Journal of Environmental Management 236 (2019) 317–322

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Journal of Environmental Management

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

Research article

Solubilization of organic matter by electrochemical treatment of sludge: T

Influence of operating conditions
M. Pérez-Rodrígueza, A. Canob, U. Durána, J.A. Barriosa,∗
a
Instituto de Ingeniería UNAM, Circuito Escolar, Ciudad Universitaria, 04510 México, D.F., Mexico
b
Tecnológico de Monterrey, Escuela de Ingeniería y Ciencias, Ave. Eugenio Garza Sada 2501, 64849 Monterrey, N.L., Mexico

A R T I C LE I N FO A B S T R A C T

Keywords: Sludge generated after wastewater treatment represents an important challenge due to the large amounts pro-
Boron-doped diamond electrode duced and the need to adequately treat it. Anaerobic digestion is the preferred treatment process to obtain
Electrooxidation renewable energy as well as a biosolid with the potential to be reused in land application. This process generates
Sludge treatment biogas (methane and carbon dioxide) that may be used for energy co-generation. However, anaerobic digestion
Solubilization
is limited by the hydrolysis step since bacteria need to break down organic matter and large molecules to allow
Taguchi experimental design
conversion into biogas. In this study, electrochemical treatment of sludge is proposed to solubilize organic
Waste activated sludge
matter. Boron-doped diamond electrodes were used to treat waste activated sludge under different experimental
conditions (current density, flow rate, time) to evaluate their influence on the solubilization of organic matter (in
terms of chemical oxygen demand). The degree of solubilization ranged between 0.31 and 1.78%. Based on the
results, optimal operating conditions were current density of 19.3 mA cm−2, flow rate of 4 L min−1, and treat-
ment time of 30 min. Furthermore, treatment flow rate was found to play a key role in solubilization, as the
process is controlled by mass transfer.

1. Introduction
Wastewater treatment generates considerable amounts of sludge
that need to be adequately treated to reduce risks to human health and
the environment. Its management may represent up to 50% of the total
operating costs of wastewater treatment plants. For this reason, careful
planning is required to reduce or offset these costs (Appels et al., 2008).
Since wastewater sludge is composed of organic and inorganic so-
lids, as well as a large percentage of water (usually more than 95%),
anaerobic digestion is used to treat about 70% of the sludge produced
globally (Tyagi et al., 2014). This process partially converts organic
matter into biogas (mostly methane) which can be used to produce
renewable energy.
Anaerobic digestion is composed of four main stages: hydrolysis,
acidogenesis, acetogenesis, and methanogenesis. These processes are
carried out by different groups of microorganisms. Among them, hy-
drolysis has been identified as the limiting step of anaerobic digestion
(Appels et al., 2010b), as it depends on the transformation of complex
organic molecules to easily biodegradable products that may be readily
used by microorganisms. In this respect, it is estimated that organic
matter degradation in the anaerobic digestion of waste activated sludge
(WAS) is limited to between 20 and 50% (Tyagi et al., 2014). This is due
to the fact that this type of sludge is mainly composed of biomass
generated in wastewater secondary treatment processes, which is dif-
ficult to degrade in the anaerobic process (Gavala et al., 2003).
Several relevant studies have been published regarding sludge
minimization in treatment facilities. For instance, Chiavola et al.
(2015), evaluated the electro-kinetic disintegration of secondary
sludge, which resulted in microbial cell lysis and the release of in-
tracellular material. In addition, following this behavior, several
treatment methods have been proposed to solubilize organic matter
prior to anaerobic digestion, with the aim of improving biogas pro-
duction. These methods may be physical, chemical, mechanical, bio-
logical, or thermal (Carrère et al., 2010; Shehu et al., 2012; Ye et al.,
2016). Subsequently, there is considerable interest in testing processes
that maximize solubilization of organic matter prior to anaerobic di-
gestion (Feki et al., 2015).
Over the last decade, different electrochemical treatments have
been applied to sludge, including electrochemical oxidation. This ad-
vanced oxidation process is based on the generation of hydroxyl radi-
cals (OH•) at the electrode surface which causes cell breakage and the
release of intracellular material as well as the conversion of organic
matter to low molecular weight compounds (Pilli et al., 2015; Xu et al.,
2014).

