Ferrer 2010 BITE
Ferrer 2010 BITE
Ferrer 2010 BITE
Bioresource Technology
journal homepage: www.elsevier.com/locate/biortech
Environmental Engineering Division, Department of Hydraulic, Maritime, and Environmental Engineering, Technical University of Catalonia (UPC),
c/Jordi Girona 1-3, E-08034 Barcelona, Spain
b
GIRO Technological Centre, Rambla Pompeu Fabra 1, 08100 Mollet del Valls, Barcelona, Spain
c
Institute of Biotechnology and Biomedicine, Universitat Autnoma de Barcelona, Bellaterra, Cerdanyola del Valls, 08193-Barcelona, Spain
d
Composting Research Group, Department of Chemical Engineering, Escola Tcnica Superior dEnginyeria, Universitat Autnoma de Barcelona, Bellaterra, Cerdanyola del Valls,
08193-Barcelona, Spain
a r t i c l e
i n f o
Article history:
Received 15 July 2009
Received in revised form 26 November 2009
Accepted 5 December 2009
Available online 6 January 2010
Keywords:
Biogas
Biosolids
Dewaterability
Hygienisation
Wastewater
a b s t r a c t
The aim of this study was to evaluate the performance of thermophilic sludge digestion at decreasing
sludge retention time (SRT) and increasing organic loading rate (OLR), in terms of methane production,
efuent stabilisation, hygienisation and dewaterability. Focus was put on determining indicators to help
prevent process failure. To this end, a lab-scale reactor was operated for nearly 2 years at 55 C. Methane
3
d 1) by decreasing the SRT from 30 to 15
production rate was increased (from 0.2 to 0.40.6 m3CH4 mreactor
3
d 1. Sludge dewaterability was
10 days, while increasing the OLR from 0.5 to 2.53.5 kg VS mreactor
worsened at SRT below 15 days; while pathogen destruction was always successful. The following
concentrations might be used to prevent process failure: VFA C2C5 (3.7 g COD L 1), acetate (0.6 g L 1),
acetate/propionate (0.5), intermediate alkalinity (1.8 g CaCO3 L 1), intermediate/partial alkalinity (0.9),
intermediate/total alkalinity (0.5), CH4 in biogas (55%).
2009 Elsevier Ltd. All rights reserved.
1. Introduction
In anaerobic digesters, biogas production depends on the
amount of organic matter biodegraded by anaerobic microorganisms. Thus, it depends on the composition of the substrate, and
presence and equilibrium between anaerobic consortia in the reactor. Design and operation parameters of the process include sludge
retention time (SRT), organic loading rate (OLR), temperature and
reactor ow, amongst others.
Sludge hydrolysis is often regarded as the rate limiting stage
of the overall process (Vavilin et al., 2008); it affects the total
amount of solids converted into soluble compounds and ultimately to biogas. However, soluble substrates utilization rates
for fermentation and methanogenesis play a key role on process
stability. The concentration of intermediate products like volatile
fatty acids (VFA) is a common indicator of process unbalance
(Marchaim and Krause, 1993; Pind et al., 2002). An accumulation
of VFA in the digester may result from problems in the synthro-
* Corresponding author. Address: Environmental Engineering Division, Department of Hydraulic, Maritime, and Environmental Engineering, Technical University
of Catalonia (UPC), c/Jordi Girona 1-3, E-08034 Barcelona, Spain. Tel.: +34 93
4016463; fax: +34 93 4017357.
E-mail addresses: [email protected] (I. Ferrer), [email protected] (F.
Vzquez), [email protected] (X. Font).
0960-8524/$ - see front matter 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biortech.2009.12.006
2973
2. Methods
2.1. Sewage sludge
The sludge used for this work was obtained from two municipal
WWTP near Barcelona (Spain), which serve an equivalent population of 130,000 equivalent inhabitants (EI) each. The conventional
wastewater treatment used in these plants consists of preliminary
and primary treatment and secondary treatment in the activated
sludge unit. Primary sludge (PS) and secondary waste activated
sludge (WAS) are thickened and mixed (sampling point), before
undergoing mesophilic (38 C) anaerobic digestion at 40 days
SRT. Finally, digested sludge is dewatered in a centrifuge.
