Sustainable Environment Research 27 (2017) 259e264

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Original Research Article

Effect of ultrasonic pre-treatment on biogas yield and specific energy

in anaerobic digestion of fruit and vegetable wholesale market wastes
Reyhaneh Zeynali, Mehdi Khojastehpour, Mohammadali Ebrahimi-Nik*
Department of Biosystems Engineering, Ferdowsi University of Mashhad, Mashhad 9177948974, Iran

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

Article history: Ultrasonic pre-treatment has been considered as an environmentally friendly process for enhancing the
Received 20 May 2017 biodegradability of organic matter in anaerobic digestion. However the consumed energy during the pre-
Received in revised form treatment is a matter of challenge especially where energy generation is the main purpose of a biogas
16 June 2017
plant. The aim of the present work was to study the efficiency of ultrasonic pre-treatment in
Accepted 10 July 2017
Available online 23 July 2017
enhancement of biogas production from fruits and vegetable wholesale market waste. Three sonication
times (9, 18, 27 min) operating at 20 kHz and amplitude of 80 mm were used on the substrate. The highest
methane yield was obtained at 18 min sonication (2380 kJ kg
1 total solids) while longer exposure to
Keywords:
Ultrasonic pre-treatment
sonication led to lower methane yield. This amount of biogas was obtained in 12 d of batch time. The
Energy efficiency energy content of the biogas obtained from this reactor was two times of the input energy for sonication.
Anaerobic digestion © 2017 Chinese Institute of Environmental Engineering, Taiwan. Production and hosting by Elsevier B.V.
Biogas This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
nc-nd/4.0/).

1. Introduction transportation and disposal costs are considerably high (around

7  109 IRR yr
1 (currently 1 USD ¼ 32,500 IRR) for Tehran [4]).
Fast rates of population growth and industrialization of nations Biogas production through anaerobic digestion (AD) is a verified
have precipitated the increase in energy consumption and waste and commercialized technology for the treatment of organic solid
production [1]. Inadequate and ineffective management of solid wastes [6]. AD is a biological process during which complex organic
waste leads to different issues like environmental pollution, global substrate is decomposed in the absence of oxygen by means of
warming, acid rain, destruction of the ozone layer, low level of public numerous types of anaerobic microorganisms. It includes four main
health and poor living conditions [2]. Decomposition of one metric closely linked steps named hydrolysis, acidogenesis, acetogenesis,
ton of organic solid waste can potentially release 50e110 m3 of and methanogenesis. There are three ranges of temperature for AD
carbon dioxide and 90e140 m3 of methane [3] into the atmosphere. process; psychrophilic (15e30  C), mesophilic (30e50  C), and
One of the main sources of mass solid waste in some cities of Iran thermophilic (> 50  C) [7]. In another categorization, based on the
is fruit and vegetable wholesale markets. These places play an total solids (TS) of substrate in reactor, AD is divided into wet, when
important role in regulating the market of agricultural products in TS is lower than 10%, semi-dry with the TS ranging between 10 and
this country [4]. About 35% of the total fruit and vegetable is wasted 15%, and dry with a TS above 15% [8]. Beyond biogas (mostly
[5] due to the shortages of processing and deficiencies in preser- methane and carbon dioxide), there is a slurry byproduct named
vation facilities. For instance, an incredible amount of 150 t d
1 of digestate which is usually used as fertilizer. The heating value of
fruit and vegetable wastes (FVW) at wholesale markets was re- 1 kg methane (55.5 MJ kg
1), the main component of biogas, is
ported in Tehran [4]. This number increases to 3e5 Mt yr
1 for the equivalent to 1.2 kg of diesel or 3.7 kg of wood [9].
entire country [5]. Such wastes are currently collected together with Methane production from AD of organic solid waste is signifi-
the municipal solid wastes and are mostly disposed in landfills. The cantly affected by the mass transfer in each biological step and,
hence, substrate availability. It is recognized that the rate limiting
step in AD is the hydrolysis of complex organic matters into soluble
compounds [10,11]. Therefore, chemical [12], physical [13] and
* Corresponding author.
E-mail address: [email protected] (M. Ebrahimi-Nik).
biological [14] pre-treatment or their combinations [15] can be
Peer review under responsibility of Chinese Institute of Environmental used to improve anaerobic efficiency. Ultrasonic technique has
Engineering. been well confirmed as the most powerful method when compared

