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Anaerobic Co-digestion of Fruit Juice and Municipal Bio-waste in

the Okanagan Valley


by

Mariel Barrantes Leiva

B.Sc. National University of Costa Rica, 2010

A THESIS SUBMITTED IN PARTIAL FULFILLMENT OF

THE REQUIREMENTS FOR THE DEGREE OF

MASTER OF APPLIED SCIENCE

in

THE COLLEGE OF GRADUATE STUDIES

(Civil Engineering)

THE UNIVERSITY OF BRITISH COLUMBIA

(Okanagan)

May 2013

© Mariel Barrantes Leiva, 2013


Abstract

Fruit harvesting and juice making is one of the most important sectors in the Okanagan
Valley. Fruit- juice production generates industrial wastewater with high organic strength
that needs to be treated, generally on-site, prior to being discharged to the municipal
wastewater treatment system. In the Okanagan Valley, the organic residuals of fruit-juice
wastewater treatment, such as screen cake and thickened waste activated sludge, are
currently being sent to local landfills or composting facilities, which is not desirable. Given
the growing interest in utilizing industrial, agricultural and municipal waste streams in
centralized bioreactors for optimized energy (biogas) recovery, this study evaluated the
anaerobic co-digestion performance of industrial organic streams from Sun-Rype Products
Ltd. wastewater treatment facility with municipal waste sludge cake from Kelowna’s
municipal wastewater treatment plant. Excess landfill leachate source at the Glenmore
Landfill was also utilized to dilute some of the concentrated streams and provided
additional buffering capacity. Both single and co-digestion scenarios were tested in
laboratory-scale mesophilic and thermophilic semi-continuous flow digesters at sludge
retention times of 20 and 10 days, corresponding to organic digester loading rates of 1.41-
4.80 g chemical oxygen demand /L/day. Digestion studies demonstrated that co-digestion
of fruit-juice streams with municipal sludge cake and leachate resulted in more stable
operation even at the higher loading due to additional buffering capacity available compare
to single scenarios. In addition, organic removal efficiencies were higher for the co-
digestion scenarios. Furthermore, dewaterability of municipal sludge cake was enhanced
by the addition of industrial secondary sludge. Thermophilic digestates could qualify under
Class A biosolids according to Organic Matter Recycling Regulation (OMRR) of BC in
terms of coliform presence; however presence of higher coliforms at mesophilic digestion
temperatires downgraded the mesophilic digestates to Class B biosolids. Finally,
ppreliminary cost analysis indicated an overall saving of $10.52 million ($2 million in
capital and $8.52 million in operational) over 25-year period for a co-digestion scenario
utilizing all waste streams over building/operating two separate digesters for municipal and
industrial waste streams.

ii
Preface

Some parts of this study were presented in 2013 British Columbia Water and Waste
Association (BCWWA) Annual Conference (April 20-24, Kelowna, BC, Canada). An
abstract has been accepted for presentation at the International Water Association (IWA)
13th World Congress on Anaerobic Digestion: Recovering (bio) Resources for the World
(June 25-28, Santiago de Compostela, Spain). A poster will be presented in 2013 II Tall
Buildings and Sustainable Cities Congress (June 22-24, San José, Costa Rica).

iii
Table of Contents

Abstract ................................................................................................................................ ii

Table of Contents ................................................................................................................iv

List of Tables ..................................................................................................................... vii

List of Figures ......................................................................................................................xi

List of Symbols and Abbreviations ................................................................................... xv

Acknowledgements ............................................................................................................xvi
Chapter 1: Introduction .................................................................................................. 1
1.1 Background and motivation................................................................................... 1
1.2 Objectives .............................................................................................................. 5
1.3 Thesis organization ................................................................................................ 6
Chapter 2: Literature review .......................................................................................... 7
2.1 Fruit juice industry in the Okanagan Valley .......................................................... 7
2.2 Treatment processes for wastewaters .................................................................. 10
2.2.1 Treatment processes for fruit juice wastewaters ........................................... 10
2.2.2 Treatment processes for raw sewage ............................................................. 13
2.3 Landfill sites ........................................................................................................ 14
2.4 Anaerobic digestion as proposed treatment ......................................................... 15
2.4.1 Hydrolysis phase ........................................................................................... 17
2.4.2 Acidogenesis.................................................................................................. 18
2.4.3 Acetogenesis .................................................................................................. 19
2.4.4 Methanogenesis ............................................................................................. 20
2.5 Control parameters of anaerobic process ............................................................. 20
2.5.1 Physical factors .............................................................................................. 20
2.5.1.1 Temperature ............................................................................................ 21
2.5.1.2 Hydraulic and solids retention time ........................................................ 21
2.5.1.3 Volumetric organic loading rate (OLR) .................................................. 22
2.5.1.4 Continuous feed ...................................................................................... 22

iv
2.5.1.5 Mixing ..................................................................................................... 23
2.5.1.6 Characteristics of the substrate ............................................................... 23
2.5.2 Chemical factors ............................................................................................ 23
2.5.2.1 pH ............................................................................................................ 23
2.5.2.2 Toxicity ................................................................................................... 24
2.5.2.3 Nutrients .................................................................................................. 24
2.6 Anaerobic co-digestion ........................................................................................ 25
2.7 Biogas as a global renewable energy ................................................................... 28
2.8 Summary.............................................................................................................. 30
Chapter 3: Materials and methods ............................................................................... 32
3.1 Industrial and municipal waste samples .............................................................. 32
3.1.1 Municipal (sewage) sludge cake ................................................................... 32
3.1.2 Industrial (fruit-juice) waste streams ............................................................. 35
3.1.3 Landfill leachate ............................................................................................ 39
3.2 Inocula samples used as digester seed and acclimation ...................................... 40
3.3 Anaerobic co-digestion studies ............................................................................ 41
3.4 Volumetric ratios for co-substrates in digester feed streams ............................... 43
3.5 Characterization of samples................................................................................. 44
3.5.1 Total solids and volatile solids ...................................................................... 45
3.5.2 Chemical oxygen demand (COD) ................................................................. 45
3.5.3 Alkalinity ....................................................................................................... 46
3.5.4 Ammonia ....................................................................................................... 46
3.5.5 Gas Chromatography for volatile fatty acids (VFAs) and biogas
composition .............................................................................................................. 46
3.5.6 Dewaterability ............................................................................................... 47
3.5.7 Total coliforms .............................................................................................. 47
Chapter 4: Results and discussion ................................................................................ 48
4.1 Characterization of raw industrial and municipal waste streams ........................ 48
4.2 Characterization of diluted industrial and municipal waste streams ................... 49
4.3 Inoculum acclimation to waste streams studied .................................................. 51

v
4.4 Effect of addition of co-digestion materials on digester performance ................ 53
4.5 Effect of addition of co-digestion materials on digester supernatant
characterization ............................................................................................................ 66
4.6 Land application of digested biosolids according to regulations ........................ 69
4.6.1 Dewaterability ............................................................................................... 70
4.6.2 Pathogens ....................................................................................................... 73
4.7 Approximate cost functions for single and co-digestion treatment
facilities ........................................................................................................................ 76
Chapter 5: Conclusions and recommendations ........................................................... 81
5.1 Conclusions ......................................................................................................... 81
5.2 Recommendations for future work ...................................................................... 82

References ........................................................................................................................... 84

Appendices .......................................................................................................................... 95
Appendix A: Calibration curves ................................................................... 95
Appendix B: Results summary of digesters fed with leachate ..................... 97
Appendix C: ANOVA Analyses .................................................................. 98
Appendix D: Heavy metals in substrates ................................................... 114

vi
List of Tables

Table 2.1 Summary of typical results of anaerobic co-digestion ...................................... 26

Table 3.1 Experimental plan for acclimation and anaerobic single and co-
digestion stages ................................................................................................ 42

Table 3.2 Characterization of samples and frequency of analysisª ................................... 45

Table 4.1 Characterizations of raw municipal and industrial waste streams


studiedª .............................................................................................................. 48

Table 4.2 Characterizations of diluted waste streams as digester feedª ............................ 50

Table 4.3 Steady state results for acclimation semi-continuous digestersª ....................... 52

Table 4.4 Inocula characteristics before and after acclimation ......................................... 52

Table 4.5 Results for semi-continuous digesters at 20 d SRT during steady


state* ................................................................................................................. 58

Table 4.6 Results for semi-continuous digesters at 10 d SRT during steady


state* ................................................................................................................. 59

Table 4.7 Characterization of industrial TWAS on sampling date and after 3


week of storage in fridge................................................................................... 65

Table 4.8 Biogas composition of single and co-digesters during steady state ................... 66

Table 4.9 Relationship between theoretical and experimental CO2 content (%)
in digester headspace ........................................................................................ 67

Table 4.10 Comparison between theoretical total ammonia toxicity limit with
measured total ammonia concentrations ........................................................... 69

Table 4.11 Summary of different substrates and digestion techniques with their
total fecal MB-poster-AD-2013-May 22-CEcoliform presence ....................... 74

Table 4.12 Approximate cost functions for solid waste treatment facilities:
single and co-digestion reactors. Based on Tsilemou and
Panagiotakopoulus, (2006) ............................................................................... 79

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Table B.1 Results for semi-continuous digesters at 20d SRT ........................................... 97

Table C.1.1 TS% removal ANOVA analyses results for temperature and sludge
retention time .................................................................................................... 98

Table C.1.2 ANOVA: two-factor with replication TS% removal results for
temperature and sludge retention time .............................................................. 98

Table C.1.3 ANOVA analysis TS% removal results for temperature and sludge
retention time .................................................................................................... 99

Table C.1.4 TS% removal ANOVA analyses results for sludge retention time
and temperature ................................................................................................. 99

Table C.1.5 ANOVA: two-factor with replication TS% removal results for
sludge retention time and temperature .............................................................. 99

Table C.1.6 ANOVA analysis removal results for sludge retention time and
temperature ..................................................................................................... 100

Table C.1.7 TS% removal ANOVA analyses results for single to co-digestion,
and sludge retention time ................................................................................ 100

Table C.1.8 ANOVA: two-factor with replication TS% removal results for single
to co-digestion, and sludge retention time ...................................................... 100

Table C.1.9 ANOVA analysis removal results for single to co-digestion, and
sludge retention time ....................................................................................... 101

Table C.2.1 VS% removal ANOVA analyses results for temperature and sludge
retention time .................................................................................................. 102

Table C.2.2 ANOVA: two-factor with replication VS% removal results for
temperature and sludge retention time ............................................................ 102

Table C.2.3 ANOVA analysis VS% removal results for temperature and sludge
retention time .................................................................................................. 103

Table C.2.4 VS% removal ANOVA analyses results for sludge retention time
and temperature ............................................................................................... 103
viii
Table C.2.5 ANOVA: two-factor with replication VS% removal results for
sludge retention time and temperature ............................................................ 103

Table C.2.6 ANOVA analysis removal results for sludge retention time and
temperature ..................................................................................................... 104

Table C.2.7 VS% removal ANOVA analyses results for single to co-digestion,
and sludge retention time ................................................................................ 104

Table C.2.8 ANOVA: two-factor with replication VS% removal results for
single to co-digestion, and sludge retention time............................................ 104

Table C.2.9 ANOVA analysis removal results for single to co-digestion, and
sludge retention time ...................................................................................... 105

Table C.3.1 TCOD% removal ANOVA analyses results for temperature and
sludge retention time ....................................................................................... 106

Table C.3.2 ANOVA: two-factor with replication TCOD% removal results for
temperature and sludge retention time ............................................................ 106

Table C.3.3 ANOVA analysis TCOD% removal results for temperature and
sludge retention time ....................................................................................... 107

Table C.3.4 TCOD% removal ANOVA analyses results for sludge retention time
and temperature ............................................................................................... 107

Table C.3.5 ANOVA: two-factor with replication TCOD% removal results for
sludge retention time and temperature ............................................................ 107

Table C.3.6 ANOVA analysis removal results for sludge retention time and
temperature ..................................................................................................... 108

Table C.3.7 TCOD% removal ANOVA analyses results for single to co-
digestion, and sludge retention time ............................................................... 108

Table C.3.8 ANOVA: two-factor with replication TCOD% removal results for
single to co-digestion, and sludge retention time............................................ 108

ix
Table C.3.9 ANOVA analysis removal results for single to co-digestion, and
sludge retention time ....................................................................................... 109

Table C.4.1 CH4% ANOVA analyses results for temperature and sludge
retention time .................................................................................................. 110

Table C.4.2 ANOVA: two-factor with replication CH4% results for temperature
and sludge retention time ................................................................................ 110

Table C.4.3 ANOVA analysis CH4% results for temperature and sludge retention
time ................................................................................................................. 111

Table C.4.4 CH4% ANOVA analyses results for sludge retention time and
temperature ..................................................................................................... 111

Table C.4.5 ANOVA: two-factor with replication CH4% results for sludge
retention time and temperature ....................................................................... 111

Table C.4.6 ANOVA analysis removal results for sludge retention time and
temperature ..................................................................................................... 112

Table C.4.7 CH4% ANOVA analyses results for single to co-digestion, and
sludge retention time ....................................................................................... 112

Table C.4.8 ANOVA: two-factor with replication CH4% results for single to co-
digestion, and sludge retention time ............................................................... 112

Table C.4.9 ANOVA analysis removal results for single to co-digestion, and
sludge retention time ....................................................................................... 113

Table D.1 Comparison of OMRR heavy metals criteria with calculated


concentration for single and co-digested thermophilic effluents at 10-
d SRT .............................................................................................................. 114

Table D.2 Comparison of OMRR heavy metals criteria with calculated


concentration for single and co-digested mesophilic effluents at 10-d
SRT ................................................................................................................. 116

x
List of Figures

Figure 1.1 Waste streams of the present study case and their respective treatment plant
source (SC: screen cake; TWAS: thickened waste activated sludge) ................. 2

Figure 1.2 Anaerobic digestion schema process ................................................................... 3

Figure 1.3 Glenmore Landfill proposed scenario.................................................................. 5

Figure 2.1 Fruit juice line production (UF: ultra-filtration). Based on Sanchez et al.
(2009); Fellows and Dillon (1995); ..................................................................... 9

Figure 2.2 Typical biological wastewater treatment plant flow diagram. Adapted
from: Droste (1997), Davis and Cornwell (2008), and Tchonobaglous et al.
(2004) ................................................................................................................ 11

Figure 2.3 Main processes for anaerobic digestion of sludge, ending in methane
production (adapted from Droste, 1997) ........................................................... 16

Figure 2.4 Hydrolysis of the different biopolymers presents in organic matter


(adapted from Droste, 1997) ............................................................................. 17

Figure 2.5 Acidogenesis general chemical reactions (adapted from Droste, 1997) ........... 18

Figure 2.6 Different reactions involved during acetogenesis phase (adapted from
Droste, 1997) ..................................................................................................... 19

Figure 2.7 Methanogenesis main chemical reactions (adapted from Droste, 1997) .......... 20

Figure 3.1 Kelowna Water Pollution Prevention Center process flow diagram (DAF:
dissolved air flotation) ....................................................................................... 33

