The Dry Batch Anaerobic Digestion: Biogas

Yield and Digestate Organic Matter Quality

Francesco Di Maria, Alessio Sordi, Caterina Micale, Giovanni Gigliotti, Claudia Zadra,
Mirko Cucina. University of Perugia

CONTACT

Name: Francesco Di Maria

E-mail: fdm@unipg.it

EXECUTIVE SUMMARY

Solid Anaerobic Digestion Batch (SADB) has some peculiar features that can lead to a wider ex-
ploitation of Anaerobic Digestion (AD) also in the field of Waste Management. Limited waste liq-
uid production along with waste pre-treatment needs represents two main advantages achievable
with SADB. Anyway, high Volatile Solids (VS) concentration can lead to excessive Organic Load
(OL) (gVS/kg) causing inhibition mainly of the methanogenic phase and consequently process fail-
ure. Several strategies are suitable for avoiding this risk leading to a stabile biogas yield ranging
from about 400 to 600 Nl/kgVS. Further the solid fraction of the digestate, >90%, shows quite good
features from the agronomic point of view even if some residual phytotoxicity has been evaluated.
The Germination Index (GI) measured by Lepidium sativum L seeds, achieves values ranging from
about 40 up to 50%. These values are lower than the suggested value of 60% even if results compat-
ible with several field crops.

INTRODUCTION

Anaerobic Digestion (AD) of the Organic Fraction of Municipal Solid Waste (OFMSW) seems to
be one of the most suitable way for improving renewable energy production in the EU contributing
to the achievement of the 2020 objective (Directive 2011/77/CE; Beurskens et al., 2011).

Wet (<15% w/w Total Solids - TS) and dry processes (<20-25% w/w TS) are currently the one most
diffused for full scale AD facilities (De Baere and Mattheeuws, 2010) even waste biodegradable
materials as received are not immediately suitable due to their size, to their solid bulk structure and
generally to their hight TS concentration (>25% w/w). These problems can be partially solved by
the adoption of adequate pre-treatment facilities, for humidity increase by water adition, and waste
conditioning that are in any case costly to manage and maintain (Vinot et al., 2010). Further, due to
high humidity concentration, these processes discharge a large amount of liquid and sludge (>50%
w/w) that represents another serious disposal problem in many EU states, requiring often its treat-
ment in Waste Water Treatment Plant. All these aspects had represented a relevant technical and
economic obstacle to the AD diffusion for MSW treatment.

A possible response to all these problems can arise from the adoption of AD technologies able to
work with TS >25% w/w, with a consequent reduced amount of discharged liquid and requiring
slight waste pre-treatments. Solid Anaerobic Digestion Batch (SADB) matches quite well these
needs being able to treat OFMSW with 25%<TS<50% w/w requiring waste pre-treatment that gen-
erally consist in mixing with wood particles for achieving an adequate level of porosity. Under this
conditions the waste is able to maintain its shape once disposed in a open heap (i.e. Solid State) and
discharged liquids results very limited <10% w/w (Di Maria et al., 2012a). In a full-scale SADB fa-
cility OFMSW is handled by weeled loader and the AD reactors are realized by an adequate number
batch, static biocells, with a gross volume ranging from about 800 m3 to 1,200 m3. In each biocell
the AD process is started by mixing the fresh OFMSW (F) with an adequate amount of digestste
exploited as Inoculums (I) (Di Maria et al., 2012a). Further, the digestate discharged by each cycle,
has suitable features for being treated in Mechanical Biological Treatment and/or Composting
plants for further stabilization and/or organic fertilizer production aims (Di Maria et al., 2012b). For
these reasons SADB can lead to a broad implementation of OFMSW AD (Bolonzella et al., 2006)
even if some reliability and stability question concerning the biological process needs to be careful-
ly managed and analyzed.

The high TS and consequently Volatile Solids (VS) concentration at which SADB digesters oper-
ates causes significant increase in reactors Organic Load (OL) (gVS/kg) and can lead to some pro-
cess instability and inhibition phenomena. The short term biodegradability materials of OFMSW
can provide to rapid carbohydrate hydrolysis and alcoholics fermentation causing a Volatile Fatty
Acids (VFA) accumulation along with a more or less relevant drop in pH (Schievano et al., 2010).
As consequence the methanogenic phase can results inhibited or strongly influenced by the VFA
concentration during the anaerobic process (Montero et al., 2010; Guendouz et al., 2010;
Dong_Hoon and Sae-Eun, 2011; Illmer and Gstraunthaler, 2009).

