AnMBR Treatment of High-Strength Starch-Based

Wastewater: Impact of Cleaning Process

and CEBs on Membrane Fouling
Joshua Snowdon 1; Kripa S. Singh 2; and Gustavo Zanatta 3

Abstract: An anaerobic continuously stirred tank reactor (CSTR) integrated with an external tubular nanofiltration membrane module was
operated for 466 days. Studies were conducted to compare the efficiencies in flux and operational permeability recovery of two different
chemical cleaning processes. Chemically enhanced backwashes (CEBs) were applied for approximately 176 days of the study and their
influence on chemical cleaning performance and membrane fouling rate following chemical cleanings were also investigated. The anaerobic
nanofiltration membrane bioreactor used in the study was fed a high-strength, potato starch–based synthetic wastewater (average chemical
oxygen demand of 83.4 g=L and average total suspended solids of 5.8 g=L). Important findings were that a static, one-phase cleaning process
using caustic cleaning chemicals outperformed a dynamic, three-phase cleaning process that also incorporated acidic cleaning chemicals; the
acidic phase of the three-phase cleaning had a detrimental effect on the overall cleaning procedure’s performance; CEBs enhanced the per-
formance of cleaning processes; and, finally, caustic cleaning solutions provided benefits to both membrane cleaning effectiveness and rate of
fouling in the short term but may lead to an increased rate of membrane fouling in the long term. DOI: 10.1061/(ASCE)EE.1943-
7870.0001524. © 2019 American Society of Civil Engineers.
Author keywords: Anaerobic membrane bioreactor; Chemical cleaning; Chemically enhanced backwash; Membrane fouling;
Nanofiltration membrane.

Introduction anaerobic systems such as high concentration of biomass retention

With an ever-growing population, sustainable water and waste-
water treatment technologies will become essential in solving water
scarcity problems prone to develop in upcoming years. Anaerobic
membrane bioreactors (AnMBRs) offer a promising means of
sustainable and value-added wastewater treatment, coalescing the
benefits of anaerobic digestion for the treatment of municipal and
industrial wastewaters with the almost 100% solid–liquid separa-
tion potential of membrane integrated wastewater treatment tech-
nologies. Anaerobic digestion for wastewater treatment provides
certain benefits over more commonly used conventional aerobic
technologies, such as high-rate suspended-growth systems, very
high removal efficiencies of biochemical oxygen demand (BOD)
and chemical oxygen demand (COD), resource recovery (value-
added products such as methane in its biogas and the possible
recovery of select biochemicals such as volatile fatty acids in its
mixed-liquor and effluent), lower sludge yield, and low carbon
footprint (Kinnunen et al. 2015; Meng et al. 2009; Ozgun et al.
2013; Pilli et al. 2016; Skouteris et al. 2012). Through the integra-
tion of membrane separation technologies within anaerobic di-
gestion, further benefits are provided over non-membrane-based
1
Graduate Student, Dept. of Civil Engineering, Univ. of New
Brunswick, 17 Dineen Dr., Fredericton, NB, Canada E3B 5A3 (corre-
sponding author). Email: h557d@unb.ca
2
Professor, Dept. of Civil Engineering, Univ. of New Brunswick, 17
Dineen Dr., Fredericton, NB, Canada E3B 5A3. Email: singhk@unb.ca
3
Process Engineer, ADI Systems, Inc., 370 Wilsey Rd., Fredericton,
NB, Canada E3B 6E9. Email: gustavo.zanatta@evoqua.com
Note. This manuscript was submitted on July 18, 2018; approved on
October 26, 2018; published online on March 6, 2019. Discussion period
open until August 6, 2019; separate discussions must be submitted
for individual papers. This paper is part of the Journal of Environmental
Engineering, © ASCE, ISSN 0733-9372.
(as the effectiveness of biomass retention becomes independent of
sludge settleability due to membranes’ near-complete solid–liquid
separation capabilities), compact design, and, most importantly, the
ability to produce a superior quality effluent for possible recycle
or high-quality discharge to meet stringent wastewater disposal
regulations (Skouteris et al. 2012).
What continues to remain the most significant factor limiting the
cost effectiveness of membranes in wastewater treatment applica-
tions (both municipal and industrial) is membrane fouling (Ramos
et al. 2014). Membrane fouling may be defined as the combination
of processes leading to flux deterioration and transmembrane pres-
sure (TMP) increase due to surface or internal pore blockage of the
membrane (Lousada-Ferreira et al. 2014). Surface or internal pore
blockage is generated through the contact and deposition of sus-
pended particles, colloids, and solutes present in the mixed liquor
on the membrane surface or in its pores, henceforth referred to as
foulants (Iorhemen et al. 2016). Membrane fouling increases TMP
and decreases flux, while the control of foulant deposition increases
manpower and energy requirements, demands costly chemical
cleaning (that further requires waste handling), and may also
result in increased deterioration of the membrane material, affecting
its lifespan (Ramos et al. 2014). Foulant mitigation for a membrane
module is a two-pronged approach: first, the membrane-fouling
rate should be minimized, and second, technologies to restore the
flux of a fouled membrane must be implemented (Liao et al. 2006).
Physical cleaning processes (e.g., gas scouring, backwashing,
relaxation) have only proven to be effective at removing some pore-
clogging and cake-layer membrane foulants (Liao et al. 2006).
Chemical cleanings, using low- to moderate-strength corrosive or
caustic solutions, are highly effective at removing both the gel layer
and cake layer developed through solids deposition on the mem-
brane surface and pore-blocking foulants, making them typically
more efficient at recovering membrane flux. These chemical

© ASCE 04019018-1 J. Environ. Eng.