Figure 3.2 Brandt’s Creek Tradewaste Treatment Plant process diagram (MLSS:
Mixed liquor suspended solids)......................................................................... 37

Figure 3.3 Glenmore Landfill process flow ....................................................................... 39

Figure 4.1 Daily biogas productions (@STP) of anaerobic digesters fed with diluted
sewage sludge cake (1), Thickened waste activated sludge (2), 1+2+L
xi
(leachate), and 1+2+SC+L (screen cake). A) Mesophilic digesters, B)
Thermophilic digesters ...................................................................................... 55

Figure 4.2 Specific daily biogas productions (@STP) of anaerobic digesters fed with
diluted sewage sludge cake (1), Thickened waste activated sludge (2),
1+2+L (leachate), and 1+2+SC+L (screen cake). A) Mesophilic digesters,
B) Thermophilic digesters ................................................................................. 56

Figure 4.3 A) Total solids removal efficiencies at sludge retention times (SRTs) of 20
and 10 days. B) Comparison of TS removal between 20d SRT mesophilic
digesters (data represent the arithmetic mean of duplicates and error bars
represent standard deviations, SRT: sludge retention time, TS: total solids) ... 61

Figure 4.4 A) Volatile solids removal efficiencies at sludge retention times (SRTs) of
20 and 10 days. B) Comparison of VS removal between 20d SRT
mesophilic digesters (data represent the arithmetic mean of duplicates and
error bars represent standard deviations SRT: sludge retention time, VS:
volatile solids) ................................................................................................... 62

Figure 4.5 A) Total chemical oxygen demand removal efficiencies at sludge retention
times (SRTs) of 20 and 10 days. B) Comparison of TCOD removal
between 20d SRT mesophilic digesters (data represent the arithmetic mean
of duplicates and error bars represent standard deviations SRT: sludge
retention time, TCOD: total chemical oxygen demand) ................................... 64

Figure 4.6 Dewaterability analysis results of single and co-digested samples (data
represent the mean and error bars represent the standard deviation of 9
replicates, SRT: sludge retention time, TS: total solids) ................................... 72

Figure 4.7 SCOD analysis results of single and co-digested samples (data represent
the mean and error bars represent the standard deviation of 74 and 38
replicates for 20 and 10 days SRT, respectively, SRT: sludge retention
time, SCOD: soluble chemical oxygen demand) .............................................. 72

xii
Figure 4.8 Coliform content of effluents from anaerobic digesters, at 20 d and 10 d
SRT with Class A limit regulation (data represent the mean and error bars
represent the standard deviation of 8 replicates, SRT: sludge retention
time, MPN: most probable number, TS: total solids) ....................................... 76

Figure 4.9 A) Initial and B) operating cost functions of anaerobic digestion facilities
(adapted from Tsilemou and Panagiotakopoulus, 2006) ................................... 77

Figure A.1 Calibration curve for biogas measurement via manometer (STP) .................... 95

Figure A.2 Calibration curve for COD determination ........................................................ 95

Figure A.3 Calibration curve for ammonia (NH3-N) determination ................................... 96

Figure A.4 Calibration curve for total nitrogen (TN) determination ................................... 96

xiii
List of Illustrations

Illustration 3.1 Sewage sludge cake before and after dilution ............................................. 35

Illustration 3.2 A)Screen cake obtained from the Salsnes screen. B) Thickened
waste activated sludge obtained from the top of the dissolved air
flotation tank at the Brandts Creek Tradewaste Treatment Plant .............. 38

Illustration 3.3 A) Eight semi-continuous digesters (four thermophilic and four


mesophilic). B) Digester configuration 1: Effluent port, 2: Biogas
exit, 3: Influent port, and 4: tedlar bag ....................................................... 43

xiv
List of Symbols and Abbreviations

BCTTP Brandt’s Creek Tradewaste Treatment Plant

COD Chemical oxygen demand

CST Capillary suction time

DAF Dissolved air flotation

L Leachate

M Mesophilic

MLSS Mixed liquor suspended solids

OMRR Organic Matter Recycling Regulation

OLR Organic loading rate

SC Screen cake

SRT Sludge retention time

T Thermophilic

TS Total solids

TWAS Thickened waste activated sludge

UASB Upflow anaerobic sludge blanket

VFA Volatile fatty acids

VS Volatile solids

WWTP Wastewater treatment plant

xv
Acknowledgements

I would like to express my sincere gratitude to my supervisor, and my friend, Dr. Cigdem
Eskicioglu. Without her guidance and encouragement, the completion of this degree
would not have been possible. I have been touched by her kindness as she guided me
through my academic journey, as well as many everyday life experiences.

The amazing staff and faculty at UBCO made my academic life experience full of special
memories. I am deeply indebted to Ms. Teija Wakeman, Ms. Karen Seddon, Dr. Steven
O’Leary, Dr. Richard Klukas, Dr. Solomon Tesfamariam and Dr. Kasun Hewage. You
surely made my academic experience unforgettable. Moreover, I am thankful to my
research group, especially to those with whom I spent most of my time: Hanna Hamid,
Kafi Wahidunnabi, Piero Galvagno, and Tim Abbot.

My fellow schoolmates and friends for life: Jessica Buriticá, Arnaud Houriet, Weronika
Michalska, Haibo Feng, Renee Leboe (and family), Courtney Dean, Karen Robles, and
Atul Porwal. Thank you for your continuous help, love, and encouragement

I cannot finish without thanking Fabricio Bianchini, the person who changed my life
forever. You came along and filled my world with love and dreams. This chapter of my
life would not be the same without you. Friends are the family that you choose: Shani
Bishop, Molly, Matt and Angus Thurston you truly are my family. Your love and
kindness made my stay in Canada extraordinary.

My friends from Costa Rica: Maureen and Kattia. Your constant care and love from far
away has a special place in my heart. My infinitive gratitude goes to my family, specially
my mom, my grandparents and Aunty Yen. You are my everyday source of inspiration
that helps me reach my greatest dreams. You are my world, my happiness, and my life.
Lastly, I would not have made this far without God being the head of my life. Thank you
God for all these blessings.

xvi
Dedication

To my parents
Quintín, Ana & Denise

xvii
Chapter 1: Introduction

1.1 Background and motivation

Fruit harvesting is one of the most important agricultural activities in the Okanagan Valley.
Within the City of Kelowna, 22,095 acres of land is zoned for agricultural land use
(Planning and Development Services, 1998). As the City of Kelowna population grows,
food and juice businesses are rapidly expanding to meet the increasing demand. Juice
production generates a relatively low volume of wastewater compared to domestic
wastewater but has high organic content (El-Kamah et al., 2010).

Fruit juice production residues consist of bagasse, marc and lees from decanting steps
(Devesa-Rey et al., 2011). The mixed waste stream is characterized by low pH and high
macronutrient (i.e., sugars, cellulose) concentration (Point, 2008).

In addition to fruit juice industrial wastewater, municipal wastewater also needs to be


treated according to provincial and federal regulations before it is discharged to surface
water (i.e., lake or river). Brandt’s Creek Tradewaste Treatment Plant (BCTTP) was built to
process the wastewater coming from the local fruit juice industry. The three major effluents
from treatment site are: screen cake (SC), thickened waste activated sludge (TWAS), and
treated wastewater; which is discharged to the domestic wastewater treatment plant
(WWTP) for further treatment.

Sewage treatment generally is subject to local, provincial and federal regulations and
standards. The City of Kelowna, with a population of 150,000, operates a WWTP, called
Kelowna Water Pollution Control Center, that daily produces high volumes of dewatered
sewage sludge cake (60,000 L/d, with 17.5% total solids), also called “biosolids” after
stabilization via composting. Due to the large production of biosolids, environmental
policies encourage the practice of biosolids disposal via addition to soil as final disposal
(Furlong et al., 2010). Figure 1.1 shows the different treatment sites and the waste streams
(substrates) coming from these sites, studied in this research.

1
The City of
Kelowna

Kelowna Water Brandt's Creek


Glenmore
Pollution Control Tradewaste
Landfill
Center Treatment Plant

Sewage sludge
Fruit juice TWAS Fruit juice SC Leachate
cake

Figure 1.1 Waste streams of the present study case and their respective treatment plant
source (SC: screen cake; TWAS: thickened waste activated sludge)

Current disposal of waste sludge (from municipal and fruit juice wastewater treatment) is
via composting at the Regional Compost Facility in Vernon, BC. Composting can have a
large number of adverse impacts. Composting can pollute the local environment and cause
an uncontrolled release of methane that is generated by the decay of organic waste (Ni et
al., 1993). Leaching is an important factor of nutrient losses from compost. For instance, it
is estimated that 20 to 40% of the loss of the nitrogen (N) and 42 to 62% of loss of carbon
(C) present in the waste occurs during composting (Tiquia et al., 2002). If the run-off from
the composting facility is not controlled, the organometallic compounds present in the
compost leachate have been shown to affect the groundwater. The water run-off from
Glenmore Landfill is controlled at the Kelowna Water Pollution Control Center.

Anaerobic systems can be used as part of the process to treat bio-waste and sewage sludge.
Anaerobic digestion is an enclosed waste treatment system, reducing biogas emissions into
the atmosphere. Figure 1.2 shows anaerobic digestion life cycle: from organic waste to
biogas production, water recycling in the system, and the utilization of digestate as

2
fertilizer. It has been shown that the biogas can be generated at a much faster rate in
engineered bioreactor systems. Biogas production can be converted into reusable energy
either for heating or electricity generation. The digester remaining content (digestate) will
have a reduced organic strength and will be less odorous (Moody et al., 2009). Digestate
comes from acidogenesis and methanogenesis of anaerobic digestion. From acidogenesis,
digestate could contain lignin and cellulose. From methanogesis phase, digestate would be
high in nutrient content, i.e., nitrates and phosphates (Evans et al., 2009). Moreover,
digestate will have a higher nutrient content than undigested solids, which makes it
particularly desirable for use as fertilizer or soil amendment.

Figure 1.2 Anaerobic digestion schema process

The Regional Compost Facility is approaching its maximum capacity. Expanding the
different facilities could be an easy way to fix this problem. However, the City of Kelowna
is trying to reach a goal of becoming carbon neutral by the year of 2020. Therefore, the
purpose of this research was to find a sustainable disposal method that combines all organic
waste streams coming from the facilities operated by the City of Kelowna in a potential
anaerobic co-digestion system.

3
There is plenty of information about aerobic and anaerobic reactor systems for treating
wastewater generated from WWTPs of juice, brewery and distillery industries (Ozbas et al.,
2006; Ahn et al., 2001; El-Kamah et al., 2010). Studies of anaerobic co-digestion systems
are limited, especially for waste sludge and other organic residues from juice production
with municipal waste. Recent studies indicate that co-digestion (simultaneous digestion of a
mixture of substrates) improves both the biogas yield, and stability of a digester. Positive
synergistic effects are mainly due to supply of missing nutrients by different substrates to
anaerobic co-digester (Ni et al., 1993).

Anaerobic co-digestion has a lower cost to benefit ratio compared to the single digestion
(Ozbas et al., 2006). Sharing equipment and utilizing free volume capabilities in existing
digesters are the main reason for a lower cost to benefit scenario. Moreover, co-digestion
achieves balancing nutrient content. Since both of the organic residues from juice
production (i.e. SC and TWAS) are high in carbohydrate (carbon) content, both substrates
would be good candidates for co-digestion with other substrates having much lower carbon
to nitrogen (C:N) ratios, such as domestic (municipal) sewage sludge.

The main motivation for this research was to reduce the environmental impact due to the
disposal of waste solids by combining domestic and industrial wastewater by-products to
produce methane. Compared to the single-substrate traditional methods (anaerobic single
digestion), the combination of different sources of waste would not negatively impact
methane production. Moreover, the combination of domestic and industrial waste solids
increases the methane production capacity, which can be used as a source of renewable
energy. Hence, this approach to sludge treatment process has potentially positive impacts.

A prospective place to build an anaerobic co-digester is at the Glenmore Landfill, located in


Kelowna, BC, due to reasons explained in Chapter 3 in detail. Figure 1.3 shows a proposed
scenario for the Glenmore Landfill incorporating an anaerobic co-digester that uses the
excess landfill leachate as dilution water for the dewatered sludge cake, and connects the
biogas generated from the co-digester to the biogas utilization system already on-site. This
landfill produces leachate, part of which is currently re-circulated in Phase 1 of the site to
enhance the generation of methane-rich landfill gas. Currently, the landfill gas is either
flared or converted to electricity, enough to power 70 homes (City of Kelowna, 2013).
4
Excess leachate is currently being pumped to the Kelowna WWTP. This excess of leachate
could be used as a source of dilution water and alkalinity for the future anaerobic co-
digester.

Figure 1.3 Glenmore Landfill proposed scenario

With the background information presented, the scope of this project was to assess the
single, as well as co-digestion potential of four organic waste streams (fruit juice SC, fruit
juice wastewater TWAS, sewage sludge cake and landfill leachate) in laboratory-scale
anaerobic digesters operated for 7 months. Analysis of centrifuge system of digestate
material for soil amendment preparation and phosphorous recovery (shown in Figure 1.3)
were not part of this study.

1.2 Objectives

The main objective of this project was to evaluate the potential yield of an anaerobic co-
digester utilizing four waste streams coming from the municipal and industrial (fruit juice)
WWTPs in the City of Kelowna. In addition, the effect of the C:N present in co-digestion

5
was also investigated. Laboratory-scale mesophilic and thermophilic single and co-
substrate anaerobic digesters were operated at sludge retention times of 20 and 10 days to
assess the specific performance criteria listed below:

Specific biogas (methane) yield, digestibility, and co-digestibility of each waste

Organic removal efficiencies

Volatile fatty acids accumulation and ammonia inhibition

Coliform content of digested biosolids (digestate) and dewaterability to assess


fertilizer reuse

Upon completion of laboratory work, the data obtained were used to determine the organic
loading rate, retention time and reactor volume requirement values that would later be used
in the design of an anaerobic co-digester.

1.3 Thesis organization

This thesis has been organized into five chapters. In the first chapter, the background and
motivation of this study case are provided. Objectives of the research are also presented in
Chapter 1. The second chapter provides a summary of relevant literature, including
WWTPs treating raw sewage and fruit juice wastewater, sludge features, and anaerobic co-
digestion. In Chapter 3, the materials and methods for this research are documented,
including a description of each substrate, and equipment and instrumentation used.
Characterization methods and experimental procedures are described in Chapter 3 as well.
Chapter 4 presents the results and discussion of the experimentation. The experimental
summary data from the lab-scale digesters are presented and compared with literature
results. Lastly, Chapter 5 concludes the thesis by compiling a summary of the results
obtained in this study and presents recommendations for future work.

6
Chapter 2: Literature review

2.1 Fruit juice industry in the Okanagan Valley

In the Okanagan Valley, many different types of fruits such as grapes, apples, cherries and
pears are produced. A growing agricultural sector in the Okanagan Valley has allowed juice
and wine production companies to become established in the area. One of the largest fruit
juice processors in Western Canada is located in the Okanagan Valley. Fruit juice
production generates industrial wastewater that needs to be treated, generally on-site, prior
to being discharged to the municipal wastewater collection and treatment system.
Understanding the fruit juice production line can provide context to characterization of fruit
juice residues.

