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Full-loop operation and cathodic acidification of a microbial fuel cell operatedon domestic wastewater Olivier Lefebvrea, Yujia Shena, Zi Tana, Arnaud Uzabiagaa, In Seop Changb, How Yong

Trang 1

Full-loop operation and cathodic acidification of a microbial fuel cell operated

on domestic wastewater

Olivier Lefebvrea, Yujia Shena, Zi Tana, Arnaud Uzabiagaa, In Seop Changb, How Yong Nga,⇑

a

Centre for Water Research, Department of Civil and Environmental Engineering, National University of Singapore, 1 Engineering Dr 2, Singapore 117576, Singapore

b

Department of Environmental Science and Engineering, Gwangju Institute of Science and Technology (GIST), 261 Cheomdan Gwagi-ro, Buk-gu, Gwangju 500-712, Republic of Korea

a r t i c l e i n f o

Article history:

Received 3 November 2010

Received in revised form 29 January 2011

Accepted 23 February 2011

Available online xxxx

Keywords:

Microbial fuel cell

Loop

Overflow

Selemion

Wastewater treatment

a b s t r a c t

The present study emphasizes the importance of overcoming proton limitation in a microbial fuel cell operated on domestic wastewater When the anode-treated effluent was allowed to trickle into the cathodic compartment (full-loop operation), high COD and suspended solids removal efficiencies over 75% and 84%, respectively, were achieved while ensuring substantial and sustainable power generation Lower removal efficiencies resulted in decreased cell electromotive force caused by excess substrate crossover By decreasing the pH in the cathodic compartment to values below 2, we were able to further increase the maximum power generation by 180% in batch mode and 380% in continuous mode as com-pared to a negative control (tap water of pH 7.6) Under the optimized conditions, the internal resistance and electromotive force were 11Xand 0.6 V, respectively, which correspond to the state of the art

Ó 2011 Elsevier Ltd All rights reserved

1 Introduction

Providing the world’s population with adequate sanitation is

among the major development challenges of this century and

recovering energy from wastewater seems the only way to allow

sanitation programs to maintain their development without

dras-tically increasing energy consumption Among the different types

of wastewater, management of domestic wastewater is

particu-larly crucial in fast growing and land-limited Singapore In the

re-cent years, there has been growing interest in microbial fuel cell

(MFC), a technology derived from chemical fuel cell that allows

simultaneous wastewater treatment and energy recovery directly

in the form of electricity However, the technology is still in its

in-fancy due to scale-up limitations and large applications in

waste-water treatment plants are hindered by the inner limitations of

the technology One of the major limitations of MFCs nowadays

is related to stacking issues Even though parallel stacking can be

efficient – at least on a limited number of fuel cells (Aelterman

et al., 2006) – series connections of MFCs rapidly lead to energy

losses and reduced stacking efficiencies (Wang and Han, 2009)

Furthermore, series stacking has been shown to result in cell

polar-ity reversal (Aelterman et al., 2006) This raises the question of whether the power should be maximized on a volumetric basis –

as is the consensus nowadays – or on a ‘‘per cell’’ basis, in order

to reduce the number of cells to be connected together

At first glance, the main difference between conventional chem-ical fuel cells and MFCs is that MFC anodes are ‘‘alive’’ and rely on microbial metabolism However, another major difference be-tween the two technologies lies in the extremely different environ-mental conditions applied to both systems In an MFC, the temperature is ambient and the pH circum-neutral to allow bacte-rial growth on the anode On the other hand, in a conventional hydrogen fuel cell the temperature is above 80 °C and the cathode

is kept under a pressure of 2 bars of oxygen and hydrogen (Barbir,

2005) This makes it possible in hydrogen fuel cells to achieve elec-tromotive force higher than in MFCs On top of it, the pH in the cat-ion exchange membrane of a hydrogen fuel cell is around 3, which implies that there are much more protons available to contribute

to the charge transfer between the electrodes, and this transfer is further facilitated by high temperatures that dramatically increase proton conductivity (Barbir, 2005) Kinetics are also much faster in chemical fuel cells, which helps to maintain their internal resis-tance at low levels, in the order of a few mX