A suggested solution for managing these phenomena is to increase the amount of reintroduced di-
gestated exploited as I causing a reduction of the F/I ratio to values < 0.35 (kgVS/kgVS) (Schievano
et al., 2010; Guendoz et al., 2010; Di Maria et al., 2012a). Anyway this can lead to a significant
economic investment and management costs increase, due to the consequent larger volume required
for the biocells together with the higher amount of material handled during discharge and loading
operations.

Aerobic pre treatment of the OFMSW before SADB can reduce the concentration of short term bio-
degradable material concentration reducing VFA production rate and consequently risks of inhibi-
tion. Anyway this can reduce the amount of biogas and consequently of energy recoverable per unit
of treated mass (Di Maria and Valentini, 2011).

Another possible solution can be represented by the exploitation of the high solubility property of
VFA. Spreading the liquid fraction produced during the process on the mass under treatment is a
used practice that can lead to many advantages as nutrients redistribution, bacterial and humidity
equalization increasing process efficiency. Contemporary during its percolation path through the
waste mass, dissolves a fraction of the VFA produced at the boundary of the solid particles that are
consequently withdrawn from the digester together with the liquid. This percolate can be stored for
a given Retention Time (RT) in a dedicate tank operating as a wet AD reactor. In this way excessive
VFA concentration in SADB reactor can be reduced and the fraction dissolved in the liquid can also
contribute to the global biogas production, leading to a whole process reliability and efficiency in-
crease. Further, depending on OFMSW quality and on Inoculum quality and quantity, the solid frac-
tion of the digestate can result quite stabilized after the anaerobic phase and consequently potential-
ly exploitable directly for agricultural needs.

All these aspects have been investigated by a long period experimental analysis involving the eval-
uation of F/I ratio, liquid recirculation, VFA evolution, Biogas Yield (BY) and Biomethane Yield
(BMY) along with the evaluation of the agronomic quality of the digestate.

METHODS

Experimental Apparatus
The effect of different F/I ratio, the BY and the digestate quality have been evaluated by the exploi-
tation of a Large Scale (LS) laboratory SADB experimental apparatus. Due to the difficulty of
withdraw samples from the LS apparatus, the analysis of the VFA evolution with and without liquid
spreading has been performed by the activation of a second static batch laboratory test exploiting
Serum Bottles (SB).

The first apparatus consist of LS laboratory SADB reactor, with a gastight, static steel, cylindrical
reactor of 100 litres (Fig. 1), with a removable top. Process temperature is maintained at mesophilic
values (35°C±2°) by a thermal band powered by a potenziometer controlled by a Resistance Detec-
tor Temperature (RTD) inserted inside the reactor volume. The F+I mixture is supported by a grid
with 1 cm diameter holes, that physically separates the solid material from the liquid fraction recov-
ered in the reactor bottom. A temporized pump spreads about 0.18 l per kg of VS on the mixture
top. The liquid flows through the F+I mixture and is recollected beneath at the reactor bottom. At
given periods the liquid is sampled for VFA and other parameters analysis. Both the biogas pro-
duced by the liquid and by the solid fractions is collected from the reactor top, piped to a dehumidi-
fier vessel and then to a thermal flow meter (0.1% FS). CH4 and CO2 concentration %v/v have been
determined by infrared sensors (±1%) whereas O2 and HS2 concentration %v/v have been deter-
mined by electrochemical sensors (±2%).

For evaluating the VFA concentration during SADB with no liquid spreading a second experi-
mental apparatus consisting of three series of 10 Serum Bottles (SB) of 1 litres each one has been
activated (Fig. 2). Inside of each bottle has been inserted the same F+I mixture exploited in the LS
apparatus. SB are immerged in a mesophilic thermal bath and two bottles per each series have been
equipped by hydraulic gasometer apparatus for biogas production measurement. At the same period
established for liquid sampling from the LS three bottles content one per each series, has been de-
finitively analyzed. The content of the bottles equipped with gasometric apparatus were the last ana-
lyzed. Generally a given amount of liquid is naturally produced during the AD process depending
on the TS concentration of the F+I mixture. For satisfying both spreading pump and sampling needs
25% w/w of deionized water has been added at run start in LS and SB reactors. In full scale SADB
reactors a given amount of ambient air remains entrapped both in waste mass porosity and in biocell
free board during loading operation, leading to an initial aerobic process. As the free oxygen con-
centration is gradually reduced, anaerobic phase starts. For reproducing also in the LS and SB tests
this phenomenon, the usual initial fluxing of reactors with inert gases has been omitted.

