment of electroplating wastewater containing hexavalent
chromium (Fig. S1). The use of a BPM enhanced significantly the
removal of soluble chromium as well as spontaneous generation
of electricity compared to those of a proton exchange membrane.
The electrochemical characteristics and long term stability of Cr
(VI) reduction on the cathode electrode were examined. Chromium
precipitation on the cathode surface was characterized by X-ray
photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and
energy dispersive X-ray spectroscopy (EDS). Scanning electron
microscopy (SEM) was used to examine the morphological struc-
ture of the chromium precipitates. To the best of the authors
knowledge, this paper is the first to apply a bipolar membrane to
the recovery of chromium from real electroplating wastewater as
well as for bioelectricity generation.
2. Materials and methods
2.1. MFC configuration and operation
A dual chamber MFC was assembled, as reported elsewhere [21]
(Supporting Information 2). In the anode chamber, an anaerobic
digester sludge (25 ml) from a sewage treatment plant (Suyoung,
Busan, Korea) was inoculated with 225 ml of sodium acetate med-
ium (Supporting Information 3). Chromium wastewater was col-
lected from the metal plating washing process in a local
electroplating plant (Taewon Industry Co., Busan, Korea). The con-
centration of hexavalent chromium in the raw wastewater was
determined to be 2070 170 ppm (initial pH of 1.8 0.1) using a
colorimetric method, as mentioned in Section 2.2. The solution
was diluted with DI water to the appropriate dilution ratio (0%,
5%, 10%, 30%, and 50%) of 93 11, 183 15, 573 62, and
998 85 ppm chromium, respectively, and added to the cathode
chamber. The pH of all the diluted wastewater was adjusted to
1.8 0.1 using 10% H2SO4 and 5 N NaOH to make the same pH as
the original wastewater. The anodic and cathodic chambers were
purged with nitrogen (99.9%) to remove the dissolved oxygen. All
experiments were conducted in duplicate.
To develop the anodic biofilm and start-up initially, MFCs with a
proton exchange membrane (hereinafter PEM-MFCs) and MFCs
with bipolar membrane MFCs (hereinafter BPM-MFCs) were oper-
ated for 2 weeks using potassium ferricyanide (100 mM, pH = 7.0)
as the catholyte. The current generation from both MFCs were 0.3
0.35 mA after 2 weeks of operation. At the end of the start-up, a
similar anode potential (0.40 V vs. Ag/AgCl) was obtained (data
not shown). When both reactors were stabilized, the fresh cathode
electrode and catholyte, including the different ratios of chromium
wastewater, were replaced. Supporting Information 4 describes the
monitoring and measurement of the electrochemical performance
during operation.
2.2. Identification of chromium reduction
The total soluble chromium concentration was analyzed using
the 1,5-diphenylcarbazide method from the absorbance at
540 nm on a UV/Vis spectrophotometer (Optizen POP, Mecasys,
Korea) [22]. The surface morphology of the cathode was observed
by field emission scanning electron microscopy (FE-SEM, SUPRA 40
VP, ZEISS, Germany). The metal precipitates on the electrode sur-
face were identified by EDS attached to the FE-SEM. The elemental
compositions and crystallinity of the particles from the air-dried
precipitate and electrode, were identified by XPS (Multilab 2000
base system with X-ray, Thermo, USA) and XRD (Dmax2500,
Rigaku, Japan), respectively.
 C. Kim et al. / Chemical Engineering Journal 328 (2017) 703707
3. Results and discussion
3.1. Electricity generation of PEM-MFCs and BPM-MFCs
Fig. 1 shows the current generated by the MFCs with 050% of
chromium wastewater in the cathode chamber. In the PEM-MFC,
the highest current generation was obtained within 10 h, which
then decreased gradually during 200 h of operation. In contrast,
the BPM-MFCs showed higher and more stable current generation
in all chromium wastewater samples compared to the PEM-MFCs.
The maximum power densities of the PEM-MFCs were 2.1, 13.9,
3.6, 2.3, and 47.2 mW/m2, while significantly higher maximum
power densities were obtained from the BPM-MFC; 4.8, 39.6,
58.2, 123.2, and 150.5 mW/m2 with 0, 5, 10, 30, and 50% of chro-
mium wastewater, respectively (Fig. S2).
Proton and cation exchange membranes are generally used as
an ion exchange membrane for MFCs because of their high ion per-
meability and low electrical resistance [23]. On the other hand, the