http://dx.doi.org/10.1016/j.serj.2017.07.001
2468-2039/© 2017 Chinese Institute of Environmental Engineering, Taiwan. Production and hosting by Elsevier B.V. This is an open access article under the CC BY-NC-ND
license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
260 R. Zeynali et al. / Sustainable Environment Research 27 (2017) 259e264

with bacterial, thermal, and chemical pre-treatment [10,12] in the 20 kHz and amplitude of 80 mm. Before pre-treatment, samples
digestion of meat industry wastes. However, it is worth mentioning were blended for 3e5 min to obtain a homogeneous mixture
that studies have indicated that the noise from ultrasonic devices (Fig. 1). Digestion of 900 mL of the substrates (a mixture of 630 mL
may cause negative symptoms in exposed operators (e.g., dizziness, FVW and 270 mL inoculum) was performed in 1000 mL glass re-
tinnitus, excessive fatigue, nausea, ear fullness and headache) [16]. actors kept in water bath equipped with circulation pump. The
Therefore, it has been suggested to control the ultrasonic pollution temperature of the water bath was adjusted to 35  C so that mes-
using steel or even glass casings, coupled with acoustic absorbing ophilic condition was guaranteed (Fig. 1). Sampling from the di-
blankets to line the machine enclosure to reduce the noise [17]. gesters was possible from a valve at the bottom of the digester. The
The effect of ultrasonic is based upon monolithic cavitation, biogas storage tank was a plastic bottle with the capacity of 2.5 L
with physical and chemical impacts in the slurry [18]. The collapse equipped with a septum in its upper portion for biogas sampling.
of cavitation bubbles during the sonication modifies the chemical Volume of biogas was daily measured using liquid displacement
structure by the creation of free radicals [19]. This physical disin- method and converted to the volume at the standard temperature
tegration leads to the enhancement of microbial activity which in and pressure conditions. In water displacement method, the pro-
turn improves biogas yield [20]. duced biogas distributes into a gas collection bottle filled with
The impact of ultrasonic has widely been investigated in AD of acidified water saturated with salt, causes an equivalent volume of
sludge and municipal wastewater; however, there are limited re- solution to be displaced to a graduated cylinder. From this displaced
ports on solid wastes. The effect of ultrasonic pre-treatment on AD solution, one can easily record the volume of biogas produced
of FVW is not documented in scientific literature. Therefore, the aim during the day [11].
of the present project was to investigate the effect of ultrasonic
duration on biogas yield, batch time, and energy performance of 2.3. Analytical methods
the reactor in AD of FVW under mesophilic conditions.
Liquid and the produced biogas samples were taken on daily
2. Materials and methods basis. The methane and carbon dioxide contents of the biogas were
determined by an Einhorn fermentation-saccharometer [23]. The
2.1. Feedstock saccharometer is a bent, graded glass pipe, which is filled with a
solution of NaOH. 5 mL of biogas sample was injected in the solu-
The FVW which was a mixture of mostly fruits, vegetables, po- tion. The carbon dioxide immediately dissolves in the solution