Because of the disadvantageous environmental conditions ap-plied to MFC systems and described above, the anode is seldom the limiting factor in a well constructed modern MFC design and the highest anodic power density achieved so far was obtained in

an MFC where the cathode was 14 times larger than the anode

0960-8524/$ - see front matter Ó 2011 Elsevier Ltd All rights reserved.

doi: 10.1016/j.biortech.2011.02.098

Abbreviations: HRT, hydraulic retention time; HCl, hydrochloric acid; MEA,

membrane electrode assembly; MFC, microbial fuel cell; OCV, open circuit voltage;

PTFE, polytetrafluoroethylene; SS, suspended solids; VSS, volatile suspended solids.

⇑ Corresponding author Tel.: +65 6516 4777; fax: +65 6774 4202.

E-mail address: esenghy@nus.edu.sg (H.Y Ng).

Contents lists available atScienceDirect

Bioresource Technology

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 / b i o r t e c h

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MFC generally combine with oxygen to form water and in this

sense, proton availability and mobility are of prime importance

and most of the time lacking in MFCs, where electro neutrality is

achieved by transport of other more abundant cation species such

as Na+, K+, NHþ

4, Ca2+and Mg2+(Rozendal et al., 2006) Bringing

pro-tons directly to the cathode could be a way to improve the

electri-cal performance of the system One way is by operating the MFC in

a full-loop mode where the anode-treated effluent is allowed to

enter the cathode compartment and, recently, some publications

have presented the advantages of such method (Clauwaert et al.,

2009; Freguia et al., 2008a; Li et al., 2009) From the point of view

of electrochemistry, this helps counterbalancing pH variations in

two-chamber MFCs, in which otherwise cathode alkalinization

and anode acidification with time are observed (Gil et al., 2003)

Furthermore, from the point of view of wastewater treatment

engi-neering, the cathodic compartment occupies a large footprint that

is not directly used for wastewater treatment in most cases With

domestic wastewater, MFC is known to produce an effluent of

insufficient quality for discharge after passing through the anodic

compartment (Cheng et al., 2006; Lefebvre et al., 2008) The

situa-tion even worsens if the MFC is optimized for electricity

genera-tion, because the power output increases when the HRT

decreases but the trend is opposite for COD removal (Ahn and

Logan, 2010; Liu et al., 2004) This means that effluent polishing

will be required in an MFC-based wastewater treatment plant If

the anolyte is introduced into the cathodic compartment, the latter

has the potential to provide aerobic post-treatment for the

anode-treated effluent, while protons are transported directly by the

ano-lyte to the cathode of the MFC Another way to overcome proton

limitation at the cathode is by bringing them intentionally into

the cathode compartment, which is the main focus of the present

study

In this paper, we disclose a prototype MFC that is suitable for

continuous treatment of domestic wastewater, according to the

re-search objectives of our laboratory This implies that the MFC has

to be of a reasonable size (a few litres) In a larger reactor, power

generation is further maximized per cell used and not on a

volu-metric basis, which – as explained above – might prove useful until

the stacking technology matures In order to overcome proton

lim-itation at the cathode, two strategies were employed –

introduc-tion of the anolyte into the cathodic compartment of the MFC,

and acidification of the cathode using HCl For that purpose, the

MFC made use of a membrane electrode assembly (MEA)