PEM is unsuitable for extremely low pH metal wastewater as the
catholyte [19]. In contrast, a bipolar membrane has been reported
to be an ideal option to resolve the pH variation and unbalanced
electrochemical reaction across the membrane, as reported by Hei-
jne et al. [19], and can be applied to a chromium wastewater MFC
(i.e. applications for a neutral anode and acidic cathode). The
increase of pH in the cathode chamber was more obvious in the
PEM-MFC (Fig. S3a) compared to that of BPM-MFCs (Fig. S3b). Sim-
ilarly, in the anode chamber, a more significant decrease in pH was
observed after 14 days in the PEM-MFC, while the decrease was
smaller in the BPM-MFC (Fig. S3b and d). This indicates that suffi-
cient protons can be provided from the BPM by water dissociation
in BPM-MFC, whereas the proton transference from the cathode to
anode through the PEM was proceeded in the PEM-MFC. The
decrease in pH of the anode chamber by reversed proton transport
might damage the anodic bacterial community and result in a
decreased bioelectrochemical reaction (Fig. 1 and Fig. S2).
600 a 0%
5%
500
10 %
Current (uA)
400 30 %
50 %
300
200
100
0 1000
600
b 7 Days
500
Current (uA)
400
300
200
100
0 5%
0 50 100 150 200
Time (h)
Fig. 1. Spontaneous current generation of MFCs using PEM (a) and BPM (b) using
chrome wastewater; 0%, 5%, 10%, 30%, and 50% of real chromium wastewater from
electroplating process.
705
3.2. Reduction of soluble hexavalent chromium to trivalent chromium
Most of the soluble Cr(VI) in the cathode chamber of BPM-MFC
were removed at lower concentrations (5 and 10%). The amount
removed increased significantly in the higher chromium wastewa-
ter (30 and 50%) (Fig. 2b). In contrast, the decrease in chromium in
the PEM-MFC was relatively low. The removal efficiencies (%) over
14 days were estimated to be 22.9, 19.2, 16.5, and 23.3% in the 5,
10, 30, and 50% with PEM-MFCs, respectively, and 100, 100, 63.6,
and 53.1% in 5, 10, 30, and 50% with BPM-MFCs, respectively.
Fig. 3 presents the precipitated chromium particles on the cathode
electrode surface, which was analyzed by SEM equipped with EDS
(Fig. 3 and Fig. S4). More abundant precipitated chromium parti-
cles were obtained in the BPM-MFC than in the PEM-MFC.
Although chromium exists mostly as the trivalent form in the
natural environment, hexavalent chromium is preferred in most
industrial applications on account of its high water solubility
(730 g/L) of chromate (HCrO 4 ) vs. insoluble chromium oxide
(Cr2O3) at 25 C. The previous two MFC studies reported a higher
current density and removal rate in more acidic chrome wastewa-
ter [11]. These results suggest that the thermodynamic favorability
of the cathodic reaction was increased under acidic conditions,
which facilitated proton-driven hexavalent chromium precipita-
tion. For hexavalent chromium reduction to the trivalent form,
HCrO 4 species (most dominant species in hexavalent chromium
forms) first approach the protonated cathode electrode by electro-
static attractions at low pH [10]. Cr(VI) is then reduced to Cr(III) by
the electrons transferred from the anodic reaction. As a result, the
reduced chromium ion (Cr3+) precipitates as trivalent chromium
oxide (Cr2O3) or chromium hydroxide (Cr(OH)3) on the electrode
surface and the bottom of the reactors. Generally, chromium pre-
cipitates form under high pH conditions, whereas soluble hexava-
lent chrome is dominant at lower pH (e.g. real electroplating
wastewater used in this study). Interestingly, Cr(III) precipitated
in the pH range of 14 under MFC operating conditions, as shown
in Figs. S3 and S4. The current flow and applied potential may pro-
mote crystallization on the cathode electrode surface. The porous
and heterogeneous carbon surface provides a favorable space for
crystal nucleation and growth on the electrode-electrolyte
interface.
The precipitated chromium oxide was analyzed by XPS (Fig. S5).
According to the reference scan and previous study, different bind-
ing energies were detected: trivalent chromium oxide (576 eV) and
a b
Soluble Cr concentration (ppm)
0 Day
800
14 Days
600
400
200
0
10% 30% 50% 5% 10% 30% 50%
Ratio of Cr-wastewater (%)
Fig. 2. Removal of soluble chromium in a PEM-MFC (a) and BPM-MFC (b) during
operation. The error bars represent the standard deviations based on an analysis of
the samples in duplicate.
706 C. Kim et al. / Chemical Engineering Journal 328 (2017) 703707