∗
Corresponding author.
E-mail address: jbarriosp@iingen.unam.mx (J.A. Barrios).

https://doi.org/10.1016/j.jenvman.2019.01.105
Received 7 October 2018; Received in revised form 9 January 2019; Accepted 27 January 2019
Available online 06 February 2019
0301-4797/ © 2019 Elsevier Ltd. All rights reserved.
M. Pérez-Rodríguez et al. Journal of Environmental Management 236 (2019) 317–322

In this respect, several electrode materials and configurations have Table 1

been studied to maximize solubilization of organic matter and improve Physicochemical characteristics of raw sludge.
biogas production. These materials include titanium coated with ru- Parameter Mean value Standard deviation
thenium dioxide (Ti/RuO2) mesh plate electrodes (Yu et al., 2014; Yuan
et al., 2016), iron electrodes (Feki et al., 2015), iridium oxide coated pH 6.99 0.20
Conductivity, μS cm−1 1263 225
titanium (IrO2/Ti) film electrodes (Yang et al., 2014), and boron-doped
Total solids, % 2.8 0.03
diamond electrodes (BDD) (Barrios et al., 2016). Volatile solids, % of total solids 71.4 0.17
In particular, BDD electrodes have been used for several environ- Chemical oxygen demand (total), mg L−1 32,036 6
mental engineering applications as these types of electrodes have been Soluble chemical oxygen demand, mg L−1 156 1
reported to be among the most stable as they exhibit a high resistance to Dissolved oxygen, mg L−1 0.10 0.01