The inoculum used to seed the digester was mesophilic digested
sludge (since no thermophilic sludge digestion plant operates in
the Barcelona area). The substrate was the mixture of thickened
PS and WAS (75/25% v/v), which was collected weekly and stored
at 4 C until use. Low-solids sludge (total solids (TS) < 40 g L 1)
was used for the rst 14 months; whereas high-solids sludge
(TS > 40 g L 1) was used thereafter. Volatile solids (VS) contents
were 1424 g L 1 (6877% VS/TS) and 3035 g L 1 (5875% VS/
TS) in the low-solids and high-solids sludge, respectively. In general, the values are typical of sludge from conventional activated
sludge WWTP entering digestion, with TS below 50 g L 1 and VS/
TS around 70% (Speece, 1988).
Table 1
Operating conditions.
Period
Time
(days)
Temperature
(C)
SRT
(d)
I
II
III
IV
V
VI
VII
VIII
IX
179
80161
162203
204256
257331
332437
484529
569606
607653
55
55
55
55
55
55
55
55
55
>30
30
25
20
15
10
10
6
10
Low-solids
Low-solids
Low-solids
Low-solids
Low-solids
Low-solids
High-solids
High-solids
High-solids
2974
High-solids sludge
80
70
60
50
4
40
3
SRT (d)
Low-solids sludge
7
30
2
20
10
0
0
80
120
160
200
240
280
320
360
400
440
480
520
560
600
640
OLR
Time (d)
SRT
Fig. 1. Sludge retention time (SRT) and organic loading rate (OLR) and during thermophilic (55 C) sludge digestion. Note: the start-up period has not been included.
Low-solids sludge
High-solids sludge
90
80
VS effluent (g VS L )
-1
70
60
50
40
30
20
10
0
80
120
160
200
240
280
320
360
Time (d)
400
440
480
520
560
600
640
% CH4
VS effluent
Fig. 2. Methane content in biogas (% CH4) and efuent VS during thermophilic (55 C) sludge digestion. Note: the start-up period has not been included.
2975
Table 2
Average feed and digested sludge characteristics and operational parameters during anaerobic digestion of low-solids (periods IVI) and high-solids (periods VIIIX) sludge.
Parameter
Period
I
Working conditions
T (C)
SRT (d)
3
d
OLR (kg VS mreactor
Feed composition
TS (g L 1)
VS (g L 1)
VS/TS
VFA C2C5 (g COD L
pH
Efuent composition
TS (g L 1)
VS (g L 1)
VS/TS
VFA C2C5 (g COD L 1)
Acetate (g L 1)
Propionate (g L 1)
iso-Butyrate (g L 11)
Butyrate (g L 1)
iso-Valerate (g L 1)
Valerate (g L 1)
A/P ratio
IA (g CaCO3 L 1)
IA/TA ratio
IA/PA ratio
pH
Removal efciency
TS removal (%)
VS removal (%)
Biogas characteristics
Biogas production rate (m3
3
mreactor
d 1)
Specic biogas production (m3 kg
II
55.3 1.2
29.1 1.5
0.47 0.1
55.4 1.3
30.3 3.3
0.69 0.1
III
55.4 0.5
25.4 4.4
0.97 0.5
IV
55.3 0.2
20.4 2.8
1.05 0.2
54.7 0.4
16.0 1.7
1.38 0.3
VI
54.2 1.7
10.4 0.5
1.65 0.3
VII
53.2 0.3
9.4 0.8
3.7 0.4
VIII
53.6 1.1
6.2 1.3
5.2 0.5
IX
52.3 1.5
10.1 1.1
2.4 0.3
19.63 1.67 32.77 8.04 31.48 10.84 30.34 7.38 28.86 6.86 23.22 5.17 45.39 3.52 54.61 7.65
40.60 10.93
13.30 0.85 22.16 4.91 23.25 7.70 21.34 4.12 21.01 5.14 17.93 3.85 34.86 2.34 31.21 3.60 24.23 2.70
