DESAHNATION

ELSEVIER Desalination 177 (2005) 15%165

www.elsevier.corn/locate/desal

Treatment of olive mill wastewater

using an anaerobic sequencing batch reactor
Bashaar Y. Ammary
Water and Environmental Engineering Department, Balqa Applied University, Huson College,
P.O. Box 50, Huson 21510, Jordan
Tel. +962 (2) 7010400; Fax +962 (2) 7010397; e-mail: bammary@yahoo.com

Received 8 December 2003; accepted 3 December 2004

Abstract
Wastewater from olive mills in Jordan has been characterized and treated using a lab scale anaerobic
sequencing batch reactor (ASBR). It was found that this wastewater has an average COD:N:P ratio of about
900:5:1.7. At this ratio, the wastewater was found to have sufficient nutrients that it was not necessary to add
nutrients or combine it with other wastewaters. For effective treatment it was necessary to reduce the strength of
the wastewater with an average COD value of about 97 g/L, to about 16 g/L by keeping part of the treated
wastewater in the reactor when a new batch of wastewater was added. This achieved more than 80% COD re-
moval at 3 d hydraulic retention time and at an organic load of about 5.3 kg COD/m3/d provided that alkalinity
was added to adjust the pH to near 7. The specific substrate utilization rate, and observed biomass yield were
about 0.37 kg COD removed/kg VSS/d, and 0.06 kg VSS/kg of COD degraded, respectively.

Keywords: Anaerobic treatment; Sequencing batch reactor; Olive mill wastewater characterization; Biomass
yield; Nutrient requirement

1. Introduction to a solid waste disposal site handling liquid

Olive oil production in Jordan is considered
a major source o f income to a large number o f
families, especially in rural areas. It is prohibited
to discharge olive mills wastewater (OMW) in-
to the sewer system. In addition, a large number
o f these mills are located in areas with no close
sewer system. Currently olive mills dispose o f
their wastewater either in cesspools or haul them
waste. Onsite treatment o f O M W is essential and
more cost effective than building large central
treatment plants treating OMW, as treatment
plants are scattered all around the country.
Onsite treatment should be low in capital
and operating cost to keep the cost o f oil pro-
duction as low as possible. At the present time,
the cost o f olive picking is about 2 5 - 3 5 % o f the
oil price. In addition, the cost of milling is about