incorpo-rating a proton selective membrane, in order to prevent accidental

acidification of the anodic compartment

2 Methods

2.1 MEA-MFC design

The reactor vessel was a vertical cylinder (length = 90 cm,

diam-eter = 7 cm) made of transparent polyacrylic plastic

(Thermoplas-tics, Singapore) and the MEA was incorporated in the middle The

MEA (length = 90 cm, diameter = 3 cm)was wrapped around a

stainless steel grid acting as the cathodic current collector and a

stainless steel mesh was tightened over the anode acting as the

anodic current collector The anodic compartment had a volume

of 2.9 L and the cathodic compartment capacity was of 0.6 L The

experimental design is shown inFig 1

The MEA consisted of an anode and a cathode wrapped on

opposite sides of an ion exchange membrane A proton-selective

Selemion ion exchange membrane (model HSF, Asahi, Japan) was

selected over the comparable Nafion membrane due to its more

competitive price Selemion HSF membrane, originally designed

burst strength of 0.2 MPa and a resistivity of 0.3Xcm2 in 0.5 mol L1HCl or H2SO4 (manufacturer data) Two layers of re-verse osmosis spacer were incorporated, between the anode and the Selemion membrane, and between the cathode and the mem-brane The purpose of such spacer was to prevent partial short-circuit between the anode and the cathode in the MEA In the absence of spacer indeed, the resistance between the anode and the cathode was only of around 200Xafter tightening the MEA, but with the use of spacer this value could be increased to over

1 MX, indicating that the partial short-circuit was largely overcome This emphasizes that, even though the anode and the cathode should be maintained as close as possible to one another

in an MFC system (Cheng et al., 2006), there is a limitation in MEA designs due to the risk of short-circuits Both the anode and the cathode were made of carbon cloth (designation B, E-Tek, USA) and the cathode was further coated with Pt (0.5 mg cm2)

on one side A detail of the MEA is shown inFig 1c

2.2 Experimental conditions

The fuel (domestic wastewater) was circulated continuously in

an upflow mode into the anodic compartment at a flow rate of

20 mL min1 (HRT = 2.4 h).Unless specified otherwise, aeration was provided by actively bubbling air into the cathodic compart-ment using an air compressor and regulating the airflow with a valve at 5 L min1 In early experiments, the anode-treated effluent collected from the top of the reactor was introduced into the top of the cathodic compartment where it was allowed to trickle along the cathodic wall (seeFig 1a) Domestic wastewater was used simultaneously as the fuel and the inoculum for the reactor, which was collected from the primary decantation basin of the Ulu Pan-dan Reclamation Plant in Singapore The pH, COD, suspended solids (SS) and volatile suspended solids (VSS) content ranged from 7.3 to 7.9240 to 459 mg L1, 152 to 288mg L1and 138 to 426 mg L1, respectively The VSS to SS ratio was ranged between 0.6 and 0.9, indicating good biodegradability The reactor was set-up at ambi-ent temperature (25 °C) and wrapped with aluminum foil to pre-vent algae growth

Cathodic acidification was performed in batch and in continu-ous modes Batch acidification used 500 mL of hydrochloric acid (HCl) solutions diluted in tap water at different pH, ranging from

6 to 1, and pumped into the cathodic compartment, which had been previously closed (Fig 1b) Air was allowed to bubble into the acidic solution at a flow rate of 5 L min1 The voltage was re-corded every 10 s across an external resistance of 40 O and, finally, the cathodic compartment was reopened to collect the catholyte and measure its pH Tap water with a pH of 7.6 was used as a neg-ative control Continuous acidification used HCl solution diluted in tap water at different pH, ranging from 1.2 to 6, and pumped at a flowrate of 250 mL min1into the cathodic compartment Airflow rate was similarly fixed at 5 L min1 The experiment began under the open circuit voltage (OCV) conditions After OCV stabilization, the external load was progressively decreased in order to record polarization curves Samples of the cathodic outlet were collected regularly during the experimental period Tap water (pH 7.6) and phosphate buffer solutions (pH 7) having ionic strengths of 102

and 104M, respectively, were used as negative controls 2.3 Analytical methods and calculations

COD, SS, VSS and pH were analyzed according to the standard methods (APHA, 2005) The cell voltage was monitored with a mul-timeter (M3500A, Array Electronic, Taiwan) connected to a com-puter by a data acquisition system (PC1604, TTi, RS, Singapore) Starting from the OCV, polarization curves were obtained by