Fruit-juice process begins after fruit harvest and finishes in the storage and transport of the
fruit juice. A typical fruit juice production line is shown in Figure 2.1 as a process diagram.
Fruit harvest is the first step of the process flow. After the fruit is collected, it is transported
to an industrial plant. The fruit juice process begins once all of the fruit is received at the
process plant. This stage consists of several phases.

The first phase for factory procurement is inspection. All good fruit is separated for quality
control. Fruits with good color and size are selected, while fruits with bruising and/or mold
are discarded. The next stage is fruit sorting. Contaminants and substandard fruit are
removed in this stage. The following step is washing and preparation. The rinse water for
washing apples is collected, and it is connected to the wastewater effluent system.
Depending on the final product, slicing and pre-filtering is also required (Food and
Organization of the United Nations, 2001).

The second phase consists of grinding and mashing the fruit. More rinse water is used as
well as some enzymes. Enzymes added to fruit juice are necessary for pressing. These
enzymes will increase the breakdown of cellulose, making an efficient pressing system
(Ribeiro et al., 2010; Food and Organization of the United Nations, 2001). Whole fruits are
milled and treated with enzymes prior to pressing to loosen cell walls and promote the free
running of the juice. After pressing, the juice is transferred to clarification tanks where an
additional enzyme is added to the juice to depectinize and hydrolyze starch prior to

7
filtration. Enzymes added are inactivated during pasteurization of the juice (Ribeiro et al.,
2010).

The majority of the liquid coming from fruit pressing is used for the juice-batch
preparation. The leftover pulp is sent to a centrifuge. The centrifuge is used to extract more
juice from the pulp and the rest of the fruit (Fellows and Dillon, 1995). The centrifuge and
pressing stages produce two effluent streams: raw leachate and raw juice (waste effluent).
Later on the process, raw leachate will be connected with the main waste stream system.

The third phase is the batch preparation. By rotary screenings, this phase involves mixing
the fruit juice with the additives. Additives will vary depending on the final product. The
batch preparation produces another waste stream.

After the additives addition, the line production is divided into two. One line is connected
to the refining system. The second line from additives-batch preparation is connected to
ultra-filtration. After these processes are completed, the filtered liquid from both processes
(ultra-filtration and refining system) are combined in the pasteurization batch.
Pasteurization is a mandatory process specified by Canadian Food Inspection Agency
regulations (Canadian Food Inspection Agency, 2012). Each procedure (ultra-filtration and
pasteurization) produces waste that contains a high amount of solids. Waste residues
coming from ultra-filtration are highly contained with macronutrients such as cellulose and
lignin. From pasteurization procedures, the proteins are expected to be present in the waste
stream (Ribeiro et al., 2010). The final phases of the procedure are the aseptic filling of the
juice into the proper containers and storage of the final product (Sanchez et al., 2009).

8
Figure 2.1 Fruit juice line production (UF: ultra-filtration). Based on Sanchez et al. (2009); Fellows and Dillon (1995);

and Food and Organization of the United Nations (2001)

9
Approximately 70% of fruit juice industry raw materials are fruit. The other 30% of raw
materials are water, enzymes, sugar, and specific chemical toppings. Therefore, the juice
production generates waste streams with high organic concentration. Wastewater that
comes from fruit juice industries has high concentrations of sugars and carbohydrates,
among other organic compounds. Due to the presence of a high organic content in the
wastewater, a biological treatment process in the WWTP is preferred.

2.2 Treatment processes for wastewaters

2.2.1 Treatment processes for fruit juice wastewaters

A biological treatment is preferred if the influent wastewater composition has


biodegradable pollutants such as sugars, proteins, yeast, filter-aid, and soluble starch. US
Environmental Protection Agency (EPA) and Canadian Department of the Environment
declare that organic wastewater effluents need to be treated under physical or biological
systems (U.S. Environmental Protection Agency, 2004; Environment Canada, 2010). For
fruit juice biological wastewater treatment, processes are based on the microorganisms’
metabolic activity. Biological metabolisms occur in the secondary phase of the WWTP,
following preliminary (screening, equalization) and primary treatment (primary
sedimentation).

In addition to pollutants listed above (section 2.1), wastewaters produced from fruit juice
production consist of the following: wastewater from cleaning containers, rinsing and
washing water, exhaust vapor condensate, wastewater from production facilities,
wastewater from surface cleaning and from cleaning conveyor facilities (Rosenwinkel et
al., 2005). Different biological treatment processes can be used to achieve a higher removal
of biological oxygen demand. These treatments can be applied directly or can be combined
with each other. Figure 2.2 shows a typical fruit juice industry WWTP system.

10
Figure 2.2 Typical biological wastewater treatment plant flow diagram. Adapted from:
Droste (1997), Davis and Cornwell (2008), and Tchonobaglous et al. (2004)

In addition to high organic strength, another challenge with treating this industrial stream is
high fluctuations. Naturally, fruit juice production waste changes depending on the process
and products that are being used (Trnovec and Britz, 1998). Furthermore, significant
variations in daily/weekly/seasonally effluent discharge load and concentration in
biological or chemical oxygen demand (COD) are typical as well (Ozbas et al., 2006). All
these pollutants are capable of disrupting the ecological equilibrium in water bodies causing
eutrophication and increasing turbidity (Droste, 1997). Moreover, the growing concern over
the quality of water enforced a higher pollution reduction on treatment facilities. Therefore,
biological treatment is preferred as the most optimal solution for treating wastewaters and
solid by-products coming from fruit juice factories (Koevoets et al., 2002; Trnovec and
Britz, 1998).

The use of product and product additives (like sugar which is often added) contributes to a
significant amount of the wastewater pollution from the fruit juice industry. The COD of
fruit juices ranges from about 50 g/L (tomato juice) to about 200 g/L (apricot juice).
Moreover, 1 kg of glucose (or of fructose) is equivalent to 1066 g COD. Besides the
wastewater, the fruit juice industry also produces cooler sludge, filtration residues, sludge
from clarifying agents, and pomace (Rosenwinkel et al., 2005).

In order to meet the discharge limits of the municipal sewer system, it is often necessary to
equalize the pH peaks and sometimes to reduce the temperature. Requirements of treated

11
wastewater disposal in terms of pH and temperature are 6.5-9, and 15oC, respectively
(Ministry of Environment, 2012). Thus, a fruit juice wastewater pretreatment plant starts
with a neutralization stage. Because of the high cost of chemicals, biological neutralization
is usually recommended (e.g., in an aerated mixing and equalizing tank). Equalization tanks
can achieve biological oxygen demand elimination between approximately 35% in daily
basis, and greater than 50% weekly equalization basis (Rosenwinkel et al., 2005).
Furthermore, equalization tanks overcome the operational problems, and flow rate
variations, to improve the processes and to reduce the size and cost of downstream
facilities.

Aerobic and anaerobic biological processes are used worldwide to treat sewage and
wastewater coming from fruit juice industry. To achieve a good performance, use of biota
is necessary (Kadam et al., 2008). Microorganisms like eukaryota and protozoa are mostly
used to consume all of the organic matter present in the wastewater (U.S. EPA: Primer for
Municipal Wastewater Treatment Systems). Ideally, biota requires a minimum specific
ratio of nutrients of 20:1 (C:N) to achieve full removal of COD in a biological treatment
system (Grady et al., 1999). The main role of the microorganisms is to transform the
dissolved and particulate biodegradable matter into acceptable end-products by capturing
and incorporating suspended and non-settleable colloidal solids into the biological floc
(biosolids). Additionally, these microorganisms transform and remove nutrients by
removing specific trace organic constituents and compounds (Tchobanoglous et al., 2004).

According to Rosenwinkel et al. (2005), for direct discharge into waterways, the activated
sludge system with cascade design has proved to be viable for the fruit juice industry.
Cascade sludge system was operated at sludge loads of greater than 0.1 kg biochemical
oxygen demand / mixed liquor suspended solids (MLSS) kg × day. Due to low nitrogen and
phosphorous amounts in the raw wastewater, it was necessary to add nutrients. In general,
fruit juice industrial wastewaters have such low nitrogen and phosphorous concentrations
that it is often necessary to add urea and phosphoric acid as a nutrient supplement. The
nutrient addition helps to achieve the minimum nutrient ratio for growth of the
microorganisms that are required for the biodegradation of waste (Rosenwinkel et al., 2005;
Ozbas et al., 2006).

12
Another alternative treatment system is the upflow anaerobic sludge blanket reactor
(UASB). Upflow systems are high-rate anaerobic reactors developed and successfully
applied in recent years for the biological treatment of effluents, and in particular those from
the food processing industries (Lettinga et al., 1997). An example of UASB is the
Biothane® UASB/ Biobed® expended granular sludge bed anaerobic pre-treatment process
in combination with an Aerothane Flash-Aeration purification (Rosenwinkel et al., 2005).
This biological treatment achieved 70 – 90% COD removal from fruit juice effluents.

Tawfik and El-Kamah (2011) studied the performance of anaerobic hybrid reactor followed
by sequencing batch reactors in order to treat fruit juice industry wastewater. The anaerobic
hybrid reactor achieved up to 42% COD removal, and 56% total suspended solids removal.
The sequencing batch reactors achieved up to 67% COD reduction.

2.2.2 Treatment processes for raw sewage

Similar to industrial wastewater treatment, the municipal wastewater (sewage) treatment is


also subject to local, state and federal regulations and standards. The process for removing
pollutants in municipal wastewater has physical, chemical, and biological stages.
Preliminary (physical) treatments are screening and grit removal. Screenings are used to
retain solids found in the raw sewage. Moreover, grit removal is another preliminary
treatment and aims to remove grit, sand, gravel, sanders, or heavy materials (Droste, 1997).
The following stage is sedimentation (primary) stage. In this stage, the wastewater is held
in static basin, called primary setting tank, which allows solids to settle to the bottom while
the oil, grease, and lighter solids remain floating. The secondary stage removes dissolved
and suspended biological matter that is typically performed by indigenous, water-borne
microorganisms in a managed habitat. Tertiary treatment, a phase in addition to primary
and secondary treatment, allows for disposal into a highly sensitive ecosystem (Kadam et
al., 2008).

Primary settling tanks are usually equipped with mechanically driven scrapers. Mechanical
systems drive the collected sludge towards a hopper in the base of the tank where it is
pumped to sludge treatment facilities (Tchobanoglous et al., 2004). Microorganisms are the

13
biological engines to minimize the organic matter in activated sludge processes. A variety
of microorganisms helps to convert colloidal and dissolved carbonaceous organic matter
into various gasses as well into protoplasm (Droste, 1997). This stage is designed to be
effective in reducing the amount of biodegradable soluble organic contaminants present
(i.e. sugars, fats, organic short-chain carbon molecules).

Biosolids (stabilized waste sludge) are the largest by-product resulting from wastewater
treatment processes. Biosolids production amount and total solids (TS) concentrations may
vary based on the treatment used, source of the wastewaters, and the method of dewatering
(if used). As an example: domestic biosolids generated from two-phase centrifugation
system, in Castilla, La Mancha (Spain) has approximately 17.9% TS (Fernandez et al.,
2010). Annual productions may vary according to the city population and WWTP capacity.
Another example is, the Annacis Island WWTP (Greater Vancouver Regional District),
with a population of 1,000,000, is producing 39,000 tonnes/year dehydrated (30%) waste
sludge (Metro Vancouver, 2008).

Because of the large production volumes of biosolids, environmental policies, such as BC


Ministry of Environment Organic Matter Recycling Regulation (OMRR), encourage the
practice of biosolids disposal via addition to soil. However, disposal policies for soil and
water conservation have not been well implemented in many countries.

The City of Kelowna relies on biological treatment as an integral part of its municipal
wastewater treatment system. Excess solids residuals (or biosolids) are produced as part of
the primary and secondary treatment. Currently, the biosolids are dewatered and hauled to
the Kelowna-Vernon District Compost Facility.

2.3 Landfill sites

A landfill is a disposal site for solid waste materials, i.e. household waste,
construction/demolition waste, waste from streets. Landfills are based on several sprayed-
on layers of wastes and biosolids, which are blankets. Generally, these layers of waste are
covered with soil layers. This cure site confines, compacts and covers the waste (Borongan
and Okumura, 2010). This waste disposal method has many negative impacts, some of
14
which include the release of odour and gasses, the production of leachate, bacteria and
fungi growth, and the potential to convey heavy metals to the soil (Aggelides and Londra,
2000).

A major waste stream coming from Glenmore landfill operation in the Okanagan Valley is
the leachate. Currently, part of the leachate is being re-circulated to provide moisture to the
solid waste pile through the landfill gas collector pipes. The remaining leachate is pumped
to the Kelowna WWTP. The future goal is to recirculate 100% of the leachate in the
Glenmore Landfill, avoiding the pumping of leachate off-site to the WWTP. This procedure
enhances decomposition, creating more methane for electrical generation and more space
for future landfilling. The Glenmore Landfill is currently operating according to a plan
called the Landfill Gas Management Program. This program aims to collect the methane
gas produced by the landfill to run three microturbines to generate electricity (Glenmore
Landfill: City of Kelowna, 2012). All regulated landfills are required to design and install a
gas collection system from the landfill site. In addition, Ministry of Environment under
Landfill Gas Management Facilities Design Guidelines, declares that all landfill gas
captured must undergo into reduction, whether by flaring, gas utilization for electricity
generation, fuel, etc. (Conestoga-Rovers, 2010).

The population growth in the Okanagan Valley may necessitate future upgrades at the
Glenmore landfill. The alternatives to these upgrades are waste reduction, recycling/reusing
strategies, or aerobic or anaerobic biological treatment of organic waste streams currently
being sent to the landfill, such as organic portion of kitchen waste. Anaerobic digestion can
be a good candidate for biogas generation from the waste streams with high organic
strength, such kitchen waste and municipal and industrial waste sludge. This treatment can
be applied after a sorting process in order to remove the unwanted materials (Fruteau de
Laclos et al., 2008).

2.4 Anaerobic digestion as proposed treatment

Anaerobic digestion processes are used for turning high-strength organic waste, such as
manure, food scraps, sewage and industrial treatment sludge (biosolids), into usable energy

15
in the form of biogas (methane and carbon dioxide). Additional benefits of the process
include diverting waste from landfills and reducing pathogens, odour and greenhouse gas
emissions.

The anaerobic digestion of complex organic waste is composed of four bio-chemical


reactions, performed in the following order: hydrolysis, acidogenesis, acetogenesis and
methanogenesis. This process is summarized in Figure 2.3. Each process is discussed in the
following sub-section.