corrosion, a high oxygen evolution potential, high thermal con-

ductivity, as well as a wide electrochemical window (Chen et al., 2003;
sludge is a heterogeneous matrix, chemical oxygen demand (COD) is
Souza et al., 2016; Wu et al., 2009). BDD application for the treatment
usually variable even for the same treatment facility as it depends on
of sludge has resulted in relatively low organic matter solubilization
several factors such as wastewater quality and process operating con-
(2.1–2.8%); however, the increase in methane production after anae-
ditions. For instance, total COD was lower than values reported for
robic digestion is somewhat higher than studies performed with other
sludge with 3 and 4% total solids (Barrios et al., 2016; Yuan et al.,
electrode materials and configurations (69–81%). In addition, it has
2016). From Table 1, it is clear that most of the organic matter is
been reported that treatment increases the biogas production rate
contained in the sludge solids as only 0.5% of the total chemical oxygen
which means that anaerobic digestion is accelerated (Barrios et al.,
demand corresponds to the soluble fraction.
2016).
Despite these encouraging results, the influence of different oper-
ating conditions such as current density, flow rate, and treatment time
2.2. Electrochemical treatment
on organic matter solubilization through electrochemical oxidation has
not so far been reported.
Electrochemical treatment was performed in a Diacell® 106 (boron-
The current density for the electrochemical reaction is directly re-
doped diamond on silicon substrate electrodes; circular geometry with
lated to the amount of hydroxyl radicals generated at the electrode
an active surface of 70 cm2; WaterDiam) operating in semi-continuous
surface, which should almost immediately react with the organic matter
mode (see Fig. SM-2). Sludge was mixed and fed to the electrochemical
(direct oxidation) and may eventually produce less powerful secondary
cell from a temperature-controlled vessel (25 °C) with a peristaltic
oxidants (mediated oxidation) such as persulfate (S2O82), percarbonate
pump (Cole-Parmer, model 7553-20, 6–600 RPM). Power was supplied
(C2O62−) and hydrogen peroxide (H2O2) (Comninellis and Chen, 2010).
by a BK Precision, model 9184 unit. Cleaning of the Diacell® was carried
Reactor design plays a crucial role in the electrochemical process,
out after each treatment using a solution of sodium sulfate (0.5% w/v)
particularly in terms of hydrodynamics: the presence of by-passes or
at a pH of 2 (adjusted with sulfuric acid) and applying the maximum
stagnant zones leads to problems in process performance in terms of
current provided by the power source (2 A, equivalent to
both efficiency and by-product formation (Palmas et al., 2007). Finally,
28.6 mA cm−2) for 30 min.
the treatment time is relevant in the solubilization of organic matter as
longer treatment times would increase the energy input needed for
treatment and would reduce the feasibility of the process.
2.3. Degree of solubilization
Consequently, this paper reports the influence of different operating
conditions (current density, treatment flow rate, and treatment time) on
The degree of solubilization has been used to measure the solubi-
organic matter solubilization using an electrochemical cell for sludge
lization of organic matter present in sludge. Several equations have
treatment and focuses on identifying the most influential of these
been proposed but the one defined by Appels et al., 2010a has been
parameters.
widely applied (Eq. (1)). This equation considers that organic matter in
sludge is determined by the chemical oxygen demand (COD), both total
2. Experimental methodology
and soluble, and evaluates the proportion of organic matter that be-
comes soluble after treatment.
2.1. Collection and preparation of sludge samples
Degree of solubilization = ((Soluble COD treated
As mentioned previously, waste activated sludge (secondary sludge)
exhibits less biodegradability than primary sludge, thus, this research − Soluble COD untreated)
focuses on WAS pre-treatment. Waste activated sludge was obtained /Total COD untreated)) ∗ 100 (1)
from a municipal wastewater treatment plant located in Mexico City
(flow rate: 2.18 m3 s−1). WAS samples were collected from the waste
valve of the secondary settling tank (see layout in supplementary ma-
terial Fig. SM-1) in plastic containers (V = 20 L) and transported to the 2.4. Physicochemical analyses
Environmental Engineering Laboratory, UNAM, where they were stored
at 3 °C. To increase the solids content of the samples (thickening), pH, conductivity, total and volatile solids, as well as total and so-
sludge was decanted after 2 h of sedimentation and it was further luble chemical oxygen demand were determined according to the
centrifuged at 1400 g for 20 min. Total solids (TS, w/w) content was Standard Methods (APHA-AWWA-WEF, 2005). Total chemical oxygen
adjusted to 3% TS based on prior studies (Barrios et al., 2016). Table 1 demand was only measured in raw sludge in order to calculate the
shows the physicochemical characteristics of thickened untreated (raw) degree of solubilization, soluble chemical oxygen demand was de-
sludge. pH and volatile solids were within typical values for untreated termined after centrifugation (1,400×g for 20 min) and filtering of the
waste activated sludge according to Metcalf and Eddy, 2003). Con- supernatant using 0.45 μm filters (Millipore®). The dissolved oxygen
ductivity was assumed to be high enough to allow electron transport concentration was measured using a YSI model 58 dissolved oxygen
through the sludge, taking into consideration that other work on elec- meter. Soluble carbohydrates were determined by the Anthrone method
trooxidation of wastewater demonstrated oxidation of organic pollu- with glucose as a standard and soluble proteins were determined using
tants at half this value (Frontistis et al., 2011). Since waste activated the Lowry method with bovine serum albumin (BSA) as a standard.