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decreasing the applied external resistance and recording the

pseu-do steady-state voltage The current was then determined using

the Ohm’s law and the Coulombic efficiency was calculated based

on the current and COD removal followingLogan et al (2006) The

cell electromotive force (Eemf, V) and internal resistance (Rint, O)

were determined using a linear regression (least squares method)

on the linear part of the polarization curve that corresponds to

the Ohmic zone The electromotive force was estimated as the

intercept of the regression with the Y-axis whereas the internal

resistance was the opposite of its slope The maximum power

(Pmax, W) supplied by the MFC was calculated according to Eq 1

Pmax¼ðEemfÞ

2

Data analyzes were assessed statistically by Student’s t-tests for

un-paired samples Two sets of data were considered significantly

dif-ferent when the P value was inferior than 0.05

2.4 Performance assessment as compared to the literature

The performance of our MFC set-up was compared to the

liter-ature available using the following criteria: OCV, Eemf, Rint, Pmax,

and the volumetric power (Pvmax) Eemfand Rintwere determined

using the polarization curves provided in the selected articles

and Pmax, was calculated using Eq 1 Furthermore, in an effort of

standardization, Pvmaxwas calculated for each study taking into

ac-count the total working volume of the MFCs, which corresponds to

the sum of the volume of the anodic and cathodic compartments

In our opinion, this shall reflect more accurately the impact of

the footprint of the treatment system

3 Results and discussion

The experiments were conducted over a period of 140 d Four

distinct stages could be identified Stages 1 to 3 (65 d) correspond

to the MFC operation in a full-loop mode and are described in

Sec-tion 3.1 Stage 4 (75 d) corresponds to the MFC operaSec-tion in a sin-gle-chamber mode with an open-air cathode (i.e., full-loop operation was ceased) Cathodic acidification experiments were carried out during stage 4 between days 95 and 120 Details of operation during stage 4 are detailed in Section 3.2

3.1 Operation in a full-loop mode (stages 1–3)

The full-loop experiments were carried over a period of 65 d and the experimental protocol is shown inFig 1a Three distinct stages could be identified Stage 1 (7 d) corresponded to the start-up of the reactor followed by stage 2 (20 d) characterized

by a deterioration of the reactor performance Finally, in Stage 3 (38 d), the anodic compartment was filled with graphite granules resulting in improved performance The detail of the three stages

is given below and the electrochemical characteristics of the reac-tor and of the treatment performance at each stage are summa-rized inFigs 2 and 3

3.1.1 Stage 1 The MEA-MFC was operated initially on domestic wastewater in

a full-loop mode in which the effluent flowed upward into the ano-dic compartment then trickled into the inner cathoano-dic compart-ment (seeFig 1a) The power rose constantly over the first week

of operation and attained 1.74 ± 0.16 mW (Fig 2) The OCV at that time was higher than 0.7 V, which indicates proper functioning of the system as an electricity generation device The cell electromo-tive force averaged 0.59 ± 0.08 V and the internal resistance was estimated at 52 ± 19X After passing through the anodic compart-ment, only 39 ± 11% of the COD and 57 ± 10% of the SS were re-moved (Fig 3) However, the treated effluent collected from the outlet of the cathodic compartment appeared much clearer in color and the COD removal averaged 71 ± 5% In addition, 78 ± 2% of the

SS were removed in the process This confirms the potential of using the aerobic cathode compartment for effluent polishing in the MFC technology The Coulombic efficiency was estimated to

air

effluent out

effluent in

effluent in

effluent out

current collector

current collector

cathode

anode

spacer

spacer Selemion

lumen

HCl in

anode compartment

cathode compartment

HCl out

(c)

Fig 1 Experimental design (a) operation in full-loop where the effluent from the anodic compartment is introduced into the cathodic compartment, (b) operation with acidification of the cathodic compartment by HCl, (c) detail of the membrane electrode assembly.