0011-9164/05/$- See from matter © 2005 Elsevier B.V. All fights reserved
doi:10.1016/j.desal.2004.12.006
158 B. Y. Ammary /Desalination 177 (2005) 157-165
one ninth of the oil price. This, in addition to
other costs, especially irrigation costs, makes it
vital that any OMW treatment cost be as low as
possible to prevent the olive-growing industry
from collapsing. Several anaerobic treatment
systems have been suggested and used for
OMW. Anaerobic treatment of OMW has a
number of advantages over aerobic treatment.
These include no aeration requirements, lower
sludge production, lower nutrient requirements,
the production of methane gas, and the quick
recovery of anaerobic systems that have been
dormant for a long time [1]. The last point is
particularly important, as the treatment unit will
be without wastewater for about 8-9 months
(from January to October).
The anaerobic treatment systems that have
been used for OMW require either high dilution
with tap water [2,3], or combined treatment with
other wastewaters, such as piggery wastes [4,5].
Others suggest the use of pretreatment systems
before anaerobic treatment [6-9] and two-stage
anaerobic treatment [10]. These systems use
either up-flow anaerobic sludge blanket
(UASB) or fixed bed bioreactors. These kinds of
systems are unsuitable for Jordanian olive mills
due to their high capital and operating costs, in
addition to high maintenance costs and the need
for skilled operators.
The anaerobic sequencing batch reactor
(ASBR) has been used successfully for the
treatment of high strength wastewaters includ-
ing slaughterhouse wastewater [11,12], non-fat
dry milk [13], landfill leachate [14], and swine
manure slurry [15,16]. ASBR has the advantage
of having only one reactor for both anaerobic
decomposition and settling. Moreover, there is
little sophistication in the process so that high
skilled operators are not necessary as in other
anaerobic reactors. The process consists of five
phases. After the filling-phase, the reactor con-
tents are mixed giving them the same reaction
time in the react-phase. Mixing is terminated at
the end of the react-phase, where settle-phase
begins. In the settle-phase, the contents may
either have a quiescent settling or flotation.
During the draw-phase, the supematant is dis-
charged out of the reactor while the sludge is
kept in the reactor waiting for another batch of
wastewater (idle-phase). At the start of the react-
phase, the food to microorganisms (F/M) ratio
is at its highest, and therefore BOD conversion
is high. As conversion proceeds, F/M is reduced
and reaches its lowest value at the end of the
react-phase, before the settle-phase. This low
F/M ratio reduces biogas production, and bio-
mass flocculation and settling behaviors are im-
proved [17].
This study is intended to evaluate the
characteristics of OMW in Jordan, and to inves-
tigate whether ASBR treatment is an appro-
priate method for onsite treatment. Variables af-
fecting the performance of the ASBR are also
investigated.
2. Materials and methods
2.1. Anaerobic reactor
The anaerobic sequencing batch reactor used
in this study was a glass bottle that had an
active volume of 2 L. It was mixed and kept at
30 + 2°C using a ma~etic stirrer/hotplate. The
reactor was covered completely to allow for
anaerobic conditions, except for a tube extend-
ing into the headspace of the reactor to allow
for the emitted gases to exit from the reactor.
The other end of the tube was submerged into a
container of water to prevent any possibility of
oxygen reaching the reactor.
2.2. Start-up and reactor operation
During the startup phase of the reactor, a
small volume of the olive mill wastewater was
mixed with domestic wastewater and seeded
with sludge from an anaerobic sludge digester.
The initial COD value was about 2,000 mg/L.
This was achieved by combining 20 ml of
OMW, 500 ml of anaerobic sludge, and
1,480 ml of domestic wastewater with a COD
value of around 1,200 mg/L. No additional
wastewater was added during the first week.
OMW was then added and the COD concen-
 B. Y. Ammary / Desalination 177 (2005) 157-165
tration was increased first to around 4,000 mg/L.
It was then doubled to around 8,000, 16,000
and finally to 32,000 mg/L in about two
months. No removal of sludge was conducted
during this period. The COD concentration was
doubled when the con-centration of volatile
fatty acids reached a value less than 300 mg/L
[18]. pH of the reactor was adjusted to around
7, a level that is necessary for effective
fornlation of methane gas, using sodimn
bicarbonate.
When steady state conditions prevailed, the
initial concentration of COD in the reactor was
controlled. Mixing and heating continued for
the specified hydraulic retention time (HRT)
(react-phase). In the present study, the fill, draw,
and idle-phases were negligible. At the end of
the react-phase, about 3 h before turning offthe
mixing, a sample was taken from the reactor for
the measurement of the volatile suspended
solids (VSS) concentration. If the concentration
of the VSS exceeded 13,000 mg/L, part of the
reactor contents were removed at the end of the
nfixing period to lower the VSS concentration
in the next reaction phase to about 11,000 mg/L.
Mixing and heating were then turned off, and
the reactor was kept quiescent for 2 h to allow
for the anaerobic sludge to settle. At the end of
the settling period, a sample from the super-
natant was taken and the COD and some other
parameters were measured. At the sanae time
the COD value of a raw OMW sample was