Figure 1 LS SADB experimental apparatus schematic

Feedstock and Inoculums

The OFMSW has been withdrawn from an existing Composting plant treating Source Selected Or-
ganic Fraction. Bulky and not rapidly biodegradable materials have been manually removed for al-
lowing the insertion also in SB apparatus. The I exploited for staring the first runs has been generat-
ed in previous laboratory mesophilic (35°C±2°) SADB tests performed on OFMSW. Following
runs have been activate by digestate arising from previous test. The initial F to I ratio by weight on
wet basis exploited in the runs ranges from 1:1 to 1:3. The test for the evaluation of VFA evolution
with and without liquid spreading have been performed with F/I ratio of 1:1.

Figure 2 SB experimental apparatus

Sampling and Characterization

The F, I and digestate Moisture Content (MC) (gravimetric, wet basis) was determined by drying at
105 ° C for 24 h. The VS content (dry basis) and ashes were determined as sample weight loss (pre-
viously oven-dried at 105 °C) upon ashing at 550 °C for 24 h in a muffle furnace. The pH of the dif-
ferent samples were determined by dilution 1:10 w/v with demineralized water and mixing for 30
minutes at room temperature.Total Organic Carbon (TOC) was determined by the Springer and
Klee wet dichromate oxidation method (Nelson and Sommer, 1996), while Total Nitrogen (TN) was
obtained by Kjeldahl method. Humic Acid (HA) and Fulvic Acid (FA) were determined by extract-
ing compost with 0.1 N NaOH in nitrogen atmosphere by using the method described by Bourbon-
niere and Creed (Bourbonniere and Creed, 2006). Phosphorus assimilated was extracted with 0.5 M
NaHCO3 solution at pH 8.5 then was used a spectrophotometer. Potassium exchangeable was
estimated with use of ammonium acetate solution, than was used atomic absorption spectroscopy. A
modified phytotoxicity test (Pullicino et al., 2007) employing seed germination, Germination Index
(GI), was used to estimate digestate maturity exploiting seeds of Lepidium sativum L. (Zucconi et
al, 1985). To perform the analysis of heavy metals content, soil samples were digested according to
the US EPA 3050B (1996) method. Heavy metals concentrations were determined by flame atomic
absorption spectrophotometry using a Shimadzu AA-6800 apparatus.

Liquid fraction sampled from the LS and from the SB runs has been acidified then centrifuged at
5,000 rpm for 15 min. The liquid fraction has been recovered through a 0.4 m sieve and analyzed
by gas chromatography for VFA determination.

RESULTS AND DISCUSSION

Biogas and Biomethane Yield

The chemical and physical characterization of the Inoculum and the OFMSW used in the runs (Ta-
ble 1) showed TS content greater than 35% w/w, VS greater than 85% w/w of TS and a TOC great-
er than 40% w/w of TS. The C/N ratio ranged from 23 to 26. The higher values of the C/N ratio for
I instead of for the OFMSW is mainly a consequence of the initial composition of the OFMSW
used in laboratory for generating the I.

The runs showed that the higher was the amount of I per unit of OFMSW, the higher was the
amount of BY and BMY producible for each kgVS of the F (Fig. 3a). This is in agreement with the
reduction in the inhibition caused when working with high TS values (Schievano et al., 2010). In
fact, for an F/I ratio of around 0.9, the BY was about 400 Nl/kgVS and the BMY was about 210
Nl/kgVS. When the F/I value was around 0.2, the BY reached about 600 Nl/kgVS and the BMY
was about 350 Nl/kgVS. The mean methane concentration in the biogas was always more than
50%, which is a suitable level for exploitation as fuel in Internal Combustion Engines (ICE) for
electrical energy production.

Table 1 Inoculum and OFMSW characterization

Parameter Inoculum (I) OFMSW (F)

TS (% w/w) 57.22±7 66.17±10
VS (% of TS) 70.16±4 93.62±1
TOC (% of TS) 37.62±5 39.69±10
C/N 27.79±13 19.93±10

In agreement with the experimental results, as I increases, at constant kgVS of F, the increase in
BMY, which influences the amount of recoverable renewable energy, is lower than the increase in
BY. This is coherent with the biochemistry of the AD process. In effect, a methane concentration
greater than 40-45% (v/v) in the biogas during SADB was generally achieved after a period of time
ranging from 2 to 7 days (Fig. 3b), depending on many factors such as waste characteristics, process
conditions (temperature, pH, ..) and on the amount and quality of the OFMSW and I used. In any
case, keeping the other parameters constant, the more I used per unit mass of OFMSW, the shorter
was the transient period, generally.