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average 0.2 ± 0.1%, which reflects that most of the COD was

removed by ways that did not contribute to electricity generation

Mostly, there was a tendency to observe sludge accumulation at

the bottom of the anodic compartment, where fermentation was

probably taking place

3.1.2 Stage 2

After 14 d, the power generation was found to be much lower

and the OCV was reduced to below 0.4 V The electromotive force

dropped drastically to 0.13 ± 0.04 V while the internal resistance

was affected to a lesser extent, averaging 70 ± 13X(Fig 2)

Conse-quently, the maximum power output (0.06 ± 0.04 mW) was found

to be significantly lower than that during stage 1 (P = 0.005;

Stu-dent’s t-test) This drop in performance was accompanied by a

poorer quality of the treated effluent that looked darker in color

and the COD and SS removal efficiencies dropped to 54 ± 11 and

32 ± 30% (Fig 3), respectively, resulting in unchanged Coulombic

efficiency of 0.2 ± 0.1% A probable reason for the observed drop

of electromotive force could be attributed to excess substrate

crossover from the anode to the cathode, resulting in a cathodic

potential mixed between that of O2 and that of the

above-mentioned substrate, as explained byHarnisch et al (2009)

Fur-thermore, another explanation could be related to aerobic bacteria

growing on the cathode due to excess substrate and further

limit-ing oxygen access for the cathodic reaction Similar problem was

also noted by Freguia et al (2008a)who used acetate as a

sub-strate When they increased the loading rate in their MFC,

over-loading of the cathodic compartment and a drop in power

occurred However, for practical reasons, it was not possible to

ac-cess the MFC cathode in the course of our experiment to evaluate

biofilm growth

3.1.3 Stage 3

In order to improve the quality of the anode-treated effluent,

the anodic compartment was filled with graphite granules having

an estimated projected surface of between 500 and 3000 m2m3

(Carbone Lorraine, Belgium) In addition, the cathode compartment was washed with plenty of water As a result, the COD and SS re-moval efficiencies after passing through the anodic compartment increased to 75 ± 21% and 84 ± 19%, respectively (Fig 3) The high variability of COD and SS removal efficiencies could be attributed

to the variability of the influent itself depending on the weather conditions (i.e., rainfall) For instance, during stage 3 the influent

SS dropped and this was accompanied by a drop in the SS removal efficiency that followed the same pattern Introducing the anolyte into the cathode further improved the COD removal to 92 ± 4%, whereas the SS removal remained unchanged In terms of electro-chemical performance, the fuel cell electromotive force rose to 0.62 ± 0.06 V while the internal resistance remained unaffected at

70 ± 9 O (Fig 2) These results confirm the hypothesis that the drop

in power observed in stage 2 could be attributed to substrate crossover as explained byHarnisch et al (2009), since only the electromotive force seemed to be affected by the quality of the anode-treated effluent The maximum power was then of 1.41 ± 0.21 mW (an increase by 2250% as compared to stage 2;

P = 0.00003 using Student’s t-test) and remained stable over the next 37 d The Coulombic efficiency was also considerably en-hanced, averaging 11 ± 1% (an increase by 5400% from stage 2).These results confirm the benefits of letting the anolyte flow into the cathode compartment to increase proton availability at the cathode However, this should be done with care to avoid overload-ing the cathode with excess substrate

3.2 Effect of cathodic acidification (stage 4) The cathodic acidification experiments were carried out with-out granules in the anode compartment This phase corresponds

to stage 4 inFigs 2 and 3 In the first place and before adding HCl, full-loop operation and active aeration were stopped so the cathode became an open-air cathode Under steady state

Fig 2 Evolution of the electromotive force (E emf ), maximum power (P max ), internal resistance (R int ) and Coulombic efficiency (CE) of the microbial fuel cell during the four stages of the experimental period Stage 1 corresponds to the start-up of the reactor Stage 2 is a period during which the reactor performance deteriorated Stage 3 corresponds to the operation of the anodic compartment with graphite granules Stage 4 corresponds to the operation in a single-chamber mode with an open air–cathode Cathodic acidification experiments were carried out during stage 4.