68.90 4.67 68.21 0.74 74.23 1.79 70.59 2.20 74.78 1.80 77.52 2.00 75.71 0.59 58.08 10.29 62.02 9.11
1.68 0.32
4.30 0.69 3.59 0.55
2.72 0.55 4.51 0.79 3.68 0.76 4.37 1.83 2.49 0.99
1.40 0.22
6.97 0.57
6.04 0.11 5.75 0.18
6.25 0.12 5.92 0.07
6.13 0.29 6.61 0.12 6.81 0.31
7.05 0.25
13.09 1.74 17.60 1.58 14.92 1.15
7.90 0.92 11.15 1.18 9.55 0.87
61.76 0.98 63.19 1.68 63.94 1.14
0.94 0.53 2.16 0.52
1.60 0.81
0.12 0.17
0.31 0.13
0.17 0.15
0.29 0.12
0.69 0.13
0.51 0.24
0.07 0.05
0.19 0.04
0.12 0.09
0.01 0.02
0.00
0.00
0.12 0.06
0.21 0.08
0.20 0.10
0.00
0.00
0.00
0.46 0.39
0.44 0.17
0.39 0.33
0.88 0.08
1.26 0.18
1.09 0.23
0.31 0.03
0.43 0.04
0.37 0.06
0.45 0.07
0.75 0.12
0.59 0.16
8.18 0.11
8.03 0.09
8.15 0.17
20.11 2.80 17.59 0.94 18.90 4.63 21.91 2.34 37.97 9.69
13.50 0.78 11.62 0.68 14.00 2.31 14.94 1.72 18.49 4.02
64.81 1.27 66.39 2.34 70.06 0.86 68.08 0.79 49.07 2.82
2.49 0.48
2.60 0.22 2.31 0.63 5.48 0.74 2.62 0.87
0.17 0.05
0.03 0.04
0.22 0.12
0.58 0.18
0.18 0.27
0.79 0.15
0.92 0.07
0.99 0.10
1.43 0.07
1.03 0.12
0.24 0.06
0.27 0.02
0.29 0.03
0.52 0.03
0.10 0.09
0.00
0.34 0.03
0.08 0.10
0.06 0.08
0.01 0.03
0.34 0.07
0.34 0.03
0.42 0.07
0.78 0.10
0.33 0.16
0.00
0.00
0.03 0.04
0.02 0.03
0.00
0.21 0.07
0.08 0.03
0.22 0.09
0.40 0.11
0.16 0.22
1.32 0.13
1.40 0.12 1.47 0.19
2.09 0.17 1.64 0.30
0.39 0.04
0.41 0.02
0.46 0.03
0.44 0.03
0.39 0.03
0.65 0.09
0.71 0.07
0.86 0.12
0.79 0.11
0.63 0.07
8.08 0.11 7.86 0.12 7.91 0.09
8.03 0.11 8.13 0.04
24.33 6.40
14.39 2.76
60.18 4.78
3.48 0.70
0.52 0.20
1.17 0.15
0.18 0.10
0.01 0.01
0.40 0.13
0.00
0.45 0.19
2.18 0.13
0.40 0.02
0.66 0.07
8.18 0.07
30.7 10.9
42.2 5.9
39.7 15.9
44.1 5.9
50.1 14.2
53.4 3.0
36.1 17.1
40.5 9.1
35.0 17.7
43.2 4.
27.5 20.9
22.7 4.5
50.2 7.5
57.3 4.2
39.8 11.1
40.6 10.1
37.2 19.0
38.6 10.6
0.18 0.06
0.28 0.07
0.35 0.12
0.41 0.14
0.36 0.11
0.56 0.14
1.07 0.15
1.46 0.14
0.61 0.14
0.37 0.11
0.36 0.07
0.42 0.12
0.43 0.08
0.29 0.10
0.37 0.10
0.30 0.03
0.28 0.03
0.27 0.04
VSfed1 )
1
Biogas yield (m3 kg VSremoved
)
Methane production rate (m3
1
3
mreactor
d )
Specic methane production (m3 kg
0.63 0.09
0.70 0.10
0.90 0.43
0.99 0.47
0.81 0.68
1.15 0.20
0.51 0.20
0.71 0.21
0.59 0.14
0.08 0.02
0.22 0.04
0.20 0.04
0.30 0.07
0.24 0.03
0.36 0.11
0.62 0.13
0.86 0.12
0.38 0.08
0.17 0.03
0.26 0.03
0.28 0.08
0.29 0.08
0.19 0.04
0.23 0.06
0.18 0.04
0.17 0.03
0.38 0.08
0.40 0.05
0.47 0.05
0.61 0.29
0.70 0.31
0.59 0.43
0.71 0.13
0.35 0.11
0.43 0.11
0.38 0.09
66.21 1.20 64.02 1.37 61.78 1.49 62.13 3.46 64.33 7.50
63.81 3.75
VSfed1 )
1
Methane yield (m3 kg VSremoved
)
Methane content (%)
below 50% and VFA accumulation (Figs. 2 and 3) as a result of decreased methanogenic activity.
Based on this study, limit concentrations to detect and prevent
digester failure during thermophilic sludge digestion are proposed
(Table 3) and discussed a follows.