J. Environ. Eng., 2019, 145(5): 04019018

cleanings can be performed either as a preventive maintenance op-
eration to maintain permeate flux [through incorporating chemical
cleanings into regular physical cleaning processes, for example
chemically enhanced backwashes (CEBs)], or as a recovery oper-
ation to recover membrane flux from a severely fouled membrane
module (Ramos et al. 2014). Chemically enhanced backwashes
combine conventional physical backwashing with chemical clean-
ing in one process, which could be of high importance for the
design and operation of membrane bioreactor (MBR) systems
for wastewater treatment. Recent studies using CEBs have typically
been performed at long intervals (weekly or monthly cleaning proc-
esses) (Zhou et al. 2014). There have been few comparative studies
on different cleaning methods and conditions, and scant informa-
tion exists on CEBs, in general, in the literature (Ramos et al. 2014;
Zhou et al. 2014). Snowdon et al. (2018) observed that one 60 s
CEB every 24 h resulted in increased permeate flux, operational
permeability, and net flux, demonstrating CEBs’ effectiveness as
a preventive maintenance operation.
This research project compared the efficiency of two different
chemical cleaning processes applied to one membrane module
integrated within a continuously operated pilot-scale AnMBR sys-
tem. The two chemical cleaning processes were applied to the
membrane module only once it was severely fouled, acting as a
recovery operation. As a secondary objective, the project investi-
gated the impact of daily CEBs on the effectiveness of each
chemical cleaning process. The novel pilot-scale AnMBR system
consisted of a 1,000 L anaerobic continuously stirred tank reactor
(CSTR) integrated with an external nanofiltration tubular mem-
brane module. The reactor and membrane configuration provided
benefits over conventional cleaning processes in that the membrane
module did not need to be removed for chemical cleanings (since it
could be isolated from the CSTR through a recirculation loop). This
resulted in minimal downtime and maintenance work required for
chemical cleaning processes. With few direct comparative studies
on different chemical cleanings applied to the same membrane
module, and little information in the literature on CEBs, there
Fig. 1. Simplified PFD of experimental setup.
© ASCE 04019018-2
J. Environ. Eng., 2019, 145(5): 04019018
are, to the authors’ best knowledge, no studies investigating the
impact of daily CEBs on the effectiveness of chemical cleaning
processes.
Materials and Methods
Reactor Configuration
A 1,000 L stainless steel anaerobic CSTR was equipped with an
external nanofiltration tubular membrane module and operated in
cross-flow mode. A simplified process flow diagram (PFD) of the
configuration may be viewed in Fig. 1. The anaerobic CSTR was
equipped with a heat wrap, which maintained the reactor temper-
ature at an average value of 36.2°C (
0.5°C) throughout the dura-
tion of the study. The operational temperature of approximately
36°C was selected since it is the upper limit of mesophilic anaerobic
digestion (25°C–35°C) and maximized biogas generation, which
was desired (Metcalf & Eddy, Inc. 1991).
Reactor-mixed liquor was continuously recirculated from the
CSTR to the membrane module and back into the CSTR by a pro-
gressive cavity pump (Nemo, New Brunswick, Canada). This pump
maintained a mixed-liquor flow rate of 6,000 L=h, which resulted
in the targeted membrane surface cross-flow velocity of 2.5 m=s
and a complete recirculation of reactor contents every 10 min.
A cross-flow velocity of 2.5 m=s was selected since it is deemed
to be the minimum operational cross-flow velocity that must be
maintained for the membrane module based on manufacturer rec-
ommendations. It was desired to operate at the lower spectrum of
the operational cross-flow velocity to minimize energy demands.
The membrane module was cylindrical in shape, composed of poly-
vinylidene fluoride (PVDF), with an outer diameter of 50 mm and
a total length of 1.436 m. The module contained 13 tubular mem-
brane channels, each 8 mm in diameter, which resulted in a total
membrane area of 0.42 m2 . The membrane surfaces had a mean
pore size of 30 nm.
J. Environ. Eng.
• No cleaning processes were able to recover clean water flux
and operational permeability very efficiently (with the highest
clean water flux recovery being 53%). However, all cleaning
processes were able to recover mixed-liquor flux and opera-
tional permeability effectively (with a lowest mixed-liquor flux
recovery of 67%).
• The citric acid portion of Cleaning Process 6 had a detrimental
effect on its overall foulant removal effectiveness.
• Daily CEBs enhanced the foulant removal of successive chemi-
cal cleaning processes applying the same cleaning conditions.
• Daily CEBs decreased the rate of foulant accumulation.
• Considering these results and those of Snowdon et al. (2018),
daily low-strength CEBs were observed to be an effective strat-
egy for both membrane fouling preventive maintenance and as
assistance in chemical cleaning recovery operations.
Acknowledgments
The authors would like to acknowledge and thank the following
funding agencies and industrial collaboration: the Natural Science
and Engineering Research Council (NSERC), the New Brunswick
Innovation Foundation (NBIF), and ADI Systems Inc. They would
also like to thank Jonathan Dargavel and Dr. Dennis Connor for
their help and contributions with data collection and testing
throughout the duration of the study.
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Wat. Sci. Tech. Vol. 28. No.2. pp. 165-176. 1993. 0273-1223/93 $6'00 0'00
Printed in Great Britain. All rights reserved. Copyright © 1993 IAWQ