Figure 2.3 Main processes for anaerobic digestion of sludge, ending in methane production
(adapted from Droste, 1997)

16
2.4.1 Hydrolysis phase

The first process in anaerobic digestion is hydrolysis where the complex organic matter is
broken down to simpler organics by different communities of microorganisms (Powrie,
2011). These microbial communities will break down the polymeric chains of organic
matter by using their extracellular enzymes. The major microbial group for this stage will
be hydrolytic fermentative bacteria (Powrie, 2011; Demirel and Scherer, 2008). Hydrolysis
will produce sugars, fatty acids, and volatile fatty acids (VFAs), amino acids, and some
other organic monomers as shown in Figure 2.4. The rate of hydrolysis stage will determine
the whole anaerobic process as it is the slowest process especially for the highly complex
waste (Neyes and Baeyens, 2003).

Figure 2.4 Hydrolysis of the different biopolymers presents in organic matter (adapted from
Droste, 1997)

17
2.4.2 Acidogenesis

Acidogenic fermentative bacteria will turn the monomers that were broken down in the
previous stage, into their respective acids (Figure 2.5). In this stage, VFAs are produced
along with ammonia, carbon dioxide, hydrogen sulfide, and other products (Demirel and
Scherer, 2008).

Figure 2.5 Acidogenesis general chemical reactions (adapted from Droste, 1997)

The VFAs present in the system will increase the acid concentrations, which can lead to
poor sludge degradation performance. Furthermore, acid production will lead to
acetogenesis, which is a key part of the anaerobic system. The acetogenesis process will
decrease the VFAs concentration, which allows for pH neutralization and keeps the
microorganisms alive in the digesters (Grady et al., 1999).

18
2.4.3 Acetogenesis

Acetogenesis is the third stage of sludge digestion. The reaction digests the acid molecules
through acetogens. The process will produce acetic acid, carbon dioxide, and hydrogen.
The acetogenic bacteria will perform several reactions only in the presence of alcohols and
acids monomers (Figure 2.6). Therefore, the acetogens need syntrophic bacteria. Also,
acetogens depend on an effective inter-species hydrogen transfer (Demirel and Scherer,
2008). It is expected that, after acetogenesis, there will be minimum of acids in the system.
The final step for the digestion of organic matter is methanogenesis.

Figure 2.6 Different reactions involved during acetogenesis phase (adapted from Droste,
1997)

19
2.4.4 Methanogenesis

Methanogenic bacteria are physiologically identified by their methane production


capability. Additionally, other substances such as carbon dioxide, water, hydrogen sulfide,
and other less complex organic matter are produced. In this process, acetate will be
converted into methane while the hydrogen and carbon dioxide are consumed, as presented
in Figure 2.7. Many physical-chemical parameters such as pH and nutrients are required to
achieve an optimal performance (Grady et al., 1999).

Figure 2.7 Methanogenesis main chemical reactions (adapted from Droste, 1997)

2.5 Control parameters of anaerobic process

Efficient digester performance depends on maintaining healthy bacteria populations. The


inactivity of any bacteria population can inhibit the activity of the other groups. The
performance and activity of methanogens are particularly important for methane (CH4)
production. This is because methanogenic microorganisms are more sensitive to changes in
the environmental conditions as discussed below (Demirel and Scherer, 2008).

2.5.1 Physical factors

From process loading to operational factors, there are many factors that affect the
performance of anaerobic treatment systems. Sludge retention time (SRT), hydraulic
retention time, organic loading rate (OLR), and hydraulic loading rate represent the main
process loading factors. Operational factors can be mixing regime (complete-mixed or plug

20
flow) and the characteristics of the substrate. To successfully design and operate an
anaerobic treatment system, it is critical that these factors are understood and managed.

2.5.1.1 Temperature

Anaerobic processes strongly depend on temperature. The anaerobic conversion of organic


matter has its highest efficiency at a temperature 35-40°C and about 55°C for mesophilic
and thermophilic conditions, respectively. However, anaerobic processes can still operate in
a temperature range of 20-45°C without major changes in the microbial ecosystem (Cuetos
et al., 2011). Enzymatic activity is enhanced at higher temperatures.

2.5.1.2 Hydraulic and solids retention time

Hydraulic retention time and SRT are two other important design parameters in biological
treatment processes. Hydraulic retention time indicates the time the waste remains in the
reactor in contact with the biomass. The time required to achieve a given degree of
treatment depends on the rate of microbial metabolism. Wastes containing simple
compounds such as sugar are readily degradable and require low retention times, whereas
complex wastes are slowly degradable and need longer hydraulic retention time to be
metabolized (Khanal, 2008).

SRT, on the other hand, controls the performance of anaerobic processes. SRT represents
the time that the biomass (acid and methane forming microorganisms) spends in the reactor.
Therefore, maintaining a high SRT produces a more stable operation, better toxic or shock
load tolerance, and a quick recovery from toxicity. The permissible organic loading rate in
the anaerobic process is also determined by the SRT (Khanal, 2008; Grady et al., 1999).

Hydraulic retention time is a deciding factor in process design for complex and slowly
degradable organic pollutants. Furthermore, SRT is the controlling design parameter for
easily degradable organics. For slow-growing microorganisms such as methanogens, longer
SRTs are required to prevent them from being washed out from the reactor. Determination

21
of SRT for an anaerobic system is equal to the hydraulic retention time for simple
calculation. Continuous stirred tank reactors without solid separation and recycling are
often prone to failure due to excessive biomass washout unless long SRTs are maintained.
Elevated hydraulic retention times require a bigger reactor volume (volume = flow rate ×
hydraulic retention time), which is costly (Khanal, 2008; Grady et al., 1999).

2.5.1.3 Volumetric organic loading rate (OLR)

Anaerobic processes are characterized by volumetric OLRs. This physical parameter is a


measure of the biological conversion capacity of the anaerobic digestion system. OLR is
particularly important control parameter in a continuous system. Many plants have reported
system failure due to overloading. OLR is expressed in kg COD or volatile solids (VS) per
m3 of reactor. It is linked with retention time for any particular feedstock and anaerobic
reactor volume (Verma, 2002). High-rate anaerobic reactors, such UASBs, are capable of
treating wastewater at volumetric OLRs of 10 – 40 kg COD/m3 × day. A high volumetric
OLR indicates that more wastewater can be treated per unit of reactor volume (Demirel and
Scherer, 2008).

2.5.1.4 Continuous feed

In order to prevent endogenous respiration among the bacteria community, daily feedstock
is required. Overfeed can asphyxiate the microorganisms. However, if the microorganisms
are not regularly fed, the bacteria will enter the starvation phase. As the rate of incoming
food decreased, the energy generation rate decreases as well. No energy present means non-
new growth of microorganisms and thus the net growth yield will decline (Grady et al.,
1999). As a result of endogenous metabolism, bacteria will use other bacteria communities
present in their enzymatic system to sustain themselves, which will decrease the treatment
efficiency of the bioreactor.

22
2.5.1.5 Mixing

An effective mixing system is critical to the successful operation of an anaerobic reactor or


digester. Mixing provides four advantages for an optimal methane yield in anaerobic
digestion. These advantages are: intimate contact between the microorganisms and their
substrate, resistant to mass transfer reduction, minimization of inhibitory reaction
intermediate build-up, and stable environmental conditions (Demirel and Scherer, 2008).

2.5.1.6 Characteristics of the substrate

Different substrates with different level of molecular complexity will have different
methane yield in an anaerobic reactor system (Lei and Rundong, 2010). The complex
substrates with higher molecular weight, such as municipal or industrial biosolids, animal
manure, will require long hydrolysis times before methane conversion. Counteraction of
inhibitors (such as ammonia or xenophobic compounds) can be achieved by adding certain
nutrients or by dilution of the waste.

2.5.2 Chemical factors

It has been pointed out earlier that anaerobic processes are severely affected by changes in
environmental conditions. The effect of environmental factors on treatment efficiency is
usually evaluated by the methane yield; because, methane forming bacteria are more
sensitive to environmental changes than the acid forming bacteria in anaerobic treatment of
wastewater/ sludge. The following is a brief summary of several chemical factors.

2.5.2.1 pH

The general optimum pH for anaerobic digesters has been found to vary from 6.8 to 7.2
(Gunnerson and Stuckey, 1986). Digester pH is governed by the interaction of various acids
and bases present in the reactor. These compounds can produce buffer systems in the
reactor. Insufficient buffer capacity in single stage digesters, where acid and methane

23
formation co-exist, may inhibit methanogenesis as a result of the pH decrease. Under the
high OLRs, the decline in pH value and the minimal or zero biogas (methane) produced
could probably be explained by the accumulation of VFAs during anaerobic digestion
(Monou et al., 2008). In such cases, external buffer addition may be beneficial/necessary to
neutralize the VFAs and subsequently lessen the adverse effect on methane formers.

2.5.2.2 Toxicity

The wastewater may contain compounds that are anaerobically difficult to degrade, such as
aromatic compounds, ammonia, heavy metals, halogenated compounds, cyanide, sulfide,
and some VFAs. Although, some anaerobic microorganisms are also capable of degrading
refractory organics that otherwise might be considered toxic (Monou et al., 2008).

2.5.2.3 Nutrients

All microbial-mediated processes require macro-nutrients and some trace elements (micro-
nutrients) during waste stabilization. Nutrients and trace elements are not directly involved
in waste stabilization. Nevertheless, they are the essential components of a microbial cell
and thus are required for the growth of an existing microbial cell and synthesis of a new
cell (Riaño et al., 2011). Nutrients and trace elements also provide a suitable
physicochemical condition for optimum growth of microorganisms. It is important to note
that if the waste stream in question does not have one or more of the important nutrients
and trace elements, the waste degradability can be severely affected. This is because of
inability of microbial cell to grow at an optimum rate and to produce new cells (Demirel
and Scherer, 2008).

The key to balancing the anaerobic digestion process lies in balancing the C:N ratio in the
substrate or co-substrate mixture, as well as other macro- and micro-nutrients. Nitrogen
requirement is governed mainly by the quantity of cells. The higher the overall cell yield,
the higher is the nitrogen requirement. For anaerobic digestion, the C:N ratio should be
close to 35:1 (Droste, 1997). The microorganisms require as well, the presence of some

24
micro-nutrients, in order to achieve their synthesis reactions. Some of these micro-nutrients
are potassium, calcium, magnesium, sulfur, sodium, chloride, iron, zinc, manganese,
copper, among other metals (Grady et al., 1999).

2.6 Anaerobic co-digestion

Application of co-digestion as an intelligent raw material management offers many


advantages (Lei and Rudong, 2010). Anaerobic co-digestion is defined as a treatment that
combines at least two different types of waste. The primarily goal of co-digestion is to
enhance biodegradation and to increase biogas production (Li et al., 2011). Co-digestion
also aims to reduce the potential negative effects, such as nutrient/alkalinity deficiency, and
toxicity on biogas production. Based on the physical and chemical characteristics of each
substrate, anaerobic co-digestion can yield its highest efficiency by making the “perfect”
co-substrate. Depending of the wastes, a co-substrate can generate higher buffering
capacity, protecting the digestion process from the accumulation of VFAs (Cuetos et al.,
2011). Furthermore, co-digestion can allow for higher nitrogen content substrates be co-
diluted with a higher concentration of COD substrate: achieving an appropriate nutrient
content (C:N). In addition, dilution of inhibitors (i.e., ammonia compounds and heavy
metals) is achieved. Thus, co-digestion reduces negative effects of specific substrates by
adding more of other substrate (Cuetos et al., 2011). Furthermore, co-digestion provides
higher efficiency in terms of land and equipment use. Additionally, cost can be shared
among the different waste producers (Cuetos et al., 2011; Riaño et al., 2011). Most
importantly, as a result of higher degradation efficiency, the co-digestion process will
reduce the amount of solid waste (dewatered digestate) that must be disposed of.

Industrial and municipal biosolids can be treated in an anaerobic co-digestion system


(Bajgain and Kellner, 2005). These processes will minimize industry’s carbon footprint,
and minimize solid disposal. Furthermore, the processes increase biogas production. Over
the past ten years, anaerobic co-digestion of biosolids with other substrates has been studied
mostly at lab-scale. Table 2.1 shows a summary of the results obtained with different
substrate combinations.

25
Table 2.1 Summary of typical results of anaerobic co-digestion

Author Substrates Type of digestion % TS removal* Biogas yield* Methane yield*


Pig manure Biochemical
Álvarez et al., 3.4 L CH4/kg
Fish waste methane potential N/A N/A
2010 TS×d
Biodiesel waste assays
Abattoir
Lab-scale semi-
Bouallagui et al., wastewater
continuous 86.2 0.85 L/g VSremoved 0.53 L/g VSremoved
2009 Fruit and vegetable
digesters
waste
Organic fraction
Dereli et al., 2010 municipal waste Full-scale digester 51 N/A 4370 m3/d
Primary sludge
Cow manure Biochemical
Lei and Rundong,
Bioorganic methane potential N/A 0.71 L/g VSadded 0.43 L/g VSadded
2010
municipal waste assays
Biochemical
methane potential
Herbal extraction
assays, and
Li et al., 2011 residues N/A 1 L/d 0.22 L/g VSadded
lab-scale semi-
Swine manure
continuous
digesters⌘

26
Author Substrates Type of digestion % TS removal* Biogas yield* Methane yield*

Potato processing
wastewater Biochemical
Monou et al., 2008 Pig slurry methane potential 72.1 1.56 L/gVS added 0.41 L/g VSadded
Abattoir assays
wastewater
*Optimum results (VS: volatile solids, TS: total solids)

27
Studies showed improvements due to addition of agricultural residues as co-substrates in
anaerobic treatments (Cuetos et al., 2011). Likewise, Lei and Rundong (2010) showed that
co-digestion of cow-manure and a municipal waste mixture had the highest biogas
production potential. In other studies, single digestion of agronomy residues presented poor
buffering capacity and higher accumulation of VFA through anaerobic digestion. However,
co-digestion of potato wastewater and pig slurry (pig waste) presented most efficient
process than single cases. For this case, manure had a high buffering capacity, plus a wide
range of nutrients needed for methanogens (Monou et al., 2008).

Currently there is not enough information available about co-digesting fruit juice and
sewage sludge, nor is there sufficient information about the correct nutrient ratio present for
each co-substrate studied so far. The closest study was on the co-digestion of winery
wastewater and sewage waste activated sludge. This particular research showed an increase
of anaerobic biodegradability, confirming that co-digestion neutralized negative effects of
some of the substrates (Rodriguez et al., 2007)

Overall, anaerobic co-digestion has more advantages than disadvantages. This technology
has the benefit of mitigating the presence of toxic compounds by diluting them, and would
help to balance the C:N ratios. As an important limitation with the existing literature, the
majority of the previous co-digestion results are based on biochemical methane potential
assays, which are conducted under batch conditions in very small vessels. These assays are
used only for preliminary screening and do not necessary represent the performance of
continuously-fed co-digesters used at the full-scale. In addition, not all the previous studies
used co-substrate volumetric ratios which were based on production rates of each waste
stream. Moreover, C:N:P ratios were not reported all the time for each single and/or co-
digestion scenarios.

2.7 Biogas as a global renewable energy

Biogas is a mixture of different gases produced from an anaerobic treatment system


including digester or co-digester. The biogas composition is mainly methane (40-75%),
carbon dioxide (25-55%), hydrogen sulfide (0-3%) and vapor water (0-10%) (Bothi, 2007).