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M. Pérez-Rodríguez et al.
2.5. Experimental design
A Taguchi's L9 Orthogonal Array (OA) experimental design was
applied since it is a statistical method widely used for identifying cri-
tical parameters in industrial processes. It is based on the concept of
orthogonal matrices that help planning a set of experiments to obtain
the optimum values of selected parameters and identify the most in-
fluential of these (Sadrzadeh and Mohammadi, 2008; Uday et al.,
2015). Experimental results from the Taguchi design are generally re-
ported based on the signal-to-noise ratio (S/N) (Googerdchian et al.,
2018a). S/N ratio is a parameter recommended by Taguchi as it mea-
sures deviation among the factors evaluated. Based on the nature of this
study, the S/N ratio was evaluated as “larger is better” to obtain the
best operating conditions of the electrochemical process in order to
maximize organic matter solubility and identify those factors that
control or have more influence in such processes.
Fixed experimental parameters were total solids (3%), temperature
(25 °C), sludge volume (1 L), and mixing speed in sludge vessel
(500 rpm) according to previous reports (Barrios et al., 2016).
Variable experimental parameters were current density, flow rate
and treatment time (see Table SM-1). The values defined for each
parameter were based on previous studies (Barrios et al., 2016) as well
as on the equipment configuration. The experimental design defined
three levels for each of these parameters (see Table SM-2) and required
9 treatment tests, which were performed in duplicate. The response
variable evaluated was the degree of solubilization of organic matter as
maximizing this parameter would be expected to result in an im-
provement of biogas production during anaerobic digestion (Feki et al.,
2015). Contour plots were carried out using Minitab software.
3. Results and discussion
3.1. Degree of solubilization (DS)
During electrochemical treatment tests, there was no apparent
polymeric film formation over the electrode surface as demonstrated by
the indirect measure of cell potential. This maintained a constant value
throughout the tests (Fig. 1). After electrochemical treatment, the
sludge supernatant increased in apparent viscosity (visual observation).
Waste activated sludge contains microbial cells that agglomerate into a
floc matrix that retains water and keep cells bound due to the presence
of extracellular polymeric substances (EPS) (Jin et al., 2004). In this
regard, it has been reported that electrochemical treatment has an ef-
fect on EPS by releasing them into the aqueous phase in the form of
proteins and carbohydrates (Yuan et al., 2011) and this may cause the
increase in viscosity (Wang et al., 2006). Preliminary results demon-
strate the release of EPS in pre-treated sludge (444% for proteins and
262% for carbohydrates vs. untreated sludge). Some authors (Kapałka
et al., 2008) have shown that BDD electrodes have a high oxidation
potential attributable to hydroxyl radicals and also dissolved molecular
Fig. 1. Cell potential during treatments.
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Journal of Environmental Management 236 (2019) 317–322
oxygen when air/oxygen saturated solutions are tested. However, in
this case, the sludge had such a high chemical oxygen demand (COD0:
32,036 mg L−1) due to the large amount of organic matter, that the
oxygen present was negligible (< 0.11 mg L−1) and thus cell breakage
was mainly related to the effect of hydroxyl radicals.
The degree of solubilization obtained for the experimental condi-
tions tested ranged from 0.31 to 1.78% which is lower than that re-
ported elsewhere (Barrios et al., 2016). Contour plots (Fig. 2) allow
visualization of the degree of solubilization under different combina-
tions of operating conditions, where darker areas indicate higher so-
lubilization values. The main findings are described below.
Fig. 2 a) shows the contour plot for the degree of solubilization for
different values of current density and time. According to this plot,
better solubilization is achieved for medium values tested for both
parameters (19.3 mA cm−2 and 30 min). In addition, the plot suggests
that low current densities require longer contact times to obtain
medium solubilization of organic matter (60% of the maximum degree
of solubilization), although this behavior does not seem to be linear.
Medium values of current density apparently produce sufficient
amounts of hydroxyl radicals merely to break-up microbial cells and
release intracellular organic matter, as well as extracellular polymeric
substances, into solution, avoiding mineralization. Higher current
densities do not result in higher solubilization as such conditions pro-
mote oxidation of organic matter and may allow the formation of sec-
ondary oxidants that have a weaker oxidation at slower rates than the
hydroxyl radicals (Feng et al., 2013). Both phenomena would even-
tually cause mineralization which is not the objective of this study as it
would reduce the amount of organic matter available for anaerobic
digestion.
Fig. 2 b) shows the plot for flow rate vs. time where best solubili-
zation is obtained when a medium time (30 min) and a high flow rate
(3.8 L min−1) are tested. This clearly shows that the process is mass
transfer controlled, as it is necessary for the sludge to come into contact
with the electrode surface for the reaction to take place. Other reports
(Nava et al., 2008) have indicated that hydrodynamics play a key role
in the electrooxidation of organics as this phenomenon promotes con-
tact between hydroxyl radicals and organic matter. Moreover, Feng
et al. (2013), suggest that electrooxidation requires a good mechanical
design to promote turbulence and reach high Reynolds values that in-
crease oxidation efficiencies. As the present work uses a commercial
cell, it was not possible to alter its geometry. However, according to the
commercial supplier, the Diacel® uses a turbulence promoter to improve
flow rate within the cell. As a result, experimental conditions only allow
modifying the operating flow rate or the inter-electrode gap to increase
mass transfer.
With respect to Fig. 2 c), contour plot presents the degree of solu-
bilization for flow rate and current density. It is clear that the highest
levels of solubilization require flow rates that exceed those tested ex-
perimentally here (1.8–3.8 L min−1). It should be noted that sludge
viscosity is generally higher than that of water and thus affects
M. Pérez-Rodríguez et al. Journal of Environmental Management 236 (2019) 317–322

Fig. 2. Contour plot analyses of the degree of solubilization for different operating conditions: a) Time vs. current density; b) Time vs. flow rate; c) Current density vs.
flow rate.