ANAEROBIC-AEROBIC TREATMENT OF
POTATO-STARCH WASTEWATER

U. Abeling and C. F. Seyfried

Institut for Siedlungswasserwirtscha/t und Abfalltechnik (Water Supply and Treatment of

Solid Wastes). University of Hannover. Welfengarten I. D-3000 Hannover I. Germany

ABSTRACT

Production of potato starch produces wastewaters witb high concentrations of COD, nitrogen and
phosphorus. The best known and most economical solution for tbe nearly full elimination of tbese substances
is tbe two-stage anaerobic-aerobic treatment. The anaerobic pretreatment must only go so far as to maintain
enougb COD for biological nitrogen and phosphorus elimination in tbe aerobic stage. To optimize tbis
process, several tests have been carried out on nitrification/denitrification by means of tbe intermediate
product nitrite. The carbon consumption amounts to only 60% in comparison witb denitrification via nitrate.
The essential parameter for regulating tbe process is tbe concentration of free ammonia in tbe reactor.
Concentrations of I to 5mg NH31l inhibit tbe nitratation but not tbe nitritation. A separation of botb partial
steps is possible. The content of ammonia was controlled by means of continuous NH4 and pH measuring.

The process is suitable for many wastewaters witb low CODrrKN ratios and higb nitrogen concentrations. If
tbere are undesired nitrite peaks in an aerobic treatment plant caused by bigh pH values and temperatures,
specific nitrogen elimination by means of nitrite is a reliable treatment system.

KEYWORDS

Potato-starch wastewater; anaerobic-aerobic treatment; high-strength ammonium wastewater;

nitrification/denitrification via nitrite; nitritation; nitratation; industrial wastewater; nitrogen removal.

INTRODUCTION

In Europe, about 4.7 Mio. t starch and starch decay products are produced each year. The main raw materials
used are com (60% of the production) and potatoes and wheat (nearly 20% each). The largest product group
is the true starches with nearly 30%, followed by glucose (23%), isoglucose (13%) and modified starch
(12%). Most starch is employed in the food industry (for example sweets, drinks, fruit manufacturing - total
57%), the paper and paperboard industry (25%), as well as the chemical and pharmaceutical industry (10%).
Whereas a short time ago most of the attention was directed to production processes and commercializing,
nowadays wastewater avoidance and wastewater treatment are becoming more and more important. The cost
share of advanced wastewater treatment in the total production costs amounts to nearly 15%.

The starch wastewaters have high nitrogen and phosphorus concentrations. In Germany both nutrients must
be largely eliminated, and this will soon apply to the whole of the European Community as far as the
harmonization of environmental protection is concerned.

For purification of industrial wastewaters, especially for starch factories, more and more two-stage
anaerobic-aerobic processes have been used during the last few years. This is useful - for energetic reasons
- when highly concentrated wastewaters are to be treated, as a substantial part of the organic load can be

1 65
166 U. ABELING and C. F. SEYFRIED

removed anaerobically, hereby producing methane gas. Only the pollution finally remaining has to be
eliminated aerobically by using certain aeration energy.

Minimizin� the Eneuy Consumption

The combined anaerobic-aerobic technology is the most economical solution for as long as only the removal
of carbon compounds is concerned. With regard to the elimination of nitrogen and phosphorus, however, this
process is problematic, as no nitrogen and phosphorus removal worth mentioning takes place during the
elimination of the greater part of the carbon compounds in the anaerobic pretreatment. The BODIN ratio
decreased from 9:1 to nearly 1:1, the BOD:P ratio from 50:1 to 5:1. It is no problem to nitrify the
ammonium in the following aerobic treatment stage, but denitrification and biological phosphorus removal
are often incomplete, possibly due to the low content of organic carbon compounds. Phosphorus may be

eliminated by precipitation with lime or metal ions, whereas the chemicaVphysical methods for ammonium
elimination cause many problems with the resulting products. A total nitrification, however, as well as a
denitrification as far as possible and an effluent concentration of 1 or 2mg PIl, is prescribed in Germany for
most industrial wastewaters (alcohol and food production (pectin, potato, starch and sugar processing
industry, slaughter-houses etc.), pulp and paper industry, animal waste).

In order to achieve a total denitrification sometimes external carbon sources (methanol, acetic acid) are used
(very expensive). In practice, anaerobic pretreatment is often evaded by means of a bypass, but this causes a
lower gas production and also sometimes problems concerning the sludge composition (bulking) in the
aerobic stage.

Our investigations aimed to realize a process which enables total denitrification in spite of far-reaching
anaerobic pre-elimination. In contrast to the process which has been used so far, nitrification/denitrification
was carried out with assistance of the intermediate product nitrate. The carbon consumption amounts to only
60% in comparison with denitrification via nitrate. The essential parameter for regulating the process is the
concentration of free ammonia in the reactor (controlled by means of continuous NH4 and pH measuring).
Concentrations of 1 to 5mg NHyt inhibit the nitratation but not the nitritation.