28
Biogas produced from organic waste is a renewable source, therefore, will support both
environmental and energy sustainability. In US, the use of biogas production could generate
enough electricity to meet up to 3% of all electricity expenditures (Omer, 2008).
Furthermore, biogas production/recovery from organic waste in an enclosed digestion
system will reduce the greenhouse gas emissions that may be released from the waste if
decomposed in an uncontrolled environment, such as a landfill without gas recovery system
or composting piles. Also, biogas production does not have any geographical and climate
limitations.

In terms of the energy equivalency, 1 m3 of biogas will generate approximately 0.57 m3 of


methane, which can replace 0.57 L of oil. Similarly, 1 m3 of biogas will generate 2 kWh of
electricity (Balat and Balat, 2009; EPA: Inventory of U.S. greenhouse gas emissions and
sinks, 2011). Biogas energy could supply domestic needs, and could be used in
electrification, irrigation and water supply, among other processes (Bhutto et al., 2011;
Omer, 2008). The shift to alternative energy sources still requires much more investment in
infrastructure, equipment and research development.

Currently, there are six major types of bio-power systems. For anaerobic digestion, the
main types are direct-fired, co-firing, gasification, pyrolysis, and modular systems. These
bio-power technologies are easy to install in small or modular systems, achieving up to 5
MW of energy (Bhutto et al., 2011). Nevertheless, it is important to emphasize that the
presence of other gasses and impurities in the biogas may affect the performance and
efficiency of these bio-power systems. Therefore, prior to selection of a bio-power system,
it is necessary to analyze the biogas composition, in order to minimize any harmful impact
or deterioration of the complete system.

Gasses, such as hydrogen sulfide, can be present in the biogas. Hydrogen sulfide (H2S) is
generated by sulfate-reducing bacteria in anaerobic digestion. Hydrogen sulfide is colorless,
highly toxic and flammable gas at concentration limits of 4.3-46% with an odor of rotten
eggs. In most of the cases, if there is presence of hydrogen sulfide in the biogas, biogas co-
generation systems for electricity or heat generation cannot be operated without
maintenance problems. Oxidation of this gas in the presence of moisture produces sulfuric
acid, a highly corrosive compound (Ahammad et al., 2008).
29
Another major challenge of burning biogas to generate electricity is the presence of
siloxanes. Siloxanes are volatile cyclic organic gasses. Generally, they are present in the
biogas streams mostly from landfill sites. If siloxanes are fired, their combustion product
will be silica deposits. These silica forms would decrease the lifetime of engine and
turbines (Clark et al., 2012). The presence of both siloxanes and H2S were the main reasons
behind the operational problems experienced for the microturbines used to generate
electricity from the Glenmore landfill gas (Kelowna, BC) in the last couple of years.

Moreover, some other gasses present in the biogas are part of greenhouse gasses (i.e.
carbon dioxide, nitrous oxide, ozone, water vapor, etc.). Therefore, a pretreatment to purity
and to clean to the biogas prior to usage is necessary in order to give a longer lifetime and
warranty to the equipment. This will also reduce the greenhouse gas emissions from the
biogas burning.

Intensifying biogas research may lead to better ways to maximize the energy potential from
waste; the implementation of which may also lead to significant waste reductions. Either of
these would decrease the environmental footprint.

2.8 Summary

Fruit juice industries and domestic households both produce large volumes of waste daily.
Waste production is an everyday disposal concern for any city. The combination of already
known process, such as anaerobic digestion with co-digestion improves the performance of
current disposal methods. Anaerobic co-digestion is an environmentally friendly disposal
method that can reduce the overall carbon footprint. In addition, the development of this
system would produce enhanced biogas that can be used as renewable energy source for the
residents of the City of Kelowna. By combining municipal and industrial wastewater by-
products in anaerobic co-digestion, the environmental impacts from the disposal of waste
solids can be significantly reduced, especially when compared to traditional single-source
solid waste treatment methods.

The previous lab- and full-scale studies indicate that combining different waste streams in
an anaerobic digester could increase the methane production capacity to produce renewable
30
energy. However, co-digestion of fruit-juice and municipal waste streams has not been
implemented at the lab- or full-scale yet. Therefore, this study aims to assess the
biodegradation efficiency of these streams under mesophilic and thermophilic digester
conditions at volumetric ratios representing their productions rates at the treatment
facilities. The biogas produced in this process could be captured and use as a possible
alternative source of energy for the City of Kelowna. If the technology is proven to be
feasible, the benefits, for the City of Kelowna, are potentially enormous.

31
Chapter 3: Materials and methods

3.1 Industrial and municipal waste samples

Grab waste samples were collected from two different WWTPs and a landfill site in
Kelowna (BC, Canada). Both treatment plants and the landfill site are operated by the City
of Kelowna; therefore, co-digestion of these various streams in a single bioreactor
(anaerobic digester) were expected to be feasible from waste management point of view.
The samples were collected bi-weekly, and their respective characterizations were made the
same day of sampling. Upon characterization, the samples were stored in a fridge at 4oC.
Four different waste samples used for this study included sewage sludge cake, industrial
(fruit-juice) thickened waste activated sludge (TWAS), fruit-juice screen cake (SC), and
landfill leachate.

3.1.1 Municipal (sewage) sludge cake

The sewage sludge cake was taken from the municipal WWTP (Kelowna Pollution
Prevention Center). By 2010, the City of Kelowna WWTP treated 37 million liters of
sewage on a daily basis. In order to meet the population demand, the Kelowna Pollution
Prevention Center upgraded its facility’s capacity from 40 to 70 million liters per day. The
treatment facility bases its treatment on biological processes, targeting organic fractions of
municipal, and pretreated industrial and agricultural streams from the Valley. The overall
treatment plant consists of eight stages: 1) screening, 2) grit removal, 3) primary clarifiers
and fermenters, 4) bioreactor, 5) secondary clarifier, 7) disc filters, and 8) ultraviolet
disinfection (Figure 3.1).

32
Figure 3.1 Kelowna Water Pollution Prevention Center process flow diagram (DAF: dissolved air flotation)
33
The screen and grit removal are used to protect pumps, valves, pipelines from damage or
clogging by removing rags and large objects. The following primary sedimentation
removes readily settleable solids and floating material under gravitation forces. The settled
“primary sludge” is sent to fermenters to generate VFAs. The clear supernatant is passed to
the bioreactor for biological C, N and P removal. The bioreactor in Figure 3.1 is a modified
Bardenpho® (barnard denitrification phosphate) or “Phoredox” system. Phoredox reactors
consist of an anaerobic fermentation zone followed by two stages of anoxic and aerobic
complete-mix activated sludge. The hydraulic retention time of the Phoredox system is 9.3
hrs. SRTs are 6 d and 13 d during summer and winter months, respectively. Nitrogen
removal is reached by sequential nitrification-denitrification in a single-sludge system:
majority of total N is lost through as nitrogen gas (Oldham and Stevens, 1984; Sattayatewa
et al., 2009). The removal of phosphorous is achieved by phosphorus accumulating
organisms. The VFAs generated in the fermenters are used as a carbon source by the
denitrifying bacteria. The excess sludge generated in the bioreactor or “secondary sludge”
is settled in the secondary sedimentation tank and thickened via dissolved air flotation
(DAF) unit. Finally, fermented primary and thickened secondary sludge streams are mixed
at a volumetric ratio of 40:60 and are dewatered to a final solids concentration of 17.5 ± 1%
TS by a centrifuge. The centrifuged mixed sludge stream is called “dewatered sludge cake”
and is currently hauled to the Vernon Composting Facility at a rate of 2.5 truckloads (~60
wet tonnes) per day. The dewatered sludge cake was the first waste stream evaluated in this
study as a potential substrate for anaerobic co-digestion.

The dewatered sludge cake at 17.5% TS is too concentrated to digest by itself. Therefore,
samples of sludge cake were diluted to 4.5 ± 0.5% TS with tap water to lower the solids
loading to a level of a typical anaerobic digester. Illustration 3.1 shows the sewage sludge
cake before and after it has been diluted.

34
Illustration 3.1 Sewage sludge cake before and after dilution

3.1.2 Industrial (fruit-juice) waste streams

Two industrial waste streams, taken from Brandt’s Creek Tradewaste Treatment Plant
(BCTTP), were evaluated for their potential of anaerobic co-digestion. Daily, BCTTP treats
approximately 1100 m3/day of wastewater. The wastewater stream is a combination of fruit
juice industry wastewater generated from Sun-Rype Products Ltd. and winery wastewater
from Calona Wines Ltd. with volumetric flow rates of 775 m3 and 333 m3 per day,
respectively.

The combined wastewater stream entering BCTTP (Figure 3.2) is pumped to an 85 µm


Salsnes screen, which collects large solids such as apple seeds and skins (Illustration 3.2a).
This waste stream is referred to as “screen cake” and used in this study as one of the two
industrial streams. Upon screening, wastewater enters to an equalization tank for flow/load
equalization. Before entering the aerobic basin for biological treatment, an anaerobic
selector adds ammonia and phosphorus nutrients to the wastewater.

The biological treatment is achieved in an activated sludge unit consisting of an aeration


basin and two clarifiers. Operation sludge and hydraulic retention times are 25 days, and 72
hrs, at winter/summer production rate, respectively. The aeration basin contains two

35
aerators that transfer air to its content. The excess of ‘waste activated sludge’ generated in
the aeration tank is first settled in the secondary clarifiers and then is sent to a DAF tank to
increase the sludge concentration to a range in 3% to 5% TS. The solid effluent from DAF
results in the form of thickened waste activated sludge (TWAS). This stream (Illustration
3.2b) is referred to as “industrial TWAS” and used in this study as the second industrial
waste. The treated industrial wastewater from the secondary clarifiers is sent to the City of
Kelowna’s sewage system for further treatment.

Currently, there is a weekly production of 1 m3 of screen cake, which is disposed in the


Glenmore Landfill. The industrial TWAS is produced at a rate of ~25 wet tonnes per day
and is then shipped to a farmland in Vernon (BC), where it is used as fertilizer. Farmland
may change ownership in the near future, and there is a possibility that a future owner
might not want to use this industrial stream. Therefore, this study incorporated both screen
cake and industrial TWAS streams as potential substrates for the anaerobic co-digester.

36
Figure 3.2 Brandt’s Creek Tradewaste Treatment Plant process diagram (MLSS: Mixed liquor suspended solids)

37
A B

Illustration 3.2 A) Screen cake obtained from the Salsnes screen. B) Thickened waste activated sludge obtained from the top of the
dissolved air flotation tank at the Brandts Creek Tradewaste Treatment Plant

38
3.1.3 Landfill leachate

Glenmore Landfill is a site for the disposal of inorganic and organic solid waste materials
including kitchen waste: as it is presented in Figure 3.3. Glenmore Landfill has various
waste management stages, such as the temporary storage, consolidation and transfer, or
processing of waste material (sorting, treatment, or recycling). The leachate (liquid that
drains from the landfill) has been collected and pumped to the City sewer system for
several years. In recent years, the City has been installing perforated piping in the landfill
pile to allow for circulation of leachate back to increase the moisture content of the pile and
to accelerate the decomposition of organic solid waste. The same perforated pipes are used
to collect/capture biogas (50-52% methane) generated within the landfill. The City has
added three microturbines (90 kW total capacity) to allow for electricity generation from
the methane. However, due to high impurities in the landfill gas, such as corrosive H2S and
siloxanes, the performance of microturbines were compromised. Very recently, Fortis BC
has received approval from the BC Utilities Commission for design/construction of a
landfill gas purification plant at the Glenmore Landfill by 2014. The purified gas will then
be injected to Fortis BC’s natural gas system for use by customers.

Figure 3.3 Glenmore Landfill process flow

39
This study used the Glenmore Landfill leachate as the 4th substrate for the following
reasons. Although, among the four waste streams studied, the highest volume is generated
by the Kelowna’s municipal WWTP, this plant has a limited footprint and is constrained by
adjacent development. Therefore, a potential anaerobic co-digester may not be located at
the Kelowna's WWTP. Furthermore, there is a concern that the potential odour from the co-
digester will affect nearby residents. Therefore, the purpose of using landfill leachate in this
study was to evaluate whether a potential co-digester located near the Glenmore Landfill
instead can utilize the excess leachate stream along with other municipal and industrial
waste to provide moisture for dilution, as well as alkalinity, without having any inhibitory
effect (due to the potential presence of heavy metals) on the acid and methane formers in
the digester. As the final advantage, methane recovered from anaerobic co-digester can be
connected and utilized as part of the existing landfill biogas system for electricity
generation.

3.2 Inocula samples used as digester seed and acclimation

Mesophilic (35oC) inoculum (mixed culture of acid and methane forming bacteria) was
taken from the effluent line of a bench-scale (6 L) automated anaerobic sludge digester in
the Environmental Engineering Laboratory at the UBC Okanagan. The digester had been
treating a mixture of TWAS and fermented primary sludge from Kelowna’s municipal
WWTP, with a volumetric ratio of 60:40 at a sludge retention time (SRT) of 20 days.
Thermophilic (55oC) inoculum was taken from the effluent line of the full-scale
thermophilic sludge digesters at Annacis Island WWTP in Vancouver (BC, Canada).
Annacis Island plant contains physical, biological, and chemical treatment units.
Preliminary phase (screening and grit removal) and primary sedimentation were followed
by trickling filters and secondary clarifiers. The full-scale digesters are fed with a mixture
of primary sludge and WAS, and undergoes an extended (approximately 20-d SRT)
thermophilic anaerobic process to ensure pathogen reduction. Sludge dewatering is done
with centrifuges to 30% TS before disposal. Before setting up the actual bench-scale
digesters with inocula, four digesters (2 mesophilic and 2 thermophilic with 1.2 L wet
volumes each) were run for 85 days to acclimatize mesophilic and thermophilic inocula to a
mixture of Kelowna sewage sludge cake, industrial TWAS and screen cake at the

40
volumetric ratios corresponding to their daily generation rates, diluted with leachate.
Acclimation phase, or the first phase of the experiments, was done in order to prevent
severe initial inhibition or lag-phase during anaerobic digestion. All four acclimation
digesters were run at an approximately 20 d-SRT. Organic loading rates of the acclimation
digesters fed with the mixture of co-substrates were 1.42 ± 0.89 g TCOD/L × d. The
digester feed concentrations were 4.6% TS (w/w), which can be considered as typical
sludge concentrations in full-scale sludge digesters.