2976
(a)
2.5
12
10
2.0
8
1.5
6
1.0
4
0.5
0.0
460
480
500
520
540
560
580
600
620
640
0
660
High-solids sludge
Time (d)
Alkalinity ratio (IA/TA)
Acetate
Intermediate alkalinity
(b)
2.5
Total VFA
2.0
1.5
1.0
0.5
0.0
460
480
500
520
540
560
580
600
620
640
660
Time (d)
Acetate
Propionate
iso-Butyrate
iso-Valerate
A/P ratio
Fig. 3. Volatile fatty acids (VFA) and alkalinity during thermophilic digestion of high-solids sludge: (a) total VFA (VFA C2C5), acetate concentration, intermediate alkalinity
(IA), intermediate to total alkalinity ratio (IA/TA) and intermediate to partial alkalinity ratio (IA/TA); (b) individual VFA concentration and acetate to propionate ratio (A/P).
Table 3
Limit values proposed to prevent process failure during the anaerobic thermophilic
digestion of sludge.
Parameter
Limit value
Acetate concentration (g L 1)
A/P ratio
VFA C2C5 (g COD L 1)
Intermediate alkalinity (g CaCO3 L 1)
IA/PA ratio
IA/TA ratio
Methane content in biogas (% CH4)
0.6
0.5
3.7
1.8
0.9
0.5
55
As well as individual and total VFA, some authors have proposed acetate concentration and A/P ratio as valuable indicators
to predict process failure (Marchaim and Krause, 1993; Pind
et al., 2002). For manure, an acetic acid concentration of 0.8 g L 1
and an A/P ratio of 1.4 have been proposed as limit values (Hill
et al., 1987; cited in Marchaim and Krause, 1993). To our knowledge, such limit values for thermophilic sewage sludge digestion
have not yet been proposed. In the present study, acetate concentration was usually below 0.6 g L 1 (Table 2, all periods) and only
in cases of organic overloading or temperature uctuations (due
to operating problems) did this value rise above 0.6 g L 1 and up
to 2 g L 1. Furthermore, concentrations above 1 g L 1 were only
reached when the SRT was reduced to 6 days, with OLR greater
3
d 1, as shown in Fig. 3. Therefore, a limit conthan 5 kg VS mreactor
centration of 0.6 g L 1 of acetic acid would seem more appropriate
to predict digester failure in the case of thermophilic sludge digestion. Similarly, during stability periods the A/P ratio was below 0.5
(Table 2, all periods); hence the limit A/P ratio to predict digester
failure ought to be reduced to around 0.5. From our experimental
results, it might be hypothesized that the total VFA (C2C5) concentration corresponding to these values would be around
3.7 g COD L 1, depending on the individual VFA concentration.
Such a high concentration would be detrimental to the quality of
the efuent sludge, meaning that subsequent post-treatments
ought to be considered.
3.2.2. Alkalinity
According to Ripley et al. (1986), the total alkalinity (TA) of a
sample is a result of HCO3 species, which is known as partial alkalinity (PA); and VFA, which is known as intermediate alkalinity
(IA). The latter is estimated as the difference between the TA and
PA. For this reason, the IA consists of an indirect measurement of
VFA, and the alkalinity ratios between intermediate and total (IA/
TA) or partial (IA/PA) alkalinities are alternative process indicators.
In the present study, the prole of the IA/PA ratio was indeed very
similar to that of total VFA, acetate concentration and A/P ratio in
Fig. 3; while variations in the IA/TA ratio were less pronounced. In
2977
general, the IA/PA ratio was more sensible to variations in the VFA
concentration than the IA/TA.
The correlation between total VFA (C2C5) concentration, acetate concentration or A/P ratio; and alkalinity ratios or intermediate alkalinity was further analysed (Fig. 4). Obviously, the best
correlated parameter was intermediate alkalinity, followed by IA/
PA and IA/TA ratios. The best correlations were obtained with respect to total VFA concentration (R2 6 0.79); while the correlations
with acetate concentration were very poor (R2 6 0.65) and no correlations were found with the A/P ratio (R2 0).