The experiments were carried out in half-technical pilot plants for a period of three years, using the
wastewater of a potato starch factory. At the same time detailed examinations were made in laboratories
with regard to the kinetics and to the inhibition of nitrification/denitrification by NH3 and HN02. The new
process is available for all wastewaters with high ammonium concentrations and pH > 7.5, which often
cause problems concerning the inhibition of nitrogen removal dependent on high nitrite or ammonium
concentrations.

TREATMENT OF POTATO-STARCH WASTEWATER

Wastewater Production

During potato starch production, there are three partial wastewater streams with different concentrations of
COD, TKN and P. Figure 1 shows a flow diagram of potato starch production. The concentrations and
specific wastewater quantities are listed in Table 1.
 Potato-starch wastewater 167

t:----I:;;.;;;,;::;;;;�)_---__1 transport and

'---.--./ washing water

starch/potato - protein -coagulation )..-----l potato juice

juice seperation

S��t-----1 process water

Figure I. Flow diagram of potatO staJeh production

TABLE 1. Potato-Starch Production - Wastewater Characteristics and Specific volumes

washing water process water potato juice

(after protein-coagulation)

pH-Value 6 - 7 6 - 7 5 - 6
COD [mg/l] 2,000 - 4,000 4,000 - 8,000 50,000 - 60,000 (25,000 - 30,000)
TKN [mg/l] 150 - 30 150 - 600 3,600 - 4,400 (1,800 - 2,200)
tot. P [mg/l] 20 - 40 20 - 40 800 - 1,000 (400 - 500)

m3/t potatoes 0. 3 - 1.0 0.6 - 1.3 0.8 - 1.0

The washing water resulting from potato washing is recycled. The solid matter (earth, plant parts etc.) is
eliminated in a sedimentation tank, and any lost part of the water is substituted by fresh water continuously.
The longer the campaign lasts, COD and TKN concentration increases, because the potato quality decreases
for the reason of storage. The process water (starch washing water) contains the contamination component
fme starch, which cannot be gained. The main component of the high strength potato juice is protein. It goes
into a protein extraction, where about 50% of the protein is coagulated, separated, dried and packed for sale.
A still highly contaminated wastewater with 25-30g CODn remains.

Modern manufacturers use circular movement of the water during washing and starch extraction to reduce
the specific wastewater quantities to keep the values preferably in the low regions of the range in Table 1.
The application of an effective technique for starch extraction also reduces the concentrations. Anyway, in
the field of potato juice the technical limits are reached by reducing the concentration by 50% by means of
protein extraction. The wastewater percentage is also layed down by the water content of the potatoes and
changes only slightly. Table 2 shows the specific wastewater quantities and concentrations of a potato starch
factory which was opened in 1987 in Germany (Liichow). The treatment capacity amounts to 300 000
t1campaign (end August until mid March).
176 U. ABELINO and C. F. SEYFRIED

remaining nitrite and ammonia concentrations is required. The process is controlled by continuous pH value
and ammonium measurements.

As the pH value must be increased to 8-8.5, the process is suitable above all for wastewaters which are
located in this pH value range. On the one hand, often undesired nitrite upgradings appear which cause
considerable operation break-downs, but with a specific decoupling of nitritation from nitratation, this can
be avoided.

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Reproduced with permission of copyright
owner. Further reproduction prohibited
without permission.
 Bioresource Technology 98 (2007) 3298–3308

Modelling of biological processes during aerobic treatment of piggery

wastewater aiming at process optimisation
a,*
F. Béline , H. Boursier a, M.L. Daumer a, F. Guiziou a, E. Paul b

a
Cemagref, Environmental Management and Biological Treatment of Wastes Unit, 17 av. de Cucillé, CS 64427, F-35044 Rennes Cedex, France
b
INSA Toulouse, Laboratory of Environmental Process Engineering, 135 av. de Rangueil, F-31077 Toulouse Cedex 4, France

Available online 7 September 2006

Abstract

A dynamic mathematical model was developed for the simulation of the aerobic treatment of piggery wastewater. This model includes
the carbon oxidation, the nitrification and the denitrification. According to the experimental results obtained during this study, a modified
version of the activated sludge model No. 1 has been developed. The model includes (1) nitrite as intermediate of nitrification and deni-
trification, (2) the distinction between the anoxic heterotrophic yield and the aerobic heterotrophic yield, respectively equal to 0.53 and 0.6
and (3) the first-order hydrolysis of the slowly biodegradable fraction. The calibration and the validation of the model was performed
using experimental data from three experiments with two piggery wastewaters. A set of kinetic and stoichiometric parameters emerged
from these tests. Except the kinetic of hydrolysis of the slowly biodegradable organic matter varying from 6 to 25 g COD (g COD day)1,
all other parameters were similar for all experiments. The dissolved oxygen concentration was identified as the main variable influencing
the nitrite accumulation during nitrification. In the calibrated model, the oxygen half-saturation coefficient of the ammonium oxidisers
(0.3 g O2 m3) was lower than for the nitrite oxidisers (1.1 g O2 m3), leading to nitrite accumulation when the dissolved oxygen concen-
tration was low. Simulations with the proposed model could be very useful for improved design and management of biological treatment
of piggery wastewaters, particularly in case of partial nitrification to nitrite directly followed by denitrification.
 2006 Elsevier Ltd. All rights reserved.