3.3 Anaerobic co-digestion studies

Upon inocula acclimation, second phase of the experiments, with an aim of assessing the
co-digestion performance of the co-substrates, was started. For the second stage, eight lab-
scale anaerobic digesters (total and wet volumes of 1 and 0.5 L, respectively), were set-up
with acclimated inocula to optimize the performance with single and co-substrate digester
feeding scenarios displayed in Table 3.1. In mesophilic (35 ± 2oC) and thermophilic (55 ±
2oC) temperature controlled shakers (at 90 rpm), digesters were evaluated on waste
minimization (total or organic solids removal efficiencies), biogas (methane) production
quantity/quality, coliform destruction and dewaterability performance of the digested
material (digestate). The single and co-digesters were started with a safe SRT of 20 days
corresponding to an organic loading rate of 2.97 ± 0.89 g TCOD/L × d. Once the steady-
state was achieved (< ±10% variation in daily gas production), digesters were operated
under identical loading conditions for the duration of 3 × SRT (i.e. 60 days for the SRT of
20 days [Eskicioglu et al., 2007]). Upon data collection during the steady state
performance, the SRT was reduced to 10 days (organic loading rate of 4.52 ± 0.86 g
TCOD/L × d) and similar operational procedure was repeated for the new SRT. Erlenmeyer
flasks with 1 L volume, shown in Illustration 3.3 A, were used as anaerobic single and co-
digesters. The flasks were sealed with two-hole rubber stoppers, one hole for effluent port,
and the second for biogas expulsion. Effluents were withdrawn and digesters were fed
(once every 24 hours including weekends) through the side arm of the flask by syringes.
Biogas was collected in 2 L tedlar bags, and measured by a manometer. Figure A.1
(Appendix A) shows the calibration curve for the manometer.

41
Table 3.1 Experimental plan for acclimation and anaerobic single and co-digestion stagesª

Total (wet) Substrate flowrate contributions for digester feed Sludge


Digester
Stage Goal Digester code digester Sludge cake TWAS Screen cake Leachate retention
temp.
volume (1) (2) (SC) (L) time
M/AC o
35 C
M/AC/d
1 Acclimation 2 (1.2) L 9.7 mL/d 3.7 mL/d 0.6 mL/d 36 mL/d 20 d
T/AC
55oC
T/AC/d
M/1 25 (50)† mL/d 35oC
(diluted with 0 0 0 20 d, 10 d o
Single T/1 55 C
1 (0.5) L tap water)
digestion
M/2 35oC
0 25 (50) mL/d 0 0 20 d, 10 d o
2 T/2 55 C

M/1+2+L 35oC
5 (10) mL/d 2 (4) mL/d 0 18 (36) mL/d 20 d, 10 d
T/1+2+L 55oC
Co-digestion 1 (0.5) L
M/1+2+SC+L 35oC
4.8 (9.6) mL/d 1.9 (3.8) mL/d 0.3 (0.6) mL/d 18 (36) mL/d 20 d, 10 d
T/1+2+SC+L 55oC
ªTWAS: thickened waste activated sludge; M: mesophilic; T: thermophilic; AC: acclimation; SC: screen cake; L: leachate
†Flowrate contributions with and without parenthesis are for sludge retention times of 20 and 10 days, respectively

42
A

1 2

Illustration 3.3 A) Eight semi-continuous digesters (four thermophilic and four mesophilic).
B) Digester configuration 1: Effluent port, 2: Biogas exit, 3: Influent port, and 4: Tedlar bag

3.4 Volumetric ratios for co-substrates in digester feed streams

Kelowna municipal WWTP currently treats wastewater from about 80% of the population.
Treatment plant load is constant throughout the whole year. Daily sludge cake production
for 2012 was 60 wet tones /d (~17-20% TS by weight). Slight changes may occur during
the different seasons throughout the year.

Fruit juice and wine industry production rates depend on harvest season of fruit. Hence,
Brandt’s Creek’s wastewater treatment volume is not constant throughout the whole year.
Major wastewater volumes are expected during winter (at the end of the harvesting in
Kelowna), and lower by summer. Industrial TWAS normalized production rate is 26,000

43
L/d (~3-4.5% TS by weight). Screen cake amounts are 1 m3 per week during high season
production.

Due to the significant differences in production rates, it was decided to test the co-digestion
of these waste streams based on their production rate. For simple references, single
digesters fed with sewage sludge cake were labeled as “1”. Industrial TWAS was identified
as “2”. Co-digestion of sewage sludge cake, TWAS and leachate for dilution was identified
as “1+2+L”, and co-digestion of the four waste streams including screen cake was labeled
as “1+2+SC+L”. According to temperature ranges, mesophilic digesters are “M” and
thermophilic: “T” as indicated in Table 3.1.

It is also necessary to emphasize that, in addition to digester scenarios displayed in Table


3.1, one additional single digestion scenario with leachate only was studied in order to
quantify biogas (methane) contribution from leachate in the co-digesters. The leachate
digester was operated for a period of 20 days. Due to very small amount of daily biogas
production, it was decided to not to monitor this digester any further. Results are
summarized in Appendix B.

3.5 Characterization of samples

Samples were characterized at room temperature (20 ± 2oC). Sample characterization


consisted of pH, alkalinity, total and volatile solid contents (TS/VS), total and soluble
chemical oxygen demands (TCOD/SCOD), volatile fatty acids (VFAs), total sugars and
ammonia measurements. To separate soluble from total solid fractions, sludge samples
were centrifuged at 8000 rpm for 20 minutes using a Fisher Scientific Sorvall Legend XT
automatic centrifuge and pre-filtered and then filtered through membrane filters with 1.2
μm and 0.45 μm pore sizes, respectively. In addition to parameters mentioned above,
dewaterability, total coliform concentrations were measured in digester effluents at the end
of each SRT to assess digestate quality for land application as fertilizer. Analytical tests and
frequency of sample characterization are shown in Table 3.2.

44
Table 3.2 Characterization of samples and frequency of analysisª

Samples Parameters Frequency


Raw waste streams TS, VS, TCOD, SCOD, pH, After each sampling from
(substrate) alkalinity, ammonia, TVFAs treatment plants (bi-weekly)
TS, VS, TCOD, SCOD, pH, Upon preparation of feed with
Digester feed
alkalinity, ammonia, TVFAs fresh substrates
pH Daily
TS, VS, TCOD Every three days
Alkalinity, ammonia, total, Once a week
Digester effluents TVFAs
Coliform test (total coliform Minimum two sets of data for
and Escherichia.coli) and each SRT at steady state
dewaterability
Biogas volume Daily
Digester biogas Biogas composition (CH4, Every three days
CO2, N2, O2 percentages)
ªTS: total solids, VS: volatile solids, TCOD, SCOD: total, and soluble chemical oxygen demands,
respectively, TVFA: total volatile fatty acids, SRT: sludge retention time

3.5.1 Total solids and volatile solids

Total and volatile solids procedures were based on Standard Methods 2540 B and 2540 E
(APHA, 2005), respectively. A well-mixed sample was evaporated in a weighed porcelain
dish and dried to constant weight in the oven overnight, at 103 to 105oC. Subsequently, the
dishes were weighted, TS was increased in weight over that of the empty dish. The residue
of the TS was ignited to constant weight at 550oC. The weight lost during ignition was the
VS fraction.

3.5.2 Chemical oxygen demand (COD)

The closed reflux colorimetric COD measurements were performed based on Standard
Methods procedure 5220D (APHA, 2005). The dichromate ion oxidizes the COD materials
in the sample. This results in the change of chromium ion from hexavalent to trivalent state.
45
In this method, samples were digested for 3 hours at 150oC. Samples were pre-diluted and
diluted before addition of reagents and digestion. With Spectronic 20D+ (Thermo-Electron
Corporation) spectrophotometer and 600 nm wavelength, the absorbance were read. A
standard curve (refer to Appendix A, Figure A.2) corresponding to 100-700 mg COD/L
was generated using potassium hydrogen phthalate solution as standard.

3.5.3 Alkalinity

Alkalinity of samples were determined according to Standard Method 2320B (APHA,


2005). In this method, 15 mL of supernatant of sample (centrifuged for 20 minutes at 8,000
rpm) were titrated with 0.1 N sulfuric acid to reach a pH value of 4.6. Alkalinity
measurements were carried out using a pH/ion electrode connected to the accumet excell
XL25 dual channel pH meter.

3.5.4 Ammonia

Dissolved ammonia concentration measurements were done on supernatant of samples. An


ammonia selective electrode connected to the accumet excell XL25 dual channel pH/ ion
meter was used for analyses. Measurements were done according to Standard Methods
4500-NH3 D procedures (APHA, 2005). In this method, dissolved ammonia (NH3(aq) and
NH4+) is converted to NH3(aq) at pH above 11. Ammonia-N calibration curve is presented in
Figure A.3 (Appendix A).

3.5.5 Gas Chromatography for volatile fatty acids (VFAs) and biogas composition

Total VFAs: acetic, propionic and butyric acids, were measured by injecting sample
supernatants (filtered through a membrane with 0.2 µm pore size) into the Agilent 7890A
Gas Chromatograph with a capillary column (Agilent 19091F-112, HP-FFAP polyethylene
glycol TPA column length x ID: 25 m, 320 µm). Detector was a flame ionization system
(oven, inlet and outlet temperatures: 200, 220 and 300oC, respectively, carrier gas flow rate:
25 mL helium/min) equipped with an autosampler. According to Ackman (1972), iso-

46
butyric acid was used as the internal standard. Biogas composition in the headspace of lab-
scale anaerobic digesters and co-digesters was determined with an Agilent 7820A Gas
Chromatograph with a packed column (Agilent G3591-8003/80002). The detector of this
system was thermal conductivity (oven, inlet and outlet temperatures: 70, 100 and 150oC,
respectively) using helium as the carrier gas (flow rate: 25 mL/min). The method was
developed by van Huyssteen (1967).

3.5.6 Dewaterability

Dewaterability of digestate samples were tested by a Capillary Suction Timer (CST, Model
440, Fann Instrument Company, TX, USA) based on Standard Methods Procedure 2710G
(APHA, 2005). According to this method, a sample volume of 5 mL was injected into a
small cylinder placed on a sheet of chromatography paper. While the paper extracts liquid
from the sludge by capillary suction, water released from sludge travels between two
contact points. A digital timer attached to the electrodes records the capillary suction time.
In this work, sludge temperature was constant (21 ± 1oC); also TS were tested in the
digestate samples, to normalize the data in units of sec/g TS.

3.5.7 Total coliforms

Total coliforms were tested with a semi-automated system, measuring presence and
quantification of pathogens in terms of total coliforms and Escherichia coli (E.coli). Using a
most probable number (MPN) method, Colilert test, after 24 h incubation, will count total
coliforms present (IDEXX Colilert Quanti-tray 2000). The procedure was developed by
IDEXX Laboratories and was previously tested by other researchers (Coelho et al., 2011)
on digestate samples with similar solid concentrations. The method provides 95%
confidence limits comparable to the membrane filtration method and can count up to 2142
colony forming units (CFU)/mL without dilution. Dilutions were done prior to testing.

47
Chapter 4: Results and discussion

4.1 Characterization of raw industrial and municipal waste streams

The results for characterization of the four different waste streams are summarized in Table
4.1. Both sewage sludge cake and screen cake (SC) had slightly acidic (less than 6) pH
values, compared to neutral pH levels of industrial TWAS (2) and leachate. Furthermore,
sludge cake had a high concentration of TVFA, which could be due to natural
decomposition of this high-strength waste during storages on site or in the fridge. From
June 7th, till December 13th, 2012 there were 10 sampling times, with a variation of ± 33%
for industrial TWAS and SC, variations for characterization of leachate and sewage sludge
cake were below ± 10%. The higher variation in the industrial waste streams were due to
changes in the fruit-juice production. Glenmore landfill is a mature landfill, therefore the
leachate contains low TS, VS concentrations and VS/TS ratios (Table 4.1).

Table 4.1 Characterizations of raw municipal and industrial waste streams studiedª

Parameter Sludge cake 2 (TWAS) SC (Screen cake)* Leachate


pH (-) 5.52 ± 0.17† 6.54 ± 0.25 5.54 ± 0.96 7.13 ± 0.10
TS (% w/w) 17.44 ± 0.66 2.43 ± 0.22 21 ± 3 0.53 ± 0.02
VS (% w/w) 14.96 ± 0.69 2.06 ± 0.21 19 ± 4 0.09 ± 0.01
VS/TS*100 (%) 85.78 84.61 ± 2.99 90.48 0.18 ± 0.02
TCOD (mg/L) 196,024 ± 31488 21,904 ± 155 91,728 ± 36318 703 ± 349
SCOD (mg/L) 10,609 ± 4360 1,403 ± 41 -- 446 ± 106
Alkalinity (mg
733 ± 208 370 ± 141 -- 3,489 ± 222
CaCO3/L)
Ammonia (mg
427 ± 38 8.33 ± 3.21 -- 84 ± 2
NH3-N/L)
TVFA (mg/L) 1,679 ± 102 36.29 ± 3.34 -- 21.17 ± 14.95
ªTS: total solids, VS: volatile solids, TCOD, SCOD: total, and soluble chemical oxygen demands,
respectively, TVFA: total volatile fatty acids, TWAS: thickened waste activated sludge
*Due to high solid concentration, there was no supernatant volume for SCOD, alkalinity, ammonia
and TVFA analyses
†Data represent the arithmetic mean of triplicates ± standard deviation

48
Among the substrates characterized (Table 4.1), the leachate had the highest alkalinity, a
neutral pH, and lower ammonia concentration. Alkalinity presence is necessary in order to
get a stable first stage of anaerobic digestion: hydrolysis and acidogenesis (Demirel and
Scherer, 2008). Alkalinity is the buffering system necessary to a potential high VFA
accumulation during digestion (Monou et al., 2008). Also, methanogenic bacteria are most
likely to cease their growth due to ammonia inhibition (Cuetos et al., 2011). Consequently,
low ammonia concentrations in the digester feed are preferred in order to have a stable
anaerobic environment. Hence, leachate with all these advantages makes it a valuable co-
substrate to dilute concentrated waste streams (i.e., sludge and screen cakes) fed to an
anaerobic digester. Industrial TWAS was the only substrate that could be fed to a digester
(without dilution) as single substrate due to its sludge concentration (2.43% TS). Finally,
VS/TS × 100 ratios reported in Table 4.1 indicated high organic fractions (> 84%) with
significant biodegradation potential; and, this was further assessed by bioreactor studies
within this project.

4.2 Characterization of diluted industrial and municipal waste streams

Characterization of raw and diluted waste mixtures, after each sampling from the WWTPs
(Kelowna WWTP and BCTTP), was essential in order to understand seasonal variations.
For co-digestion scenarios, waste streams were mixed according to their daily production
rates and also utilized landfill leachate to bring (dilute) the solids concentrations down to
typical digester influent concentrations. Table 4.2 displays the feed characterization for
both single as well as co-digestion scenarios after dilution/mixing according to Table 3.1.

As it can be seen from Table 4.2, although waste streams of 1, L and 1+2+SC+L had
similar TS, VS and COD concentrations, VS/TS ratios of the 1+2+SC+L was the lowest.
Furthermore, the co-digester feeds had higher alkalinity due to addition of landfill leachate,
which provided an advantage/additional buffering capacity. Overall, the characterization
results indicated that the mixture of the four substrates (waste streams) produced safe pH,
ammonia, alkalinity, VFA levels.