If threshold values were to be set in order to predict process
failure based on alkalinity measurements (which is common practise at industrial scale); the values corresponding to the aforementioned VFA C2C5 concentration of 3.7 g COD L 1 would be around
0.9 for IA/PA ratio, 0.5 for IA/TA ratio and 1.8 g CaCO3 L 1 for intermediate alkalinity.
cess may fail due to an excessively low methanogenesis rate compared to acidogenesis rate, while above 8.3 the process might be
inhibited by free ammonia (Lay et al., 1997). Ammonia inhibition
is favoured by high process temperature (Angelidaki and Ahring,
1994) and is pointed out as a major cause for low biogas production
treating pig slurries (Bonmat and Flotats, 2003).
12
10
IA/TA
y = 17.902x - 4.4868
R2 = 0.6084
IA/PA
y = 5.8407x - 1.375
R2 = 0.593
IA
y = 2.9499x - 1.5781
R2 = 0.7855
0
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
1.0
20
0.9
18
0.8
16
0.7
14
0.6
12
0.5
10
0.4
0.3
0.2
0.1
VS (g L -1)
2978
P CH4
y = 0,1481x + 0,0738
R2 = 0,964
Effluent VS
y = 1,7619x + 9,4017
R2 = 0,7789
Effluent VFA
y = 1,1516x + 0,9602
R2 = 0,9579
0.0
0
the higher the CST. Hence, it may be speculated that any increase
in efuent VS and TS resulting from changing the OLR and/or SRT
may ultimately affect digested sludge dewaterability. From the results of this study, it seems that digested sludge dewaterability
was deteriorated with TS higher than 26 g L 1 and VS higher than
3
d 1 and
17 g L 1; which corresponded to OLR above 3 kg VS mreactor
SRT below 10 days.
According to the work by Miron et al. (2000), the dewaterability
of PS worsened under acidogenic conditions (SRT 6 8 days), while
it improved under methanogenic conditions (SRT P 10 days). This
was related to a decrease in the mean particle size, thus an increase
in the total surface area, under acidogenic conditions. Moreover,
only at high SRT of 15 days was digested sludge dewaterability improved compared to that of inuent sludge. The results of the present
study are quite consistent with those ndings, since only at SRT
above 15 days was the CST value (60160 s) below that of inuent
sludge (437 s). Sludge dewaterability was worsened (CST 630
1370 s) at shorter SRT (106 days), which were typically associated
to higher efuent VFA, thus higher soluble VS. Indeed, an increasing
trend was followed by CST with respect to efuent VFA (Fig. 6c).
Some controversy exists in the literature regarding the effect of
anaerobic digestion on sludge dewaterability, and it is still not
clear whether mesophilic and thermophilic digestion has any effect
in sludge dewaterability. It has been shown that sludge dewaterability, as well as the amount of chemicals required for sludge conditioning, are directly dependant on the concentration of
biopolymer in the solution (Novak et al., 2003). Houghton et al.
(2000) and Houghton and Stephenson (2002) reported that the
composition of microbial extracellular polymer (ECP) varied after
sludge digestion and was also affected by the feed composition;
attributing excess ECP production to acidogenic bacteria. This
might also explain higher CST values obtained in the present study
in samples with higher VFA concentration, in which the presence
of acidogenic bacteria should be higher.
2979
(a)
1600
70
1400
CST (s)
1200
50
1000
40
800
30
600
20
400
60
CST/VS
y = 13.451x - 5.5537
R2 = 0.8977
CST/TS
y = 6.909x - 0.7302
R2 = 0.7831
CST
y = 301.53x - 211.01
R2 = 0.9207
10
200
0
0
(b)
1600
1400
CST/VS
y = 121.51x - 1455.1
R2 = 0.9213
CST/TS
y = 52.145x - 865.07
R2 = 0.9403
CST (s)
1200
1000
800
600
400
200
0
0
10
20
30
40
50
TS and VS (g L-1)
(c)
70
1400
60
CST (s)
1200
50
1000
40
800
30
600
20
400
CST/VS
y = 19,982x - 42,85
R2 = 0,5916
CST/TS
y = 11,598x - 24,382
R2 = 0,6591
CST
y = 428,78x - 982,56
R2 = 0,556
10
200
0
0.0
1600
0
1.0
2.0
3.0
4.0
5.0
Table 4
Microbiological analyses of inuent and efuent sludge samples.
Pathogens
E .coli (CFU mL 1)
Salmonella spp. (in 50 mL)
Inuent
Efuent (SRT)
(PS + WAS)
30 d
25 d
20 d
15 d
10 d
6d
1.0 106
Absence
Absence
Absence
Absence
Absence
Absence
Absence
1.0 101
Absence
1.0 101
Absence
1.1 102
Absence
2980
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