Keywords: Piggery wastewater; Modelling; Nitrification; Denitrification; Carbon oxidation; AMA

1. Introduction batch reactor without decantation phase (modified SBR)

The biological nitrogen removal by nitrification and
denitrification generally provides the most economical
means of controlling nitrogen in wastewater effluents. Con-
sequently, the biological nitrogen removal by nitrification
and denitrification is becoming increasingly common for
the treatment of piggery wastewaters in France (Béline
et al., 2004). About 300 treatment units are in operation
in France. The treatment unit is generally composed of
a mechanical separation of the wastewater (press-auger,
decanter centrifuge, . . .) followed by the biological treat-
ment of the liquid fraction resulting from the separation.
The biological treatment system is a modified sequential
*
Corresponding author. Tel.: +33 2 23 48 21 21; fax: +33 2 23 48 21 15.
E-mail address: fabrice.beline@cemagref.fr (F. Béline).
in which the anoxic and aerobic phases alternate. The
non-biodegradable suspended solids content of the piggery
wastewaters is high, leading to a difficult decantation.
Thus, no decantation was applied in the reactors and the
hydraulic residence time is equal to the solids residence
time and ranges between 35 and 50 days. Few scientific
data related to the piggery wastewater biodegradability
(Boursier et al., 2005) and to the biological degradation
processes are available in the literature. Consequently,
the optimization of the cost of treatment, while respecting
nitrogen removal efficiency, is difficult. Moreover, due
to the complexity of the processes and the temporal
fluctuations of the piggery wastewater concentrations
(Béline et al., 2004), the heuristic optimization is rarely effi-
cient and a model-based approach would be very useful
(Coelho et al., 2000). In fact, once calibrated to a particular

0960-8524/$ - see front matter  2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biortech.2006.07.004
 F. Béline et al. / Bioresource Technology 98 (2007) 3298–3308 3299

Nomenclature

SNH NHþ 4 þ NH3 nitrogen (g N m )

3
SS readily biodegradable organic matter (g O2 m3)
SND soluble biodegradable organic nitrogen XS slowly biodegradable organic matter (g O2 m3)
(g N m3) SI soluble inert organic matter (g O2 m3)
XND particulate biodegradable organic nitrogen XI particulate inert organic matter (g O2 m3)
(g N m3) XBH active heterotrophic biomass (g O2 m3)
XNI particulate inert organic nitrogen (g N m3) XBAI active NHþ 3
4 oxidisers biomass (g O2 m )
SNOI NO 3
2 nitrogen (g N m ) XBAA 
active NO2 oxidisers biomass (g O2 m ) 3

SNOA NO3 nitrogen (g N m3) XP particulate inert organic matter from biomass
SO oxygen (g O2 m3) decay (g O2 m3)

wastewater, a model allows to quickly screen many poten- chemical oxygen demand (COD) hydrolysis could signifi-
tial design and management alternatives. cantly affect the denitrification.
For the evaluation and the optimization of the treat- The objective of this work was to develop and to cali-
ment of urban wastewaters, various models have been brate a mathematical model for the simulation of the mod-
developed and edited by the IWA task group (Henze ified SBR, treating piggery wastewaters. First, an analysis
et al., 1987), such as the activated sludge models (ASM). of the processes involved in nitrogen removal was carried
These models are largely used for domestic sewage but out based on the experimental results. Then, a mathemati-
the modelling is overlooked in the treatment of livestock cal model was built and calibrated using the experimental
wastes and industrial effluents (Orhon, 1998). The available data.
activated sludge models were specifically designed and cal-
ibrated for urban wastewater treatment, and therefore, the 2. Methods
extension of such models to more concentrated influents
such as piggery wastewaters, appears particularly interest- 2.1. Description of the pilot-scale reactor
ing but requires specific experiments and research.
In contrast to the domestic sewage, a very limited A pilot-scale modified SBR was built for the experimen-
amount of data on the kinetic and stoichiometric processes tal study of the treatment of piggery wastewaters. A simpli-
and on the influent fractionation are available for piggery fied scheme of this pilot plant is shown in Fig. 1. The
wastewaters (Andreottola et al., 1997). The ASM models modified SBR consists of a succession of cycles, during
describe the processes of nitrification and denitrification which the aerobic and anoxic phases alternate. Before the
as one-step processes. However, nitrogen removal for con- biological treatment in the reactor, the piggery wastewaters
centrated wastewaters, as the piggery wastewaters, might were stored at 4 C. At the beginning of each cycle, a
result in the inhibition of nitrification by free ammonia
and nitrous acid (Anthonisen et al., 1976), and nitrification
might be limited by the dissolved oxygen (DO) concentra-
tion (Wiesmann, 1994). Therefore, the simplified assump-
tion, used in the ASM models, is no longer applicable
for the description of nitrogen removal processes in this
case. In fact, the free ammonia inhibition and/or the
nitrous acid inhibition and/or the dissolved oxygen limita-
tion frequently lead to nitrite accumulation. High temper-
atures can also lead to nitrite accumulation (Hellinga
et al., 1998). Consequently, more sophisticated model
assumptions are required for an adequate description of
the system efficiency. In this case, each process must
be described as a two-step process including nitrite as
intermediate (Andreottola et al., 1997). Moreover, some
authors studied and compared the heterotrophic yields
under aerobic and anoxic conditions (Gujer et al., 1999;
Orhon et al., 1996; Boursier et al., 2004). The observed
lower anoxic heterotrophic yield leads to a lower COD to Fig. 1. Scheme of the pilot, treating piggery wastewaters: (1) storage tank
(500 l), (2) buffer tank and weighing system, (3) reactor (100–110 l), (4)
NO 3  N ratio for the denitrification. That is more partic- foam breaker, (5) mixing system, (6) fine bubbles diffuser, (7) pH, ORP,
ularly important for the wastewaters with high N concen- DO and temperature sensors, (8) system for water addition, (9) gas flow
tration where the kinetics and the stoichiometry of the meter and (10) withdrawal and weighing system.
3300 F. Béline et al. / Bioresource Technology 98 (2007) 3298–3308