49
Table 4.2 Characterizations of diluted waste streams as digester feedª

Anaerobic single digestion Anaerobic co-digestion


Parameter (1) (2) 1+2+L 1+2+SC+L
pH (-) 5.72 ± 0.26† 6.54 ± 0.25 6.61 ± 0.24 6.72 ± 0.11
TS (% w/w) 4.48 ± 0.05 2.43 ± 0.22 4.33 ± 0.28 4.39 ± 0.29
VS (% w/w) 3.81 ± 0.04 2.06 ± 0.21 3.65 ± 0.31 3.38 ± 0.17
VS/TS × 100 (%) 85.16 ± 1.42 84.77 ± 2.91 84.27 ± 5.10 77.20 ± 5.01
TCOD (mg/L) 41,620 ± 166 21,904 ± 155 41,049 ± 1813 43,874 ± 385
SCOD (mg/L) 5,336 ± 109 1,403 ± 41 5,929 ± 148 6,371 ± 89
Alkalinity (mg
728 ± 396 370 ± 141 2,572 ± 702 2,416 ± 617
CaCO3/L)
Ammonia (mg NH3-
287.38 ± 142.82 8.33 ± 3.21 268.79 ± 88.16 251.84 ± 65.66
N/L)
Volatile Fatty Acids (VFAs)
Acetic acid (mg/L) 862 ± 456 17 ± 9 649 ± 61 668 ± 72
Propionic acid
558 ± 127 17 ± 11 383 ± 36 401 ± 35
(mg/L)
Butyric acid (mg/L) 264 ± 24 2±1 162 ± 24 162 ± 22
Nutrient availability
C:N ratio² 7.4:1 12.1:1 7.5:1 n/a*
ª(1): diluted sewage sludge, (2): industrial TWAS, SC: screen cake, L: leachate, TS: total solids,
VS: volatile solids, TCOD, SCOD: total, and soluble chemical oxygen demands, respectively,
TVFA: total volatile fatty acids
†Data represent the arithmetic mean of triplicates ± standard deviation)
*Could not be estimated due to absence of data for total nitrogen and phosphorus in screen cake.
However screen cake, comprised of fruit seed and skin, is expected to contain total nitrogen and
phosphorous, therefore this substrate mixture should contain C:N:P values as minimum as 1+2+L
²C:N ratios in municipal sludge cake and leachate were reported by City of Kelowna and in
industrial TWAS by Sun-Rype Beverage Inc.

As it was emphasized earlier, the ideal C:N ratio for anaerobic digestion ranges from
approximately 30:1 to 35:1 (Droste, 1997). Higher ratios will produce a slower digestion
rate. The addition of co-digestion materials can improve the C:N ratio, thereby increasing
methane production. In this study, C:N ratios were reported in Table 4.2 for the feed

50
streams for both single and co-digestion scenarios. In general, fruit juice wastewaters are
well known for poor nutrient contents (Ozbas et al., 2006). Therefore, BCTTP adds
nutrients to its wastewater before it enters into the biological treatment process. On the
other hand, in general municipal waste streams do not need external nutrient addition due to
high urea content. Due to these reasons, after characterization, both municipal and
industrial streams indicated adequate nutrient content in Table 4.2.

4.3 Inoculum acclimation to waste streams studied

As it was described in Chapter 3, both mesophilic and thermophilic inocula were


acclimated to a mixture of waste streams comprised of municipal sludge cake, industrial
TWAS and screen cake at volumetric ratios representing their daily production rates. As the
initial inocula were taken from anaerobic digesters treating only municipal sludge,
acclimation phase was necessary for both acid and methane forming bacteria to adapt
themselves to industrial waste streams. The adequate acclimation period minimizes
inhibition risk on methanogenic bacteria, sensitive to environmental changes and inhibitory
substances and improves the biodegradation rate (Droste, 1997).

When the mesophilic and thermophilic inocula were being acclimatized in four semi-
continuously fed digesters, daily biogas productions reached a stable value. Steady state
was defined as the period of time in which less that 10% variation was observed from data
related to biogas production, organic (solids or COD) removal efficiencies, or digester pH
readings (Schimel and Boone, 2010). Table 4.3 summarizes the loading conditions as well
as steady state biogas and methane yields achieved from the acclimation reactors, fed in a
semi-continuous mode. The four digesters were acclimatized to industrial sludge without
any indication of acute or chronic toxicity. Table 4.4 summarizes thermophilic and
mesophilic inocula characterization before and after acclimation phase. After acclimation,
lab-scale anaerobic digesters were set-up with these acclimatized inocula.

51
Table 4.3 Steady state results for acclimation semi-continuous digestersª

Mesophilic (35oC) Thermophilic (55oC)


Parameter
digesters digesters
Sludge retention time (SRT) (d) 20 20
Organic loading rate (OLR) (g TCOD/L × d) 4.0 ± 3† 3.8 ± 5
Daily biogas production (mL/d) 1,221 ± 50 1,172 ± 9
Specific biogas yield (L/g VS removed × d) 0.92 ± 0.09 1.08 ± 0.07
Methane (CH4) composition in biogas (%) 66.28 ± 1.00 66.39 ± 1.43
Specific methane yield (L/g VS removed × d) 0.61 ± 0.02 0.72 ± 0.01
ªVS: volatile solids, TCOD total chemical oxygen demands
†Data represent the arithmetic mean of 30 data points, duplicates ± standard deviation

Table 4.4 Inocula characteristics before and after acclimation

Mesophilic (35oC) inoculum Thermophilic (55oC) inoculum


Parameter Before acclim. After acclim. Before acclim. After acclim.
pH (-) 7.52 ± 0.05† 7.65 ± 0.07 8.01 ± 0.01 7.95 ± 0.02
TS (% w/w) 2.68 ± 0.15 3.28 ± 0.02 1.93 ± 0.00 2.91 ± 0.07
VS (% w/w) 1.79 ± 0.02 2.38 ± 0.01 1.40 ± 0.01 2.06 ± 0.05
TCOD (mg/L) 17,857 ± 3030 25,847 ± 2549 18,714 ± 202 28,124 ± 983
SCOD (mg/L) 7,936 ± 768 1,211 ± 82 1,236 ± 10 3,216 ± 122
Alkalinity
5,325 ± 35 3,342 ± 63 8,967 ± 210 5,737 ± 210
(mg CaCO3/L)
Ammonia
799 ± 37 1,124 ± 101 252 ± 19 1,610 ± 194
(mg NH3-N/L)
TVFA (mg/L) 52.29 ± 0.03 104.3 ± 0.19 2.81 ± 0.01 56.78 ± 12.78
ªTS: total solids, VS: volatile solids, TCOD, SCOD: total, and soluble chemical oxygen demands,
respectively, TVFA: total volatile fatty acids
†Data represent arithmetic mean of triplicates ± standard deviation

52
4.4 Effect of addition of co-digestion materials on digester performance

Upon acclimation, the actual single and co-digesters were continuously operated for
another 4 months, achieving steady states at two different SRTs. Digestion operation started
at a safe SRT of 20 d (Khanal, 2008), OLR starting from 1.41 ± 0.77 g TCOD/L/d (Table
4.5). Long SRTs with a lower organic loading are always used first in lab-scale digesters in
order to avoid instability until microbial culture is fully acclimatized (Schimel and Boone,
2010). Steady state was accomplished after a week of digestion and digesters were kept
under the same loading for another 74 days. After completion of the 20-d SRT, the SRT
was reduced to 10 d (OLR of 3.02 ± 0.12 g TCOD/L/d (Table 4.6)). Under this 10-d SRT
period, steady state conditions were achieved after 3 days of operation (based on biogas
production) and data were collected for another 38 days under the same loading. The data
collected during the un-steady state were not presented in this thesis.

Figure 4.1 shows daily biogas productions at standard temperature and pressure (STP; 0oC,
1 atm). This figure is an example of a digester operational pattern during steady state
conditions. Additionally, Figure 4.1 shows the transition between the changes of SRTs
from 20 d to 10 d. From Figure 4.1, at the 20-d SRT, mesophilic digesters with higher
average biogas production were 1 (digester M-1: 433 ± 15 mL/d) and 1+2+L (digester M-
1+2+L: 411 ± 23 mL/d). During the 10-d SRT, the digesters that generated the highest daily
average biogas volume were: 1+2+SC+L (M-1+2+SC+L with 731 ± 18 mL/d) and 1 (M-1
with 715 ± 14 mL/d). On the other hand, at both SRTs, digester M-2 was the lowest in
producing biogas.

For thermophilic digesters, through the 20-d SRT, daily average biogas productions were
up to 418 ± 11 mL/d, with the digester T-1+2+SC+L being the highest producer. While
thermophilic digesters were running with 10-d SRT loadings, higher biogas producers were
T-1+2+L (T-1+2+L with 702 ± 17 mL/d) and T-1 (T-1 with 701 ± 20 mL/d). From these
results, no significant differences were observed in the biogas production pattern of
digesters fed with 1, 1+2+L and 1+2+SC+L. The addition of industrial co-substrates to
municipal sludge cake did not improve or deteriorate biogas production from the municipal
waste stream.

53
Furthermore, between the single digestion scenarios, the scenario of 2 with industrial
TWAS only, had the lower performance. At both mesophilic and thermophilic temperatures
and SRTs, digester 2 was the lowest biogas producer. In addition, as it can be seen from
Figure 4.1, at the SRT of 10 days, digester 2 could not achieve steady state with biogas
production gradually declining at both mesophilic and thermophilic digester temperatures.
It is also necessary to emphasize that Brandt’s Creek juice production rate is seasonal;
therefore, significant changes have been found in their waste characterization according to
the time of the year.

Furthermore, the average daily biogas productions are directly linked to total and organic
(volatile) solids fed to digesters with incoming streams. The higher solids present in
digester feed should yield more biogas volumes. Therefore to be able to compare biogas
yields for different digestion scenarios with varying solids concentration as in this study
(Table 4.2), normalizations should be made. Figure 4.2 shows the specific daily biogas
volumes normalized per g volatile solids (VS) removed during digestion.

54
A 1 2 1+2+L 1+2+SC+L

800
Sludge retention time = 20-d
600

400
Daily biogas production (mL/d)

200

0
0 20 40 60 80 100 120

B
Sludge retention time = 10-d
800

600

400

200

0
0 20 40 60 80 100 120

Digestion time (days)

Figure 4.1 Daily biogas productions (@STP) of anaerobic digesters fed with diluted sewage sludge cake (1), Thickened waste activated
sludge (2), 1+2+L (leachate), and 1+2+SC+L (screen cake). A) Mesophilic digesters, B) Thermophilic digesters

55
1 2 1+2+L 1+2+SC+L
A
Specific daily biogas production (L/g VSremoved) 1,4 Sludge retention time = 10-d
1,2
1
0,8
0,6
0,4
0,2
0
0 20 40 60 80 100 120
B
Sludge retention time = 20-d
1,4
1,2
1
0,8
0,6
0,4
0,2
0
0 20 40 60 80 100 120
Digestion time (days)

Figure 4.2 Specific daily biogas productions (@STP) of anaerobic digesters fed with diluted sewage sludge cake (1), Thickened waste
activated sludge (2), 1+2+L (leachate), and 1+2+SC+L (screen cake). A) Mesophilic digesters, B) Thermophilic digesters

56
The averages of specific biogas yields from 8 digesters were similar or above of the
expected biogas yield, reported by Droste (1997) as 1 L/g VSremoved × d for municipal mixed
(primary + secondary) sludge. For mesophilic conditions through the 20-d SRT, single
substrate digester (2) utilizing industrial TWAS only had the highest yields numbers.
However, for the 10-d SRT, co-substrate digesters had a better performance as it is shown
in Figure 4.2.B. Thermophilic digesters during the 20-d SRT had a different pattern: co-
digested substrates had a higher specific biogas yield compared to single digestion. Same
behavior as mesophilic digesters, while 10-d SRT was running, thermophilic co-digesters
had the highest specific biogas yields.

Similar to responses analyzed for Figure 4.1, single and co-digested digesters did not
indicate any instability problems at the 20-d SRT in terms of specific daily biogas volumes
normalized based on solids removal (Figure 4.2). However, digesters M-2 and T-2 at 10-d
SRTs started to reduce their specific biogas productions (Figure 4.2), which is in agreement
with the patterns observed in Figure 4.1. This biogas generation decline started after 20
days of running at 10-d SRT. Summarized steady state values of the monitored parameters
during 20-d SRT and 10-d SRT are shown in Table 4.5 and Table 4.6, respectively.

57
Table 4.5 Results for semi-continuous digesters at 20 d SRT during steady state*

SRT = 20 d
Mesophilic Thermophilic
Parameter 1 2 1+2+L 1+2+SC+L 1 2 1+2+L 1+2+SC+L
Loading rates for digesters
OLR
2.73(0.79)† 1.41(0.77) 2.84(0.92) 2.97(0.89) 2.73(0.79) 1.41(0.77) 2.84(0.92) 2.97(0.89)
(gTCOD/L × d)
OLR
3.77(0.12) 2.19(0.23) 3.81(0.26) 3.73(0.36) 3.77(0.12) 2.19(0.23) 3.81(0.26) 3.73(0.36)
(gsubstrate/d)
Specific CH4 yield
0.53(0.07) 0.35(0.05) 0.45(0.09) 0.55(0.04) 0.48(0.04) 0.38(0.05) 0.45(0.06) 0.50(0.04)
(L/g VSremoved × d)
Specific CH4 yield
0.23(0.03) 0.13(0.03) 0.24(0.03) 0.24(0.02) 0.22(0.01) 0.16(0.05) 0.23(0.02) 0.25(0.01)
(L/g VSadded × d)
Removal efficiencies
TS (%) 36.75(4.17) 27.66(3.94) 40.42(6.71) 40.03(3.66) 39.06(5.78) 33.25(5.77) 40.95(4.28) 43.21(3.16)
VS (%) 43.01(2.57) 36.81(6.80) 50.21(2.64) 44.20(4.41) 46.62(3.65) 41.04(5.25) 51.02(4.12) 49.22(2.60)
TCOD (%) 54.89(4.57) 50.49(14.13) 56.58(7.58) 58.54(10.22) 58.06(4.93) 55.57(10.79) 58.51(6.81) 61.27(7.94)
Reactor pH (-) 7.37(0.16) 7.26(0.16) 7.48(0.16) 7.50(0.17) 7.92(0.15) 7.83(0.13) 7.98(0.24) 8.12(0.12)
Effluent supernatant characterization
Alkalinity
3,936(230) 2,535(412) 4,503(839) 5,032(462) 4,816(258) 3,536(373) 4,901(1077) 5,596(751)
(mg CaCO3/L)
Ammonia
1,476(392) 772(184) 1,161(258) 1,235(342) 1,588(542) 1,057(355) 1,475(465) 1,406(422)
(mg NH3-N/L)
TVFA (mg/L) 117(20) 4(3) 58(16) 166(57) 86(16) 25(3) 343(39) 144(102)
*SRT: sludge retention time, OLR: organic loading rate, TS: total solids, VS: volatile solids, TCOD: total chemical oxygen demands, respectively,
TVFA: total volatile fatty acids
†Data represent the arithmetic mean of minimum of duplicates for loading rates and 74 replicates for the remaining parameters collected during
steady state (standard deviation)