tatoes, and paper was prepared in our lab according to Fountoulakis while the methane forms a gas bubble at the top of the pipe. By
and Manios [21]. The wholesale market wastes always contain determining the volume of the gas bubble, the amount of methane
papers from fruits packaging. The mixture was shredded using a in the biogas can be easily calculated. The pH was measured by a pH
household blender to get a particle size of less than 5 mm and then meter (pH-201). Total Kjeldahl nitrogen (TKN) was determined by
stored at 4  C. The characteristics of the feedstock are summarized titration with 0.1 N H2SO4 after distillation using a Kjeldahl auto-
in Table 1. The FVW had a C:N ratio of 24 which is within the op- sampler VAPODEST 50s Carousel. Samples were dried at 105  C,
timum range (15e30) proposed by many investigations [7,22]. The titrated with 0.5 N ammonium iron(II) sulfate after digestion with
value of initial pH was low, hence, 30 mL of 7 M NaOH solution was H2SO4 in order to determine the organic carbon content. TS, volatile
added to each digester in order to get close to the optimal pH range solids (VS), and ash were measured by the Standard Methods for
for AD. At the start of the tests, FVW was diluted with tap water to the Examination of Water and Wastewater [24]. Total of 12 exper-
obtain the TS content of 5%. Digestate from a lab digester fed with iments were done in 3 replicates for 25 d (Table 2). Reactor R1,
cow dung was used as inoculum. Before the experiment, the corresponded to not pretreated FVW as the control reactor.
inoculum had been kept at mesophilic condition (35  C) for several
days until no gas production was observed. It had a TS, VS, and C/N 2.4. Theoretical analysis
ratio content of 10.4%, 25.8% and 24, respectively. The value of pH
for the inoculum was 7.88. The specific energy (SE) was used to describe the energy con-
sumption during the ultrasonic pre-treatment. SE was calculated
2.2. Experimental set-up for each reactor based on sonication energy and the TS of the
€ z et al. [25]:
sample (Eq. (1)) as described by Alago
Ultrasonic pre-treatment was applied by a Qsonica XL2020
Pt  
sonicator equipped with a 38 mm diameter sonotrode, operating at SE ¼ kJ kg
1 TS (1)
V  TS0
Table 1
Characteristics of the substrate.
where P is the exposure power constant (0.1 kW); t is the exposure
FVW Parameter time (s) of the sample to sonication; V is the volume (L) of the
40 Fruit waste content (%, w.b.) treated sample; and TS0 is the initial TS (kg L
1).
25 Vegetable waste content (%, w.b.) Statistical analysis was carried out with the software package
25 Potato waste content (%, w.b.) SPSS, version 21. In the first step, means and frequency distribu-
8 Bread waste content (%, w.b.)
tions of the data were determined. The ANOVA was used to
2 Paper waste content (%, w.b.)
18.7 Total solids (%, w.b.) determine whether there were any statistically significant differ-
81.3 Moisture content (%, w.b.) ences between the means.
75.8 Volatile solids (% of TS)
24.3 Ash (%)
3. Results and discussion
189.5 Bulk density (g L
1)
4.51 pH
39.6 Total carbon (%, d.b.) 3.1. ANOVA
1.65 TKN (%, d.b.)
24 C/N ratio Table 3 illustrates the analysis of variance of biogas and methane
Note: w.b., wet base; d.b., dry base. volumes, and methane percentage. Ultrasonic pre-treatment had
 R. Zeynali et al. / Sustainable Environment Research 27 (2017) 259e264 261