known amount of piggery wastewater was added in the the reactor reached steady-state conditions (after more
reactor through a buffer tank where the quantity added than three hydraulic residence times), the characterisation
was weighed and recorded. The reactor was equipped with of the effluent was done (COD, soluble COD and total
a foam breaker working during the aerobic phases and a nitrogen) and was followed by a study of the evolution
fine bubbles diffuser fed with a compressor (2–5 m3 h1). of NHþ  
4 , NO2 and NO3 in the reactor, during one
For the mixing, a centrifugal pump (30 m3 h1) circulated cycle.
the activated sludge, during the anoxic phases from the Immediately after run 1, a second study of the evolution
 
bottom to the top of the reactor. Water was continuously of NHþ 4 , NO2 and NO3 , during one cycle, was performed
added in the reactor (65 l per day) to compensate for the (run 2). At the beginning of this cycle, 1 l of ammonium
evaporation caused by the high temperature and the aera- carbonate solution (13.5 kg N m3) was added in the reac-
tion. At the end of each cycle, an amount of the activated tor during the feeding phase, together with the piggery
sludge equal to the piggery wastewater added at the begin- wastewater (PW1). For this experiment, the other experi-
ning of the cycle was withdrawn from the reactor. The bio- mental conditions were similar to run 1.
logical reactor was equipped with on-line measurements of For run 3, as for run 1, the reactor was initially filled
DO (WTW Oxi197 oxygen meter), temperature (Ponselle with 50 l of activated sludge coming from the same farm
PONAPF-TTRANS), oxidation–reduction potential (Pon- and 50 l of tap water. About 600 l of raw piggery waste-
selle PONAPF-EHTRANS) and pH (Ponselle PONAPF- water was collected in an experimental farm near Rennes
PHTRANS) allowing measurements at 10 min. intervals. (France) and was mechanically sieved (1 mm) using a
The system operated without sludge recirculation nor rotary screen. The liquid fraction called piggery wastewater
decantation in the reactor, leading to a solids retention 2 (PW2) was stored at 4 C and was used for run 3. For this
time equal to the hydraulic retention time. For each exper- run, the duration of a cycle was equal to 12 h, consisting of
iment, each whole-cycle of the modified SBR was scheduled 7 h of anoxic conditions and 5 h of aerobic conditions. At
as follows: the beginning of each cycle, 4.4 l of PW2 was added in the
reactor, leading to a working volume of 104.4 l and a HRT
• a feeding phase, equal to 11.9 days. At the end of each cycle, the same
• an anoxic phase, amount of activated sludge was withdrawn. A characterisa-
• an aerobic phase, tion of the effluent (COD, soluble COD and total nitrogen)
 
• a withdrawal phase. and a study of the evolution of NHþ 4 , NO2 and NO3 dur-
ing a cycle, were performed when more than 3 hydraulic
residence times had passed.
2.2. Experimental The main characteristics of each piggery wastewater
used in this study are presented in Table 2.
During this study, three experiments were carried out
using the pilot-scale modified SBR (Table 1).
Table 2
For run 1, the reactor was filled with 50 l of activated Characteristics of the piggery wastewaters
sludge coming from a farm equipped with a modified
Variable PW1 PW2
SBR at the beginning of the experiment. The reactor
3
was supplemented with 50 l of tap water. At the same TS, kg m 54.0 (0.4) 31.1 (–)
VS, kg m3 42.5 (1.0) 20.1 (–)
time, about 600 l of raw piggery wastewaters were col-
COD, kg O2 m3 50.6 (0.3) 39.4 (1.0)
lected and were manually sieved (5 mm mesh). The liquid CODs, kg O2 m3 21.8 (0.1) 14.8 (0.4)
fraction called piggery wastewater 1 (PW1) was stored VFA, kg O2 m3 10.7 (0.2) 6.2 (–)
3
at 4 C and was used for this experiment. For this run, NHþ 4  N (or SNH), kg N m 3.0 (0.1) 3.4 (0.1)

the duration of a whole-cycle was equal to 24 h consisting NO2  N (or SNOI), kg N m3 0 0
NO 3  N (or SNOA), kg N m
3
0 0
of 4 h of anoxic conditions and 20 h of aerobic conditions.
TN–N, kg N m3 4.6 (0.1) 4.3 (0.05)
At the beginning of each cycle, 10 l of PW1 were added SS, kg O2 m3 5.2 (0.5) 6.0 (1.0)
in the reactor, leading to a working volume of 110 l and XS, kg O2 m3 14.1 (3.6) 23.9 (1.4)
a HRT equal to 11 days. At the end of each cycle the Inert COD, kg O2 m3 31.3 (3.4) 9.5 (1.4)
same amount of activated sludge was withdrawn. When Standard errors shown in parenthesis, n = 5.