a b
Cu
O O S
C C Cr
Cr Pt Cu

10 m 20 m

c d
O O
C Cr C S Cr
PS Fe Cu

10 m 20 m

Fig. 3. SEM with EDS images of the cathode electrode: 5% Cr-wastewater MFC with PEM (a) and BPM (b) and 30% Cr-wastewater MFC with PEM (c) and BPM (d).

hexavalent chromium oxide (579 eV) [24]. The binding energy of
the precipitates of the BPM-MFCs with 10% and 30% wastewater
were 576.2 and 576.9 eV, respectively, which were identified as
typical trivalent chromium oxide (Fig. S5). Hexavalent chromium
still remained in the BPM-MFC with 50% chromium wastewater
(Fig. S5c). XRD was performed to determine the crystallinity of
the precipitated chromium oxide (Fig. 4). The results showed no
specific peaks for chromium oxide; however, clear peaks related
to Cr2O3 were identified after heat treatment (500 C in 1 h) in an
Ar environment. This suggests that the precipitates formed on
the cathode surface were amorphous chromium species, which is
facilitated by the bioelectricity generation of MFCs (Fig. S6).
3.3. Implications
Several attempts have been made to use real electroplating and
synthetic chromium wastewater as the electrolyte in MFCs, as
summarized in Table S1. Most studies, however, used only a PEM
or CEM (cation exchange membrane) [10,11,15,17,2527].
Although these studies showed that hexavalent chromium can be
used as a cathodic electron acceptor, they also found a drastic
decrease in current generation and less stable performance in the
MFC. This might be due to the significantly low pH of the chro-
mium wastewater, and the pH imbalance across the ion exchange
membrane. The migration of cationic chromium ions and protons
from the cathode to anode by the concentration gradient can inhi-
bit the anodic biological oxidation significantly, and eventually fail
the system. On the other hand, the results obtained in this study,
showed that the use of BPM enhances significantly the stable bio-
electricity generation and simultaneous removal of hexavalent
chromium in real electroplating wastewater.
Environmental pollution by spills of industrial wastewater con-
taining toxic heavy metals has been a concern, and the regulations
are being enforced. Conventional treatment strategies require a
heavy dose of chemical reagents, and results in secondary contam-
ination as well as additional cost for the operation. Therefore, an
environmentally friendly and energy effective treatment with pos-
sible recovery and reuse for such industrial wastewater is needed.
In this respect, MFCs have considerable advantages if the metal
containing wastewater is used as a catholyte, and provides a plat-
form for the recovery of chromium by bioelectrochemically driven
electrical regulation.

Acknowledgements

Fig. 4. XRD analysis of the precipitates on the cathode electrode in the 50% BPM- This study was supported by C1 Gas Refinery Program through
MFCs before and after heat treatment (HT). the National Research Foundation of Korea (NRF) funded by the
 C. Kim et al. / Chemical Engineering Journal 328 (2017) 703707
Ministry of Science, ICT & Future Planning (NRF-
2016M3D3A1A01913248).
Appendix A. Supplementary data
Supplementary data associated with this article can be found, in
the online version, at http://dx.doi.org/10.1016/j.cej.2017.07.077.
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