measured. Depending on these two values of
COD, and the required initial COD in the re-
actor in the next reaction phase, a volume of the
supernatant was replaced by raw OMW. Any
volume taken fi'om the reactor for the control of
VSS was taken into consideration in the calcul-
ation of the replaced volume. The next reaction
phase started by turning on the mixing and
heating. The same procedures conducted for the
previous reaction phase were conducted for all
the next phases till the end of the study. During
the settling period, the reactor temperature drop-
ped and that may have improved the settling
efficiency by stopping or reducing gas pro-
159
duction during the settling period. Sludge
volmne index (SVI) was measured occasionally
to check the settlability of the sludge. No attempt
was made to measure the volume or the content
of emitted gas.
2.3. Analytical methods
All the tests were conducted according to
standard methods [19]. COD was measured
using method 5220 C (closed reflux, titrimetric
method). The macro-kjeldahl method (method
4500-Norg B) was used to measure the total
kjeldahl nitrogen (TKN) concentration. Phos-
phorous concentration was measured after di-
gestion using the vanadomolylgdophosphoric
acid colorimetrie method (method 4500-P C).
The concentration of the fat, oil, and grease
(FOG) was measured using method 5520 B
(partition-gravimetric method), while total phe-
nol concentratkm was measured using the direct
photometric method (method 5530 D). Volatile
fatty acids concentrations were determined
using method 5560 C (distillation method), All
other tests were also conducted according to
standard methods [ 19].
2.4. Substrate
Table 1 shows the range and average value
of a number of wastewater characteristics taken
from a three-phase extraction mill in the Irbid
area (northern Jordan).
3. R e s u l t s a n d d i s c u s s i o n
3.1. O M W characteristics
Wastewater from olive mills has a wide
range of characteristics depending on the type
of the mill and the type of olive and equipment
employed. Most of the olive mills in Jordan use
a three-phase extraction process. However, some
of the newer ones use the two-phase extraction
process. Manual mills are still present but to a
limited extent. Table 1 shows that the COD
value is very high and therefore anaerobic treat-
ment is necessary for such wastewater. The TKN
160 B. Y. Ammary / Desalination 177 (2005) 157-165
Table 1
Average OMW characteristics during the study period
Parameter Average concentration/value
BOD5, mg/L 30,600
COD, mg/L 97,000
pH 5.72
Total kjeldahl nitrogen, mg/L as N 532
Total-P, mg/L as P 182
TDS, mg/L 27,300
TSS, mg/L 26,000
FOG, mg/L 8,100
Total phenol, mg/L 3,600
Alkalinity, mg/L as CaCO3 2,800
concentration in Table 1 is essentially equal to
the total nitrogen concentration as the concen-
trations of nitrate and nitrite were found to be
negligible. Therefore TKN will be referred to as
nitrogen concentration in the present study. The
average ratios of COD to nitrogen (COD:N)
and phosphorous concentrations (COD:P) are
equal to about 180 and 530, respectively. The
COD:N:P ratio then equals 911:5:1.7. The
maximum ratio that is usually reported in the
literature as the required ratio is 250:5:1-500: 5:1
depending on the extent of loading or COD in-
fluent concentrations [1,20]. The present ratio
suggests that the concentrations of nitrogen and
phosphorous are lower than what is required for
anaerobic treatment of such wastewater. There-
fore, nutrients, especially nitrogen, have to be
added to the OMW. The table also shows the
high concentrations of total dissolved solids
(TDS), total suspended solids (TSS), FOG, and
phenols. The high TDS of the raw OMW makes
it unsuitable for use in irrigation. A number of
farmers in rural areas in Jordan, occasionally,
use raw OMW for irrigation due to what they
think is its high fertilizing value. The high TSS
can affect the efficiency of treatment of the
OMW. If the TSS are not broken down in the
anaerobic reactor, they can displace biomass
and reduce the removal efficiency. The high
phenol and FOG concentrations could also
Range
17,200-38,700
55,000-10,8000
5.15-5.93
395-714
118-243
11,400-33,400
7,600-42,000
4,200-12,600
2,200-5,300
1,100-4,200
affect the treatability of the wastewater. The
alkalinity of the wastewater is high, but may not
be enough for the very high COD of the waste-
water.
As shown in Table 1, the pH of the waste-
water was in the acidic range and therefore
adjustment of the pH to around 7 was neces-
sary. As the reaction progressed and the form-
ation of fatty acids took place, the pH of the
reactor dropped and the addition of sodium bi-
carbonate was necessary. The pH in the reactor
was never allowed to drop below 6.5. The
maximum pH that was reached after the
addition of sodium bicarbonate was 7.7.
3.2. Start-up
As mentioned earlier, the experiments started
by using a small volume of olive mill waste-
water mixed with domestic wastewater and
seeded with sludge from an anaerobic domestic
sludge digester. The amount of olive mill waste-
water was increased until the COD of the waste-
water reached about 32,000 mg/L. At this
concentration, the amount of fatty acid con-
centration increased dramatically (about
1,300 mg/L) so it was concluded that the
reactor was overloaded. From this point on, the
COD in the ASBR was kept around
16,000 mg/L. At this value of COD, the reactor
performed at a high level of efficiency as was
 B.Y. Ammary / Desalination 177 (2005) 157-165 161