Table 1
Summary of the conditions during the three experiments carried out with the pilot-scale modified SBR
Runs PW HRT (days) P1 (h) P2 (h) P3 (h) P4 (h) Observations
1 1 11.0 0.1 3.9 19.9 0.1 Effluent characterisation and study of a cycle
2 1 11.0 0.1 3.9 19.9 0.1 Study of a cycle (ammonium carbonate was added)
3 2 11.9 0.1 6.9 4.9 0.1 Effluent characterisation and study of a cycle
PW: piggery wastewater, P1: feeding phase, P2: anoxic phase, P3: aerobic phase, P4: withdrawal phase.
 F. Béline et al. / Bioresource Technology 98 (2007) 3298–3308
2.3. Analytical methods
Total solids (TS), volatile solids (VS), COD and total
nitrogen (TN) were analysed according to standard
methods (APHA, 1992). The soluble COD (CODs) was
analysed after centrifugation at 4000 rpm during 15 min.
Volatile fatty acids (VFA) were analysed using HPLC
(Peu et al., 2004). NHþ
4 was analysed by steam distillation
(Bremner and Keeney, 1965) directly on the effluent
(NHþ 4TOT ) and on the liquid fraction after centrifugation
 
at 4000 rpm during 15 min (NHþ 4SOL ). NO2 and NO3 were
analysed by ion chromatography on a Dionex DX120
system equipped with a Dionex AS9HC column. Eluant
was a 10 mM Na2CO3 solution, flowing at 1 ml min1.
Respirometry, widely recognised as the most convenient
tool to determine the biodegradable wastewater fractions
(Sollfrank and Gujer, 1991), was used for the COD frac-
tionation during this study. The oxygen uptake rates
(OUR) were measured for each wastewater and allowed
to determine the readily biodegradable COD (SS) and the
slowly biodegradable COD (XS) as described by Orhon
and Okutman (2003); Boursier et al. (2005). The inert
COD fraction was calculated as the difference between
total COD and biodegradable COD (SS + XS).
2.4. Modelling
For the modelling, the mathematical equations were
implemented in the Scilab software using the Scicos
interface. This software is available as a toolbox called
AS-Model1.0 (see Web references). The integration routine
was chosen automatically by the software. A run time of
more than three times the HRT was used to establish the
pseudosteady-state conditions. For the calibration of the
model, the parameters were estimated manually by com-
paring the simulated output with the experimental data
until the best fit was achieved.
3. Results and discussion
3.1. Experimental results
The evolution of the nitrogen species during a cycle was
used for a better characterisation of processes involved in
the nitrogen transformations. As an example, the evolution
of the nitrogen forms during run 1 is presented in Fig. 2.
At the beginning of the cycle, the addition of piggery
wastewater in the reactor led to an increase of NHþ4TOT from
163 to 465 mg N l1 and an increase of NHþ 4SOL from 0 to
170 mg N l1. After the addition of piggery wastewater,
both NHþ þ
4TOT and NH4SOL concentrations were quite stable
during the anoxic phase. During the aerobic phase, both
concentrations decreased simultaneously, probably due
to the nitrification process. At the beginning of the cycle,
the quantity of NHþ þ
4 found as soluble (18 gNH4SOL  N)
in comparison with the added quantity as soluble
(30 gNHþ 4SOL  N) showed that a part was probably
3301
Fig. 2. Nitrogen species concentrations during the run 1 cycle (F: feeding,
W: withdrawal).
adsorbed to the activated sludge flocs, as previously
observed by Nielsen (1996). However, NHþ 4 was available
almost entirely for nitrification and the adsorption did not
significantly limit the nitrification process. Therefore, the
process of adsorption of NHþ 4 on the flocs was neglected.
In the remainder of this paper, the nitrifiable ammonium
(NHþ þ þ
4NIT ), rather than NH4SOL or NH4TOT , was considered.
þ
NH4TOT found at the end of the nitrification was considered
as the NHþ þ
4 not available for the nitrification (NH4NO–AV ).
NH4NIT was calculated as the difference between NHþ
þ
4TOT
and NHþ 4NO–AV (Nielsen, 1996). For all runs, the NH4NIT
þ
corresponded to the amount added at the beginning of
each cycle. The NHþ 4NO–AV was probably organic nitrogen
considered as NHþ 4 because of an analytical error (steam
distillation).
As shown in Fig. 2, the NO 3 concentration decreased
quickly from 210 to 0 mg N l1 during the anoxic phase.
1
Concurrently, an accumulation of NO 2 up to 115 mg N l
occured. During the aerobic phase, an increase of NO 3
from 0 to 220 mg N l1 was obtained and an accumulation
1
of NO 2 up to 110 mg N l was also observed. The same
evolution of nitrogen, particularly the accumulation of
NO 2 during the nitrification and the denitrification, was
observed for all runs and was previously described by
several authors (Andreottola et al., 1997; Kim et al.,
2004; Huang and Hao, 1996).
Concerning the denitrification process, various environ-
mental factors were found to be responsible for nitrite
accumulation: the type and quantity of organic substrate,
oxygen, pH, nitrate availability, and temperature (Wilderer
et al., 1987; Oh and Silverstein, 1999).
During the nitrification process, a partial inhibition of
the NO 2 oxidisers by the free ammonia or by the nitrous
acid (Andreottola et al., 1997; Abeling and Seyfried,
1992) could induce the observed accumulation of NO 2.
During our experiments, and more generally during the
treatment of piggery wastewaters, the pH (higher than
7.5–8) led to nitrous acid concentrations lower than the
3306 F. Béline et al. / Bioresource Technology 98 (2007) 3298–3308