Fig. 1. Experimental setup including water bath, reactors, and volume measurement bottles (right), ultrasonic pre-treatment (left).

Table 2 3.2. Biogas production

Anaerobic digestion tests based on C:N ratio of 24.

Reactor Symbol Sonication Specific energy Initial The findings showed that the batch time of 25 d was adequate to
time (min) (kJ kg
1 TS) VS (g L
1) observe the targeted effect of pre-treatment. The production of
R1 FVW 0 0 31.09 biogas was almost stopped after 22-d digestion. The highest
R2 FVW9 9 1175 32.02 methane yield occurred in the digester with FVW pretreated for
R3 FVW18 18 2380 32.05 18 min (237 mL CH4 g
1 VSin, 80% higher than the control). Signifi-
R4 FVW27 27 3560 31.93
cant improvement in methane yield by ultrasonic pre-treatment has
been reported by several researchers [29,30]. Recently, Vieitez and
Ghosh [3] examined the effect of ultrasonic pre-treatment on biogas
significant effects on methane yield (p < 0.01), and the biogas yield yield from kitchen waste and stated that the sonication time and
(p < 0.05), while it had no significant effect on methane percentage. density (W mL
1) have a significant effect on biogas yield. Fig. 3a
The coefficient of variation for the biogas and methane production compares the cumulative methane production over the time in
was 13.4 and 13.7%, respectively. different ultrasonic exposure times. At the beginning of the process,
Comparison of means by Duncan test showed that there was a the rate was slow and then increased smoothly for all the cases. The
significant increase in total biogas yield (from 249 to 396 mL biogas process of hydrolysis and acidogenesis release CO2 which is the
g
1 VSin) as ultrasonic exposure time increased from 9 to 18 min, dominant gas in the first days of AD as reported by others [29,31].
however the impact of longer exposure time (27 min) was not The reactor fed with non-pretreated FVW produced the total of
significant (Fig. 2). Therefore, it can be concluded that there is an 132 mL CH4 g
1 VSin, which is the least among the other treatments.
optimum exposure time above which, higher biodegradability may When the FVW was pretreated by ultrasound with the specific
not be occurred. There is the possibility of even lower amount of energy of 1057; 2380 and 3560 kJ kg
1 TS, methane production
biogas production as the result of longer sonication time as re- increased by 29, 80, and 63%, respectively. As discussed above,
ported by Peces et al. [26]. decreased particle size and improved organic matters solubility
These outcomes could be related to particle size changes due to after ultrasonic might be the reason of these increases [29,32].
the sonication effects. As sonication progresses, flocs are firstly The pH values throughout the study are good indicators of AD
reduced, but in longer sonication time, more release of intercellular stability. On the first day, pH dropped (Fig. 3b) due to the progress
polymers happens due to cell lysis which is favorable for re- of the fermentative process [33]. AD mainly includes four steps:
flocculation. Re-flocculation of the particles leads to increased hydrolysis, acidogenesis, acetogenesis, and methanogenesis. Dur-
particle size [10,27] and consequently lower hydrolysis rate, which ing the first two stages, production of a large amount of volatile
in turn, leads to lower biogas yield. Cesaro et al. [28] found that fatty acids leads to decline in pH. At low pH values, non-
increasing the ultrasonic SE from 2100 to 6300 kJ kg
1 TS slightly methanogenic microorganisms can be active, while methanogenic
reduced the methane production for dried distilled grain. activities are significantly inhibited [29].

3.3. Effect of ultrasonic on SE

Table 3
Analysis of variance of biogas, methane yield, and methane percentage. Although the positive effect of ultrasonic on biogas yield is
proven, the efficiency of this pre-treatment in term of net energy
Sum of Degrees Mean square F
squares of freedom yield has yet to be considered. The main concern on practical
application of ultrasonic is its high energy consumption [34]. The
Biogas production 35,620,227 3 11,873,409 6.16*
Methane percentage 80 3 27 3.57ns energy needed for sonication is related to the power and time.
Methane production 17,534,667 3 5,844,889 13.53** Generally, ultrasonic power has more effect than its exposure time
**
99% confidence level.
[35].
*
95% confidence level. On the other hand, longer sonication time not only consumes
ns
Not significant. more energy, but also may reduce the microbial activity [36]. In this
262 R. Zeynali et al. / Sustainable Environment Research 27 (2017) 259e264

300
Control: Without Pre-treatment

Cumulative Methane Yield (mL g-1 VSin)

250 Ultrasonic Pre-treatment
B
B
200
A

150 A

100

50

0
0 9 18 27
Ultrasonic Exposure Time (min)

Fig. 2. Cumulative methane yield in different ultrasonic exposure time (different letters indicate significant differences at p < 0.01, TS ¼ 5%, T ¼ 35  C).

research, the effect of longer ultrasonic time (18 and 27 min) on in 12 days. Shorter batch time means more economic profitability
methane yield was not significant (Fig. 2). The VS reduction in through smaller digester or more feedstock loading rate.
reactor with 18 min was 64% and the methane yield was 237 mL Longer ultrasonic time not only upsurges energy input of the
CH4 g
1 VSin. Moreover, in this reactor, the process was completed digester, but also decreases the net energy yield. Therefore, in

250
(a)
Cumulative Methane Production

200
(mL g-1 VSin)

150

100
FVW
FVW9
50 FVW18
FVW27

10
(b)
9

8
pH

5
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25
Time (d)

Fig. 3. Cumulative methane production (a) and changes of pH (b) of FVW with different exposure time of sonication (FVW: control, FVW9, FVW18 and FVW27: ultrasonic pretreated
for 9, 18 and 27 min, respectively, TS ¼ 5%, T ¼ 35  C).
 R. Zeynali et al. / Sustainable Environment Research 27 (2017) 259e264 263

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