noticed from the low and stable concentration
of fatty acids (between 50-90 rag/L), and the
high removal of COD (about 80% at 3 d HRT).
3.3. COD conversion
The second part of the experiments were
conducted at COD values of about 16,000 mg/L
and with a hydraulic retention time of 3 d. The
average VSS in the reactor was kept around
12,000 mg/L. Sludge wastage was conducted
whenever the VSS exceeded 13,000 mg/L,
about every 6-9 d. The average sludge age at
these conditions would be around 45 d. Fig. 1
shows the irffluent and effluent COD concen-
tration and the removal efficiency when steady
state conditions prevailed for 3 d HRT. The
influent (or initial) COD to the reactor was
calculated based upon the mixing proportions
of measured raw OMW and the effluent COD
concentration in the reactor (see below). In a
few cases (places where the COD is different
than exactly 16 g/L in Fig. 1) the influent COD
was measured as a quality control step. The
COD removal efficiency averaged a value of
about 83%, with an average effluent COD
concen-tration of about 2,700 mg/L. This was
achieved without the need for nutrients
addition. At these conditions, the observed
yield was found to be around 0.06 kg VSS/kg
COD removed. The specific substrate
utilization rate then would be
equal to about 0.37 kg COD removed/kg VSS/d.
In order to keep the operation more economical,
the dilution water used in this part of the experi-
ments was the effluent from the reactor. Thus the
mills will not have to bring domestic waste-
water from distant locations to the ASBR, or
dilute it with tap water, both of which are very
costly. This was achieved by keeping part of the
effluent of the reactor in the reactor, and only
replacing the disposed part by raw wastewater.
This would, of course, increase the volume
of reactor necessary to treat a certain amount of
OMW. This, however, increases the average
HRT for the raw OMW, which may increase
the removal efficiency of the pollutants. This is
particularly important for the high concentra-
tion of suspended solids present in the OMW.
It should be noted that the 3 d HRT men-
tioned above is the actual time for the diluted
COD (16,000 mg/L). The hydraulic retention
time for raw OMW would be the product of the
3 d multiplied by the dilution factor. The dilu-
tion factor in the present study depended mainly
on the raw OMW strength (see Fig. 2). For high
raw OMW COD values, the volume added was
lower than when the raw OMW COD was low
to get the COD of the diluted OMW to about
16,000 mg/L. The dilution factor also depended
on the effluent COD of the previous cycle of
treatment. Fig. 2 shows the COD concentrations
120 m. 400