A.2. Process stoichiometry for organic matter oxidation, nitrification and denitrification

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15
SI SS XI XS XBHI XBAI XBAA XP SO SNOI SNOA SNH SND XND XNI
1 ð1Y H Þ
q1 YH 1 YH  iBN

1 1Y HD
q2 Y HD 1  1:71Y HD
 iBN

1 1Y HD 1Y HD
q3 Y HD 1  1:14Y HD
 1:14Y HD
iBN

q4 1  3:43Y
Y AI
AI 1
Y AI iBN  Y1AI

q5 1  1:14Y
Y AA
AA
 Y 1AA 1
Y AA iBN
q6 1  fP 1 fP iBN  fP fP Æ iBN
Æ iBN
q7 1  fP 1 fP iBN  fP fP Æ iBN
Æ iBN
q8 1  fP 1 fP iBN  fP fP Æ iBN
Æ iBN
q9 1 1
q10 1 1
q11 1 1

A.3. Default values at 20 C for the model and parameters used for simulating run 1, 2 and 3 (-: default value was used)

Symbol Definition Default Run 1 Run 2 Run 3 Ref.

value
YH Aerobic yield heterotrophic 0.6 – – – Boursier et al. (2004)
biomass (g COD g COD1)
YHD Anoxic yield heterotrophic 0.53 – – – Boursier et al. (2004)
biomass (g COD g COD1)
lH Maximum specific growth rate for 6 – – – Henze et al. (2000)
heterotrophic biomass (day1)
bH Decay coefficient for heterotrophic 0.62 – – – Henze et al. (2000)
biomass (day1)
KS SS half-saturation coefficient for 20 – – – Henze et al. (2000)
heterotrophic biomass (g COD m3)
KOH SO half-saturation coefficient for XBH 0.2 0.05 0.05 0.05 Henze et al. (2000)
(g COD m3)
KNH SNH half-saturation coefficient 0.05 – – – Henze et al. (2000)
for biomass (g N m3)
KNOI SNOI half-saturation coefficient for XBH 0.5 – – – Henze et al. (2000)
under anoxic conditions (g N m3)
KNOA SNOA half-saturation coefficient for 0.5 – – – Henze et al. (2000)
under anoxic conditions (g N m3)
gG Correction factor for lH under anoxic 0.8 – – – Henze et al. (2000)
condition (dimensionless)
gH Correction factor for hydrolysis under 0.4 – – – Henze et al. (2000)
anoxic condition (dimensionless)
KH Maximum specific hydrolysis rate 3 25 25 6 Boursier et al. (2004)
(g COD (g COD day)1)
KA Ammonification rate 0.08 – – – Henze et al. (2000)
(m3 COD (g day)1)
(continued on next page)
 F. Béline et al. / Bioresource Technology 98 (2007) 3298–3308 3307

Appendix (continued)
Symbol Definition Default Run 1 Run 2 Run 3 Ref.
value
fp Fraction of biomass leading to inert 0.08 – – – Henze et al. (2000)
particulate products (dimensionless)
iBN Mass of nitrogen per mass of 0.086 – – – Henze et al. (2000)
COD (g N g COD1)
YAI Yield for NHþ 4 oxidisers autotrophic 0.15 – – – Hao et al. (2002b);
biomass (g COD g N1) Hao et al. (2002a)
lAI Maximum specific growth rate for NHþ 4 0.8 – – – Hao et al. (2002b);
oxidisers autotrophic biomass (day1) Hao et al. (2002a)
bAI Decay coefficient for XBAI autotrophic 0.05 – – – Hao et al. (2002b);
biomass (day1) Hao et al. (2002a)
KOAI SO half-saturation coefficient for XBAI 0.6 0.3 0.3 0.3 Hao et al. (2002b);
biomass (g COD m3) Hao et al. (2002a)
KNAI SNH half-saturation coefficient for XBAI 2.4 5 5 5 Hao et al. (2002b);
biomass (g N m3) Hao et al. (2002a)
YAA Yield for NO 2 oxidisers autotrophic 0.041 – – – Hao et al. (2002b);
biomass (g COD g N1) Hao et al. (2002a)
lAA Maximum specific growth rate for NO 2 0.79 – – – Hao et al. (2002b);
oxidisers autotrophic biomass (day1) Hao et al. (2002a)
bAA Decay coefficient for XBAA autotrophic 0.033 – – – Hao et al. (2002b);
biomass (day1) Hao et al. (2002a)
KOAA SO half-saturation coefficient for XBAA 2.2 1.1 1.1 1.1 Hao et al. (2002b);
biomass (g COD m3) Hao et al. (2002a)
KNAA SNOI half-saturation coefficient for XBAA 5 2.5 2.5 2.5 Hao et al. (2002b);
biomass (g N m3) Hao et al. (2002a)

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