This means that the increase in biogas methane content was limited with respect to the production
of Biogas (BY), due to the F/I ratio.

In all the runs the waste liquid fraction produced during the SADB process results lower than 10%
w/w of the whole mass of the fresh OFMSW and Inoculum processed in the SADB reactor.
700
650 Biogas
600 CH4
550 Mean Trend a)
500
450
NL/kgVS

400
350
300
250
200
150
100
50
0
0,20 0,29 0,45 0,49 0,91
F/I (kgVS/kgVS)

Figure 3 BY, BMY a) and CH4 concentration b) for different F/I.

Liquid Spreading and VFA Evolution

The evaluation of VFA evolution for SADB with and without liquid spreading has been performed
comparing the VFA concentration in the LS apparatus with the average one measured for three par-
allel SB runs exploiting the same F+I mixture of the LS test.

Table 2 shows characteristics of the Inoculum and OFMSW exploited in the specific VFA test. The
ratio of the kg VS of MSWOF and I exploited in the tests is of 0.91, with mass ratio, on wet basis,
of 1:1. The pH of the I is quite alkaline whereas the pH of the MSWOF results definitely acid.
The BY of the SADB experimental apparatus results to be higher than the one produced by the
same mixture in the bottles laboratory test (Fig. 4a). During the first 7-10 days, the biogas rate per
kg of VS results very similar for the two runs. After this initial period, the SADB apparatus biogas
rate becomes decisively higher than the one produced by the bottles. This trend is also confirmed by
the daily biogas production curves (Fig. 4b). Infact, during the first 7-10 days the daily biogas rates
curves overlaps with a high precision. After this period, the two curves become decisively divergent
until 22nd day of the process. Infact, after 20 days, the SADB daily production curve achieve a max-
imum whereas the bottles one a minimum value. In the successive days the SADB curve show a
constant decrease (Fig. ab) whereas the bottles curve shows a growing trend, even if with a signifi-
cant fluctuation around the mean value. Furthermore, this fluctuation seems to have a growing trend
around the last days of the AD process. This behaviour is the consequence of the strong VFA con-
centration during the process. The TVFA concentration in the both tests is very similar, around
20,000 mg/l, until the 5th day (Fig. 5).

Table 2 Inoculum and MSWOF exploited for VFA runs characterization

Parameter Inoculum (I) OFMSW (F)
TS (% w/w) 37.72 27.33
VS (% of TS) 95.04 93.27
pH 8.90 4.97
N (% of TS) 1.03 2.67
C/N 40.78 10.90

400 14

SB LS
350 12
LS SB
300
10

250
b)
Nl/kg VS/day

8
Nl/kg VS

200
6
150

4
100

50 a) 2

0 0
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75
day Day

Figure 4 Cumulate BY a) and Daily biogas rate b) for the LS and SB runs

45000

40000

35000
SB
30000 LS
TVFA(mg/l)

25000

20000

15000

10000

5000

0
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75
day

Figure 5 TVFA evolution in the LS and SB runs

Then, the TVFA concentration in the percolate of the SADB decrease significantly, achieving a
concentration lower than 5,000 mg/l after the 25th day. The TVFA concentration in the bottles runs,
without percolation, continues to rise constantly until the 30th day reaching a maximum value higher
than 42,000 mg/l. After this maximum value the TVFA concentration show a decreasing trend, even
if with significant oscillation. This phenomenon justifies the strong instability in the daily biogas
production. In more detail, has shown by Figure 6, the Acetic and Butyric acid concentration re-
mains higher than 10,000 mg/l for a very long period (Fig. 6a). Also the Valeric and Propionic acid
(Fig. 6b) has a significantly higher concentration during the whole bottle test compared to the one
measured in the SADB apparatus. The significant variation of the different VFA, causes the strong
instability of the daily biogas production instead of the one achieved in the SADB apparatus.