100
g
16 100 : : ='¶ i .350 "o

14 80 o~ 8O , . . , ,, / '~,- 300
12
10 ......... Influent COD 60 o 60 0
O3 E GI
Effluent COD O • :: it "i ~.." i 250
8
40 O 40 "6
O 6 - - - Percent removal = R a w O M W COD 200
O o ---*,-- Effluent COD
4 20
20 - • - . - Volume of raw OMW added i 50
13. >

i t i l =--k.~--=,-~_, ~ -_ ~_... ,¢ ,L ~-~'-~,~,..t~-,~--~ t, .~ ~-..~. , 100

0
0 5 10 15 20 25
0 5 10 15 20 25
Cycle number
Cycle n u m b e r

Fig. 2. Reactor effluent and raw OMW COD values

Fig. 1. Influent and effluent COD and percentage COD and the corresponding volume of raw OMW added to
removal in the ASBR for 3 d HRT, cycle length. the reactor to achieve an initial COD of 16 g/L.
162 B. Y. Ammary /Desalination 177 (2005) 15 7-165
of the raw OMW and the reactor effluent, along 3.4. Removal o f phenol, FOG, and TSS
with the volume of raw OMW added to each
Phenol and FOG are usually responsible for
cycle to get the influent COD concentration to a
the inhibiting action of OMW. Therefore dilu-
value of 16,000 mg/L. In the present study, the
tion in this study was necessary to reduce the
raw OMW volume that was added to the reactor
concentrations of these compounds to a level
every 3 d was between 234 ml and 400 ml de-
that is not inhibiting. FOG removal efficiency
pending on the COD of raw OMW and the
was higher than TSS and phenol removal effi-
COD of the effluent from the reactor. The dilu-
ciencies, and reached a value of 99%. Removal
tion factor for these two cases, which is equal to
of high TSS concentrations in anaerobic treat-
the volume of the reactor (2000 ml) divided by
ment is usually considered a problem. It is usu-
the volume of raw OMW added, would be equal
ally reported that the ratio of TSS to COD in
to 8.5 and 5.0 respectively. For an average
the influent should have a maximum value of
dilution factor value of about 7, the average
10-20% for effective anaerobic treatment [20].
HRT for raw OMW would be around 21 d.
In the present study, the average TSS/ COD
Similarly, the efficiency of the ASBR is the
ratio in the influent is more than 25%. The
actual efficiency taking into account that the
removal efficiency of TSS at 3 d HRT was high
influent COD used in the calculation of effi-
in the present study (91%) due to the fact that
ciency is the diluted COD. The efficiency would
the suspended solids were kept at an average of
be much higher if the undiluted COD
around 21 d in the reactor. This period is
(97,000 rag/L) is used in the calculation of effi-
sufficient to break down these suspended solids.
ciency.
SVI values of generally less than 30 ml/g indi-
During a number of experiments with the 3
cated good settling behavior of the solids.
d HRT, samples after 0.5, 1, and 2 d were taken
Average removal efflciencies of suspended
from the reactor and analyzed for COD. The
solids are shown in Table 3. The table also
results shown in Table 2 are average values of
shows the average effluent concentrations for
the results obtained. Table 2 shows that the
COD, FOG and total phenol, and the maximum
COD removal efficiency is much higher for 3 d
allowable concentrations allowed to be dis-
HRT than the lower HRT's. The use of the
charged to the sewer system. The ASBR
lower HRT's cannot be justified, as they pro-
effluent concentrations of TSS and FOG are
duce much higher COD values than that re-
lower than the Jordanian standards. COD and
quired by law if the treated OMW is to be
phenol concentrations, however, exceed the
discharged into the sewer system or to the en-
standards.
vironment.