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conditions, the maximum power averaged 2.29 ± 0.32 mW, an

in-crease by 62% as compared to stage 3 (P = 0.0002; Student’s t-test)

The internal resistance was reduced to 48 ± 11 O and the

electro-motive force reached 0.66 ± 0.04 V However, the COD and SS

removal efficiencies were reduced to 50 ± 9% and 61 ± 12%,

respec-tively, as compared to stage 3 (Fig 3), and the Coulombic efficiency

dropped to 0.9 ± 0.4%, due to the absence of granules The

increased electrochemical performance of the MFC reactor in

open-air cathode conditions comes as no surprise, knowing that

this mode of operation results in increased oxygen availability at

the cathode and reduced internal resistance, as it has largely been

documented in the literature (Liu et al., 2004) After assessing the performance without HCl, the actual cathodic acidification experi-ments were carried out between days 95 and 120 subsequently in batch mode and in continuous manner

3.2.1 Batch experiments

In the beginning, cathodic acidification was conducted over a period of 14 d under different pH conditions in a batch mode by pumping 500 mL of diluted HCl solution into the cathodic com-partment The power response is shown in Fig 4, from which it can be seen that the injection of diluted HCl solution resulted in

(a)

(b)

Fig 3 Evolution of the (a) COD and (b) suspended solids (SS) concentrations in the influent, anodic outlet, cathodic outlet and corresponding total removal efficiencies during the four stages of the experimental period.

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an immediate power increase However, the improvement caused

by the decreasing pH was not steady and the power rapidly

de-creased again after the protons were consumed As a result the

catholyte had a pH around 8 at the end of the experimental time,

regardless of the initial pH applied It should be noted that both

the maximum power and the time taken to stabilize increased

when the pH was decreased Ultimately, the power went back to

the steady state conditions under neutral pH after a period of time

varying from 20 min to 8 h depending on the initial pH applied

According toFig 4, the optimal power production was attained

when the cathodic pH was decreased to 2 Under these conditions,

a maximum power of 4.5 mW (Rext= 40X) was achieved after

2.5 h, an increase by 180% as compared to a negative control (tap

water of pH 7.6) In a comparable test, also in batch mode but at

a cathodic pH of 1,Erable et al (2009)found an increase of power

by 250% in batch mode as compared to neutral conditions,

achiev-ing 3.5 mW in their 700 mL MFC system consistachiev-ing of two

cham-bers with an open-air cathode However, in our case when the

catholyte pH was further decreased to 1, the power production

reached a maximum of 3.6 mW after 2.3 min, followed by a rapid

decrease The catholyte was then characterized by a green color

and an acidic pH of 2, which indicated that the protons had not

been consumed in their entirety by the reaction at the cathode

The resistance to HCl of the stainless steel current collector used

at the cathode and that of the platinum coated carbon cloth

cath-ode were tested by exposing samples at a pH of 1 and, within two

days, stainless steel was completely degraded resulting in a green

color solution, whereas the carbon cloth was unaffected The green

compound was identified to be FeCl2 – a greenish tetrahydrate

responsible for the green colored solution – and it can be

hypoth-esized that Fe and HCl combined to form FeCl2, a reaction that is

shown in Eq 2

Such redox reaction was detrimental to the cathodic reaction

and resulted in decreased power production at pH 1 It should be

noted here that in the study ofErable et al (2009), this problem

was not encountered as they utilized brass as current collector

3.2.2 Continuous experiments

Continuous acidification experiments were carried out over a

period of 10 d between day 110 and 120 Under continuous

acidi-fication, stable power could be generated Power curves at different

catholyte pH confirmed the trend of increasing power generation

with decreasing pH (Fig 5a) Continuous cathodic acidification at

pH = 1.2 allowed the generation of power supply 380% as high as

what could be obtained with tap water (pH 7.6) Under such

con-ditions, the reactor generated a maximum power of 7.4 mW

(Rext= 15X), the maximum observed in this study Two phosphate buffer solutions with ionic concentrations of 102and 104M to cover the entire range of our acidic solutions were used as negative controls to demonstrate that the improved concentration is due to increased proton access and not simply due to increased ionic strength It appears clearly from Fig 5 that the effect of ionic strength was limited as compared to that of pH