The experimental results show the higher biogas production and process stability of the process per-
formed in the SADB apparatus. The main difference occurring among the two tests is represented
by the presence of the percolate recirculation in the SADB apparatus. Infact, a fraction of the VFA
produced are solubilised in the periodically recirculated percolate, reducing its concentration and
inhibition effect in the solid phase of the SADB reactor. Furthermore, in the percolate stored at the
bottom of the reactor, a second wet AD process take places. The high humidity at which this second
process takes places, allows a rapid metabolism of the acids leading to a higher total biogas rate.
This phenomenon contributes also to the higher stability shown by the process performed in the
SADB apparatus.
15000 8000
Propionic
7000
12500 Acetic Isobutyric
Butirric Isovaleric
Acetic 6000

10000
SB Butirric
Valeric
5000
SB
(mg/l)

LS
(mg/l)

7500 4000

3000
5000

2000
LS a) b)
2500
1000

0 0
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75

day Day

Figure 6 Acetic and Butyric a) and Propionic, Isobutyric, Isovaleric and Valeric acids concentration evolution b)
in the LS and SB runs

In the bottles runs, the AD process occurs with percolate in static conditions. This means that the
solid and the liquid phase are not physically separated. During the fermentation phase, the alcohols
and VFA produced are continuosly solubilised in the liquid phase, leading to a very high concentra-
tion. This causes a process inhibition both in the liquid phase and at the solid particle surface. These
preliminary results show that the percolate recirculation is able to reduce SADB inhibition phenom-
enon, increasing both process stability and biogas yield. This is an aspect of fundamental im-
portance in the management of full scale SADB reactors, able to ensure a quite efficient and viable
SADB process. Further positive effects of percolate recirculation can also lead to a significant re-
duction of I needs, with a consequent reduction in full scale investment costs.

Digestate Agronomic Quality

Four consecutive runs exploited with the LS apparatus with different F/I ratios have been uti-
lized for evaluating both the F+I and the digestate quality from the agronomic point of view.
Total Organic Carbon ranged between 35-45% TS and the C/N ratio resulted in a maximum
value of 40.78 for the digestate during the 3rd run. No differences were observed in the
HA+HF content among the fresh mixture and the digestates in each run, with values which
ranged between 5-15 %DM and 7.5-10% respectively (Fig.7). The Germination Index (GI) is
relatively low, but the use of this digestate as soil fertiliser may be considered not dangerous
for field crops. The GI values not enable the use of the digestate as growth medium.

The Total Nitrogen (Ntot) content showed a decrease during each run, whereas mineral nitro-
gen concentration remains quite constant during the process. Heavy metals concentration
showed a reduction from the inlet material respect to the outlet one whereas nutrients concen-
tration, as K, decreased (Fig. 8). Generally during AD the heavy metal, K and N concentra-
tions increase, due to the degradation on organic matter. In this case the different behaviour
observed was probably due to the relatively low mass loss and to the leaching effect of liquid
spreading (Fig. 9).

60

55
C/N
50 TOC IN
HA+FA OUT
45
GI
40

35

30
% TS

25

20

15

10

0
1 2 3 4 Run n°
0,49 0,45 0,21 0,91 F/I

Figure 7 C/N, TOC, HA+FA, GI of digestate variation vs F/I for the different runs
2,2
Ntot IN
2,0 OUT
Nmineral
1,8
Norganic
1,6

1,4

1,2
% TS

1,0

0,8

0,6

0,4

0,2

0,0
a)1 2 3 4 Run n°
0,49 0,45 0,21 0,91 F/I
)

Figure 8 Total, mineral and organic Nitrogen for F+I (IN) and Digestate (OUT) vs F/I
 60

40

20

8 Cu ppm DM
Pb ppm DM

% TS - ppm TS
7 Cr ppm DM
K % DM
K (K2O) % DM
6 P % DM
P (P2O5) % DM
5

3
IN
2 OUT

0
1 2 3 4 Run n°
0,49 0,45 0,21 0,91 F/I

Figure 9 Heavy metals concentration vs F/I ratio for the different tests

CONCLUSIONS

Several experimental runs show how the Solid Anaerobic Digestion Batch (SADB) process can rep-
resent an interesting solution for allowing a higher spreading of the Anaerobic Digestion (AD) also
in the field of Waste Management. Narrowed waste liquid fraction produced and slight pre-
treatment required represent two main advantages that makes SADB a sustainable and competitive
solution if compared to other AD technologies. Process instability arising from high Organic Load,
due to high Total Solids concentration, affecting viability of SADB, can be successfully managed
by liquid spreading during SADB process. The Biogas and Biomethane yield results significantly
influenced by the amount of inoculums exploited for process start up, ranging respectively from 400
to 600 and 200 to 350 Nl/kgVS. The quality of the digestate obtained after SADB show quite good
agronomic properties both in terms of nutrient and in terms of fixed carbon. Some problems of ma-
turity are pointed out by the phytotoxicity evaluated by the Germination Index (GI). GI values ob-
tained ranges from about 40 to 50% being quite lower than the minimum values suggested by some
authors (i.e. 60%) but in anyway acceptable from several field crops.

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