3.5. Nutrient requirements

Table 2 OMW was treated anaerobically in the
Average effluent COD concentrations and removal ef- ASBR without the addition of nitrogen or phos-
ficiencies at different HRT for an influent COD of
about 16,000 mg/L phorous. The OMW was also not combined
with other wastewater containing high concen-
Retention Averageeffluent Averageremoval el- tration of nitrogen and phosphorous. The con-
time, d COD, mg/L ficiency, % centration of nitrogen in the OMW studied in
0.5 7,600 53 this work is higher than other OMW reported in
1 5,500 66 the literature where nitrogen was added to the
2 3,800 76 wastewater for effective treatment to take place
[3,10]. However, (as mentioned above in the
3 2,700 83
OMW characteristics section) the concentration
 B. Y. Ammary / Desalination 177 (2005) 157-165
Table 3
ASBR average treatment efficiency and reactor effluent concentrations for 16,000 mg/L COD concentration at 3 d
HRT.
Parameter Removal efficiency, % Averageeffluent concentration,mg/L
COD 83 2,700
TSS 91 530
FOG 99 18
Total phenol 63 230
is still lower than the concentration reported in
the literature as required for the anaerobic treat-
ment. So how was nitrogen sufficient for the
treatment at this low concentration? It should be
noted that nitrogen is needed for assimilation in
the biomass in biological processes. Biomass
has been universally accepted to have the chemi-
cal formula CsHTNO2P0.074 [1]. In this formula
the ratio of COD:N:P is approximately 100:5:1
for aerobic treatment. For anaerobic treatment,
the ratio is 250:5:1-500:5:1 assuming 40-20%
sludge production, respectively, in anaerobic
treatment compared to aerobic treatment.
In deriving the above ratios, it was assumed
that the efficiency of removal is 100%. The fact
that different wastewaters have different biomass
yields was not taken into account. Therefore
when addressing nutrient needs, one should
take into account both the microbial yield and
the efficiency of COD removal. Giving a ratio
between COD:N:P is misleading as this does
not take into account the previously mentioned
factors (biomass yield and efficiency). This is
especially true for industrial wastewaters that
have low removal efficiency and yield. In the
present study, biomass yield was found to be
about 0.06 g VSS/g COD removed. In addition,
the efficiency of COD removal was about 83%.
In this case, the increase in biomass would be
about 0.05 g VSS/g COD initially present. For
an 11% nitrogen requirement in a biological
cell [21], the nitrogen requirements would be
around 0.0055 g/g COD present. The ratio of
163
Jordanianstandards for sani-
tary sewer discharge, mg/L
2,100
1,100
50
10
COD to nitrogen would then be around 900:5.
For 2% phosphorous requirement in biological
cells [21], the phosphorous requirement would
be around 0.0011 g/g COD present, and the
ratio would then be around 900:1.
If nitrogen content is assumed 11% in an-
aerobic biological cells, and 100% COD re-
moval, then the ratio COD:N of 250:5 would
occur at an observed yield (Yobs) of 0.1818 kg
VSS/Kg COD degraded. In case the observed
yield is different than the above value, and
removal efficiency (E) is different than 100%,
the COD:N ratio required in the wastewater
would be 0.1818(250)/EYobs:5, or 45.5/EYob~:5.
If phosphorous content is assumed 20% of nitro-
gen content then the required ratio of COD:N:P
in an anaerobic reactor should be calculated
from the following formula 45.5/EYob~:5:1. This
formula should be used instead of using a con-
stant value such as 250:5:1 or 500:5:1 for all
wastewaters regardless of the removal effi-
ciency or biomass yield.
In the present study, the observed yield was
found to be equal to 0.06 and efficiency of
COD removal was equal to 83%. The required
COD:N:P ratio will then be equal to
45.5/(0.83)(0.06):5:1, which is equal to 914:5:1.
The average COD:N:P ratio in the present study
(911:5:1.7) was a little bit lower than these
values (914:5:1).
Henze and Harremoes [22] based the
COD:N requirements on loading rates. For
highly loaded processes (0.8-1.2 kg COD /kg
164 B. Y. Ammary / Desalination 177 (2005) 157-165
VSS/d), they recommended a value of 250:5.
For lower loading rates, the value can be in-
creased from 250:5 by multiplying it with a
factor equal to the loading rate in kg C O D / k g
VSS/d divided by 1.2. For the present study, for
a loading rate of 0.44 kg C O D / k g VSS/d, the
COD:N ratio required would be 682:5
(250:5(0.44/1.2)). According to their method of
calculation, the anaerobic treatment of the
OMW used in the present study would not have
been possible without nitrogen addition, which
was not the case. This is due to the fact that
their method also depends on influent COD
concentration, and does not differentiate be-
tween different removal efficiencies. Biomass
yield is also not considered. Therefore, the use
o f loading rates for nutrient requirement deter-
mination is as misleading as the use o f constant
ratios of COD to nitrogen and phosphorous.
More accurate determination of nutrient re-
quirements should be based on both removal
efficiency and biomass yield as suggested
above.
4. Conclusion
The following conclusions can be drawn
from the present study:
• Removal efficiencies of COD, phenol, FOG,
and TSS using ASBR with 3 d retention
time and at an organic load of 5.3 kg COD
/m3/day was equal to 83, 63, 99, and 91%,
respectively.
• OMW in Jordan has sufficient nitrogen and
phosphorous concentrations that addition of
such nutrients was not necessary, nor was it
necessary to combine it with other waste-
waters.
• The COD:N:P ratio required for anaerobic
treatment o f wastewater should be calculated
from a formula that takes into account the
removal efficiency and observed yield for
the wastewater in concern (45.5/EYob,:5:l)
instead of using a constant value for all
different wastewaters, or based on loading
rate.
• Dilution of the OMW was necessary for the
anaerobic treatment of such wastewater.
This was achieved by adding raw OMW to
the reactor containing treated OMW from
the previous batch. This, in addition to no
nutrient requirement, substantially reduces
the cost of treatment.
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