The polarization curves provide a deeper insight into the impact

of acidification on the electrical performance of the MFC (Fig 5b) First, the internal resistance decreased with the pH from 58 O at pH 7.6 to 11Xat pH 1.2 The effect on the electromotive force was more complex Eemffirst increased when pH was decreased and reached an optimum value of 0.7 V at a pH of between 3 and 2 The Nernstian effects, whereby the cathodic potential increases with the proton concentration, can explain this However, further decrease in pH resulted in a decreasing electromotive force that reached 0.58 V at a pH of 1.2 and this was related to the corrosion reaction previously described that affected the potential of the cathode when the pH became too acidic However, in terms of power generation, higher values were obtained at pH 1.2 than 2, which shows that, overall, the impact of acid on the internal resis-tance was stronger than that on the electromotive force

Finally, we analyzed the pH of the solution in the outlet of the cathodic compartment and it appeared that the pH was slightly higher than that of the feed to the cathodic compartment for feed

pH higher than 2 For a solution of pH 2 or less, the pH in the outlet was similar to that of the inlet, indicating that the proton limita-tion might be overcome under these condilimita-tions in our MFC system

At pH 2, the maximum power was achieved at a current of 15 mA (Fig 5a) and, since 1 mol of electron reacts with 1 mol of protons in the cathodic reaction, the quantity of pH 2 solution to maintain the

0

1

2

3

4

5

Time (min)

pH 7.6 pH 6

pH 4 pH 3

pH 2 pH 1 01

2 3 4

Time (min)

Fig 4 Power response after batch acidification of the cathode (R ext = 40 O) Insert:

details of the first 30 min.

0 2 4 6 8

0 0.2 0.4 0.6 0.8

Current ( A)

Current ( A)

Buffer 10 M Buffer 10 M

(a)

(b)

Fig 5 (a) Power curves under continuous acidification of the cathode at different pH; (b) polarization curves under continuous acidification of the cathode at different pH.

Trang 7

current at 15 mA was estimated at 1.3 L d1 That corresponds

roughly to as little as 2 mL of 37% HCl solution, as commonly

avail-able for sale Considering the HRT of the reactor (2.4 h), this

corre-sponds roughly to 0.07 mL of 37% HCl solution used per litre of

wastewater treated

3.2.3 Reversibility of the cathodic acidification experiments

With the use of the Selemion membrane that allows protons to

be transferred only in one direction from the anode towards the

cathode, the pH at the anode was never affected by the drastic

change of pH in the cathode compartment The MFC operation in

a reversible mode from cathodic acidification back to open-air

cathode operation was further assessed at the end of stage 4

(day 120–140) As can be seen fromFig 2, the MFC immediately

re-verted to performance similar to what was observed before the

cathodic acidification experiments The internal resistance and

electromotive force averaged 47 ± 8 O and 0.63 ± 0.05 V,

respec-tively, resulting in a maximum power of 2.17 ± 0.01 mW, not

significantly different from the values obtained before the

acidifi-cation experiments (P = 0.6; Student’s t-test) FromFig 3, it can

be further seen that the COD and SS removal efficiencies were also

largely unaffected by the cathodic acidification experiments, with

mean values of 53 ± 7% and 62 ± 2%, respectively As a result the

Coulombic efficiency also remained stable at 0.4 ± 0.2% This

further shows that bacteria possibly present as a biofilm on the

cathode played little to no role in power generation as compared

to abiotic processes catalyzed by platinum This is because any

bio-film on the cathode would have been damaged by the acidic

treat-ment but nevertheless, the electrical performance remained stable

3.3 Performance assessment as compared to the literature

Table 1compares the performance of our MFC set-up to the

lit-erature available

Under the optimized conditions, the internal resistance of our

MFC system was 11Xand the electromotive force was 0.6 V These

values correspond to the state of the art as showcased inTable

1.The maximum power attained was 7.4 mW, which corresponded

to a volumetric power of 2 W m3by considering the total volume

of our MFC being of 3.5 L (anodic compartment of 2.9 L and catho-dic compartment of 0.6 L) This can appear low considering the state of the art presented inTable 1 However, in terms of power generated on a per cell basis, our MFC was in the highest range This is because the volumetric power is a decreasing function of the geometrical parameters However, by reducing the size too much, the raw power output is also expected to decrease and this mathematically increases the number of cells that would have to

be stacked together in order to provide enough power to be of use Considering the very low maturity of MFC-stacking, this is a serious obstacle to MFC application Furthermore, the electrical resistivity and the volume of all the connectors that will be used

to perform stacking will also affect the electrical performance of the system and its total volume The impact on a volumetric power based on the total volume and not on the working volume may be-come negative