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M. Pérez-Rodríguez et al.
Fig. 3. Main effects plot for S/N ratios.
hydrodynamic behavior in reactors. At low flow rates, solubilization is
also low since organic matter is not being transferred to the surface of
the electrode by convection, and thus hydroxyl radicals may accumu-
late in a thin layer at the interface of the electrode and the sludge,
where they may react with each other to form hydrogen peroxide
(Martínez-Huitle and Andrade, 2011). Even though hydrogen peroxide
is considered a powerful oxidant, it is neutralized by catalase, an en-
zyme present in biomass (Baldry, 1983). Moreover, medium current
densities, which are lower than those evaluated previously (Barrios
et al., 2016) may reduce the cost of energy needed for treatment and
result in a positive energy balance.
3.2. Statistical analysis
To obtain the greatest solubility, the optimum conditions have the
highest S/N ratio (Adewale et al., 2017). This corresponded to Ex-
periment D (30min, 19.3 mAcm−2 y 3.8 L min−1) with a S/N ratio of
4.4022, within a range of −7.7443 to 4.4022. To determine the factor
with the highest influence in solubilization, Fig. 3 shows the main ef-
fects plot for S/N ratio for each of them (time, current density, and flow
rate). The factors with the higher values are current density and flow
rate. Medium (19.3 mA cm−2) and high values (3.8 L min−1) for these
factors, respectively, result in higher organic matter solubilization.
An analysis of variance (ANOVA) led to the same conclusions as for
the S/N ratio obtained with the Taguchi design. For a confidence in-
terval of 95%, identified with the F distribution, the most influential
factors would have values above 1 (Googerdchian et al., 2018b). In this
case, these factors were the flow rate (F = 1.91) and current density
(F = 1.54) while time had the lowest significance (F = 0.19).
4. Conclusions
Different operating conditions for sludge electrooxidation, in terms
of current density, flow rate and time, resulted in different degrees of
solubilization of organic matter. The maximum degree of solubilization
obtained was 1.78% which appears to be low in comparison with other
advanced oxidation treatments. These results are slightly lower than
values recorded under similar conditions (2.1–2.8%). However, pre-
vious studies with a similar degree of solubilization, using the same
types of electrodes and configuration, showed increases of up to
76–80% following the anaerobic digestion process (Barrios et al.,
2016). Soluble organic matter increased after all treatments due to
rupture and release of intracellular and extracellular material. As a
result, the sludge supernatant increased its viscosity due to the solu-
bilization of extracellular polymeric substances. Of the experimental
conditions tested, the sludge flow rate was the most important para-
meter confirming that the process is mass transfer limited and requires
high flow rates that promote turbulence within the cell. In this sense,
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Journal of Environmental Management 236 (2019) 317–322
the solubilization of extracellular polymeric substances after treatment
is being evaluated to demonstrate the destruction of biomass with
electrochemical treatment (Song et al., 2010). More studies are needed
to confirm the correlation between the degree of solubilization and
biogas production as well as to provide information on physicochemical
changes of biomass after treatment.
Acknowledgments
This work was supported by the Instituto de Ingeniería Research
Fund 2016–2017 Project 6328. Mónica Pérez is a graduate student at
Posgrado de Ingeniería UNAM with a scholarship from Consejo
Nacional de Ciencia y Tecnología(CONACYT). The experimental work
was performed at the Environmental Engineering Laboratory
(Laboratorio de Ingeniería Ambiental, LIA) of the Instituto de Ingeniería
UNAM. The Laboratory is certified under ISO 9001:2015 (Certificate
number: CMX C SGC 155 2017; valid through November 9th, 2020).
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://
doi.org/10.1016/j.jenvman.2019.01.105.
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