Moreover, the substrate used to operate an MFC – ranging from acetate or glucose to complex industrial wastewater – is known to impact widely on its performance and the best perfor-mance from the electrical as well as from the wastewater treat-ment point of views is usually obtained with synthetic and simple substrates (see Table 1) However, in view of optimizing MFCs for wastewater treatment, it is also useful to assess their performance with domestic wastewater, but this does not play

in favor of our system It is interesting to see that our system could remove in average above 50% of the COD and 56% of the

SS at a HRT of 2.4 h With domestic wastewater, Ahn and Logan (2010) found COD removal higher than 88% in batch mode However, in that same study, during continuous operation max-imizing power generation and at ambient temperature, COD re-moval was reduced to 19%, with a Coulombic efficiency of 0.7%

at a HRT of 4.2 min In our study, the COD removal efficiency was higher but Coulombic efficiency also remained below 1%,

Table 1

State of the art in microbial fuel cell research.

Substrate OCV (V) E emf (V) R int (X) P max (mW cell 1

) V (mL) Pv max (W m 3

) Ref.

Two chamber design, ferricyanide catholyte

Two chamber design, aerated cathode

Two chamber design, open-air cathode

Single chamber design, open-air cathode

NA, not available.

Trang 8

granules In the latter case, Coulombic efficiency was much

high-er at 11%

Low Coulombic efficiency has to be related to the complex

nat-ure of domestic wastewater allowing fermentation and other

biological processes to interfere with electricity generation

Fur-thermore, it seems that electrochemically active bacteria can only

use a limited range of products For example,Freguia et al (2008b)

showed that glucose had to be converted into acetate before it can

be utilized for electricity generation It is consequently not

surpris-ing that butyrate and acetate, respectively, generated 62% and 82%

more power than domestic wastewater in the study of Ahn and

Logan (2010) Even though the low Coulombic efficiency could be

seen as a problem, it is merely the result of the MFC having reached

its maximum capacity as an electricity generation device The

elec-tromotive force cannot be expected to go much beyond the values

observed in the present study – the theoretical maximum voltage

achievable in open circuit being approximately of 1.1 V in typical

MFC conditions (Logan et al., 2006) – and our values of internal

resistance are also competitive As a result, any organic matter in

excess is further removed by other means The vertical

configura-tion of the reactor allowed sludge accumulaconfigura-tion at the bottom of

the anodic compartment, where fermentation and even probably

methane production were allowed to take place, even though our

design did not allow for any gas collection and analysis to verify

that hypothesis This made our MFC a hybrid system that overall

contributed to improve the elimination of organic matter, which

is the primary goal of a wastewater treatment plant Overall, it

seems more important to optimize the effluent COD and SS

removal efficiencies in the anodic compartment rather than the

Coulombic efficiency in wastewater treatment application, which

further renders possible the introduction of the anolyte inside

the cathode compartment without reducing the performance of

the reactor, as shown in this study

4 Conclusion

The present study shows the importance of overcoming proton

limitation in an MFC system and this was achieved first by letting

the anolyte flow into the cathode compartment (full-loop

opera-tion) and second by acidifying the cathode The latter experiment

led to the best electrochemical performance and it appeared

clearly that the anolyte quality must be good enough before being

allowed to enter the cathodic compartment We believe that the

future of the MFC technology as a treatment plant lies in the design

of hybrid systems that will harvest part of the energy in the form of

electricity and the rest in the form of biogas

Acknowledgements

This work was supported by a Grant from the Environment &

Water and Industry Development Council, Singapore (MEWR

651/06/159)

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