58
Table 4.6 Results for semi-continuous digesters at 10 d SRT during steady state*

SRT = 10 d
Mesophilic Thermophilic
Parameter 1 2 1+2+L 1+2+SC+L 1 2 1+2+L 1+2+SC+L
Loading rates for digesters
OLR
4.02(0.22) 3.02(0.12) 3.98(0.21) 4.38(0.23) 4.02(0.22) 3.02(0.12) 3.98 (0.21) 4.38(0.23)
(gTCOD/L × d)
OLR
7.80(0.38) 4.52(0.86) 7.76(0.12) 7.66(0.86) 7.80(0.38) 4.52(0.86) 7.76(0.12) 7.66(0.86)
(g substrate/d)
Specific CH4 yield
0.40(0.04) 0.22(0.20) 0.39(0.05) 0.45(0.03) 0.37(0.04) 0.32(0.15) 0.40 (0.04) 0.42(0.04)
(L/g VSremoved × d)
Specific CH4 yield
0.19(0.03) 0.08(0.05) 0.19(0.03) 0.21(0.01) 0.18(0.03) 0.13(0.05) 0.19(0.02) 0.20(0.02)
(L/g VSadded × d)
Removal efficiencies
TS (%) 38.56(4.12) 29.67(4.13) 42.28(5.01) 43.71(6.80) 42.02(4.38) 39.78(4.58) 40.56(3.59) 40.69(3.55)
VS (%) 47.39(3.67) 39.05(6.34) 47.32(3.00) 46.28(2.82) 49.07(4.29) 40.96(5.57) 48.25(2.27) 47.24(4.32)
TCOD (%) 45.95(7.21) 31.62(7.29) 50.34(3.43) 57.43(4.38) 42.67(5.01) 40.45(10.07) 46.90(9.14) 50.76(5.84)
Reactor pH 7.48(0.09) 6.99(0.27) 7.59(0.09) 7.68(0.10) 7.93(0.09) 7.71(0.17) 8.17(0.07) 8.20(0.15)
Effluent supernatant characterization
Alkalinity
3,810(390) 2,097(292) 4,967(354) 5,257(301) 4,633(1019) 3,512(418) 5,958(302) 5,908(319)
(mg CaCO3/L)
Ammonia
1,764(342) 849(102) 1,485(262) 1,641(194) 2,368(413) 1,475(196) 2,178(261) 2,171(260)
(mg NH3-N/L)
TVFA (mg/L) 109(20) 985(287) 144(53) 65(26) 1,074(498) 1,067(254) 798(260) 738(33)
*SRT: sludge retention time, OLR: organic loading rate, TS: total solids, VS: volatile solids, TCOD: total chemical oxygen demands, respectively,
TVFA: total volatile fatty acids
† Data represent the arithmetic mean of minimum of duplicates for loading rates and 38 replicates for the remaining parameters collected during
steady state (standard deviation)

59
As shown in Tables 4.5 and 4.6, specific methane yields for the 20-d SRTs varied from 0.35
to 0.55 L/g VSremoved × d. Mesophilic digesters had the highest methane yields compared to
digesters ran at thermophilic temperatures. For both digesters, in general, single digesters had
lower specific methane yields than the co-digestion scenarios. This effect was possibly due to
good buffering capacity provided by addition of the leachate (Table 4.5) for the co-digestion
scenarios. For 10-d SRT digesters, specific methane yields had the same pattern, however,
values were lower compared to the 20-d SRT results due to two times higher organic loading
rates, challenging acid and methane formers.

Organic removal efficiency can be quantified by VS and TCOD removals (Droste, 1997). In
general, mesophilic and thermophilic digesters at 20-d SRT had TS removals up to 40-43%,
respectively. As it is shown in Figure 4.3A, co-digesters had higher organic removals (40%-
43%) compared to single-substrate digesters. Figure 4.3B showed a close-up removal
comparison between single and co-substrate digesters. For the 10-d SRT, mesophilic co-
digestion scenarios had also the higher removal efficiencies compared to single digestion
scenarios.

Furthermore, from Figure 4.4, it can be seen that VS removal performances of digesters did
not have a significant change between 20-d and 10-d SRT. In order to understand whether the
differences were statistically significant, ANOVA with two variables has been performed.
Statistical analysis results for solid removal efficiencies in terms of both TS and VS
removals, indicated that, with 95% of confidence, the effects of digestion temperature
(mesophilic or thermophilic) and SRT (20-d or 10-d) were not significantly different.
However, single and co-digestion scenarios presented statistically significant differences (p <
0.05 for TS and p ≤ 0.05 for VS removals, respectively), suggesting that co-digestion has a
better performance than the single digestion in terms of solid removal efficiencies. The
ANOVA analyses are shown in Appendix C.1 and C.2.

60
Mesophilic Thermophilic
60
A
50
Total solids removal (%)

40

30

20

10

0
1 2 1+2 1+2+SC 1 2 1+2 1+2+SC
Single digestion Co-digestion Single digestion Co-digestion
Sludge retention time = 20 d Sludge retention time = 10 d

60
B
50
Total solids removal (%)

40

30

20

10

0
1 1+2
Single digestion Co-digestion
SRT = 20 d

Figure 4.3 A) Total solids removal efficiencies at sludge retention times (SRTs) of 20 and 10
days. B) Comparison of TS removal between 20d SRT mesophilic digesters (data represent the
arithmetic mean of duplicates and error bars represent standard deviations, SRT: sludge
retention time, TS: total solids)

61
Mesophilic Thermophilic
60
A

50
Volatile solids removal (%)

40

30

20

10

0
1 2 1+2 1+2+SC 1 2 1+2 1+2+SC
Single digestion Co-digestion Single digestion Co-digestion
Sludge retention time = 20 d Sludge retention time = 10 d

B 60

50
Volatile solids removal (%)

40

30

20

10

0
1 1+2
Single digestion Co-digestion
SRT = 20 d

Figure 4.4 A) Volatile solids removal efficiencies at sludge retention times (SRTs) of 20 and 10
days. B) Comparison of VS removal between 20d SRT mesophilic digesters (data represent the
arithmetic mean of duplicates and error bars represent standard deviations SRT: sludge
retention time, VS: volatile solids)

62
Figure 4.5 shows the TCOD removal efficiencies. Values for TCOD removals in mesophilic
digesters through 20-d SRT were among 58% (1+2+SC+L) and 50% (2- digesters). For 10-d
SRT, removal values dropped to 57% (1+2+SC+L) and 31% (2-digesters). It is clear that
both single and co-digestion scenarios were negatively affected by the higher organic loading
rates at the shorter SRT, indicating reduced TCOD removals and the difference was
statistically significant (p < 0.05). Furthermore, between the single and co-digesters, single
digesters experienced higher level of decline in their TCOD removal performances, however
the effect was statistically significant only at a confidence limit of 92% (Appendix C.3).
These results once again confirmed that adding municipal waste and landfill leachate to fruit-
juice waste increased the stability of anaerobic digesters.

Among all the digester scenarios studies, single digestion of industrial TWAS (2) had the
lowest performance in terms of TS, VS and TCOD removal efficiencies. Since industrial
TWAS is purely a secondary sludge with higher amount of microbial cells creating resistance
to biodegradation than those in municipal cake (60:40% secondary: primary by weight),
lower biodegradation efficiencies were somewhat expected for TWAS. Furthermore, the
extended HRT (72 hrs) and SRT (25 days) operational parameters used for treating fruit-juice
wastewater in the activated sludge tank must have created a relatively old TWAS with highly
refractory content limiting biodegradation/ methane potential. Although both mesophilic and
thermophilic digesters achieved relatively stable performance at an SRT of 20 days, the daily
biogas production started declining gradually at an SRT of 10 days (Figure 4.1). To be able
understand the reason behind this decline observed under both mesophilic and thermophilic
digestion, the feed characterization was repeated once again to account for any change that
may have occurred during storage in the fridge. Due to the seasonal production in Brandt’s
Creek Tradewaste Treatment Plant, the same feed was used for the last SRT (10 days) for
three weeks after sampling from Brandt’s Creek WWTP. The feed characterization results,
displayed in Table 4.7, indicated signs of acidification (pH drop from 6.4 to 5.6 and TVFA
increase from 138 to 3259 mg/L) that occurred during storage in the fridge. It is highly
probable that high VFAs being fed to the single digesters at an SRT of 10 days contributed
consumption of alkalinity which eventually led to drop in reactor pH and biogas production.
The co-digestion digesters, on the other hand, took advantage of the additional alkalinity

63
provided by the landfill leachate and remained stable in terms of both organic removals as
well as biogas production.

Mesophilic Thermophilic
80
A 70

60
TCOD removal (%)

50

40

30

20

10

0
1 2 1+2 1+2+SC 1 2 1+2 1+2+SC
Single digestion Co-digestion Single digestion Co-digestion
SRT = 20 d SRT = 10 d

80
B
70
TCOD removal (%)

60
50
40
30
20
10
0
1 1+2+SC
Single digestion Co-digestion
SRT = 20 d

Figure 4.5 A) Total chemical oxygen demand removal efficiencies at sludge retention times
(SRTs) of 20 and 10 days. B) Comparison of TCOD removal between 20d SRT mesophilic
digesters (data represent the arithmetic mean of duplicates and error bars represent standard
deviations SRT: sludge retention time, TCOD: total chemical oxygen demand)

64
Table 4.7 Characterization of industrial TWAS on sampling date and after 3 weeks of storage
in fridge
Parameter TWAS @ sampling date TWAS after 3 weeks
pH (-) 6.41 ± 0.01† 5.55 ± 0.02
TCOD (mg/L) 22,571 ± 51 21,400 ± 485
SCOD (mg/L) 152 ± 20 142 ± 1
TS (% w/w) 2.44 ± 0.01 2.37 ± 0.01
VS (% w/w) 2.14 ± 0.01 2.06 ± 0.01
Alkalinity (mg CaCO3/L) 533 ± 94 367 ± 0
Ammonia (mg NH3-N/L) 7±2 266 ± 5
Volatile fatty acids
Acetic acid (mg/L) 24 ± 12 572 ± 48
Propionic acid (mg/L) 41 ± 10 711 ± 6
Butyric acid (mg/L) 73 ± 6 1,976 ± 11
*TWAS: thickened waste activates sludge, TCOD, SCOD: total and soluble chemical oxygen
demand, TS: total solids, VS: volatile solids
†Data represent the arithmetic mean of triplicates ± standard deviation

Biogas composition of each single and co-digester was measured in order to assess whether
substrate type has an impact on methane content of biogas accumulated in headspace. During
20-d and 10-d SRTs, all digesters had methane productions above 62%. Table 4.8 depicts the
biogas composition through steady state period of the digesters. Results indicated that the
methane percentage was not affected by the substrate type (single or co-digestion of different
substrates). Statistical analyses results indicated that with 95% of confidence, the effect of
changing digestion temperature (35 or 55oC) or substrate type (single or co-substrate) on
methane percentage in biogas composition were not statistically significant (Appendix C.4).
On the other hand, there was a statistically significant (p < 0.05) increase in methane
percentage from the 20-d to the 10-d SRT, for both the mesophilic and thermophilic
digesters. As an example of this percentage increase, methane content in digester fed with
1+2+SC+L went from 66 ± 5% to 69 ± 1% as SRT was reduced from 20 to 10 days.

65
Table 4.8 Biogas composition of single and co-digesters during steady state
20-d SRT*
Mesophilic Thermophilic
(%) 1 2 1+2+L 1+2+SC+L 1 2 1+2+L 1+2+SC+L
CH4 68 ± 2† 63 ± 3 66 ± 4 66 ± 5 62 ± 2 67 ± 3 63 ± 11 66 ± 0
CO2 29 ± 1 20 ± 1 27 ± 4 27 ± 3 23 ± 1 25 ± 1 24 ± 4 24 ± 1
O2 1±0 2±0 1±0 1±0 4±0 1±3 5±2 2±1
N2 2±1 15 ± 3 6±1 6±2 11 ± 2 8±2 8±5 8±1
10-d SRT
CH4 69 ± 2 65 ± 2 68 ± 1 69 ± 1 70 ± 5 68 ± 4 68 ± 1 66 ± 2
CO2 28 ± 1 23 ± 2 26 ± 1 26 ± 1 25 ± 3 19 ± 3 26 ± 1 26 ± 1
O2 0±0 2±1 1±0 1±0 1±1 4±3 1±0 2±0
N2 3±1 10 ± 2 5±1 4±1 4±2 9±2 5±1 6±2
*SRT: sludge retention time
†Data represent the arithmetic mean of 22 replicates collected during steady state ± standard deviation

4.5 Effect of addition of co-digestion materials on digester supernatant


characterization

Digester stabilization was also monitored with respect to pH, as well as TVFA, alkalinity,
ammonia concentrations that were measured from supernatants of the digester effluents.
Methanogens are sensitive to acidic or basic environments; a safe pH range is between 6.5
and 8.5 (Tchobanoglous et al., 2004). Table 4.5 showed that, at 20-d SRT, pH values were
not affected by TVFA presence. For all digesters, both mesophilic and thermophilic, TVFA
values were under 250 mg/L, which is considered a safe range for anaerobic respiration
(Tchobanoglous et al., 2004). However, for 10-d SRT, TVFA values were above 250 mg/L
(Table 4.6). At the same time, for the majority of the digesters, alkalinity values were high
enough to keep the TVFA: alkalinity ratios between 0.01-0.3, less than the suggested limits
for digester failure (0.3-0.4; Droste 1997), with the exception of the single substrate digester
2, which had a TVFA: alkalinity ratio of 0.5. In this study, alkalinity measurements were in
the expected range of 2,097 to 5,958 mg CaCO3/L, similar to Venkateswara et al. (2011)
results with their co-digested reactors (2,250-5,000 mg/L). Bouallagui et al. (2009) co-
digested fruit and vegetable waste obtaining alkalinity values between 850-4,400 mg/L

66
(mesophilic) and 1,200-10,500 mg/L (thermophilic). Nevertheless, the results indicated that
for a full-scale digester fed with industrial TWAS, it might be necessary to add external
buffer solutions to stay below the TVFA: alkalinity ratio of 0.3 for a 10-d SRT. Between the
SRTs of 20 and 10 days, since the loading rate is doubled and the pH is on acidic side, the
alkalinity initially present will be consumed at a much faster rate, comprising the stability.

Alkalinity values in the thermophilic digesters were higher compared to the mesophilic ones.
This phenomenon was partly due to higher alkalinity originally present in the thermophilic
inoculum. In addition, there is equilibrium between the digester alkalinity and carbon dioxide
content in headspace. A stable digester will have pH and alkalinity ranges of 6.8-7.5 and
1,000-5,000 mg/L, respectively (Grady et al., 1999). Table 4.9 shows the effect of pH on the
alkalinity of the liquid and the carbon dioxide content of the gas phase in the anaerobic
process. High alkalinity concentrations will decrease carbon dioxide going into gas phase as
it is shown in Table 4.9 (thermophilic digesters).
Table 4.9 Relationship between theoretical and experimental CO2 content (%) in digester
headspace
CO2 in digester gas (%)

Mesophilic (35oC) Thermophilic (55oC)

pH Theoretical† Experimental pH Theoretical† Experimental

*SRT of 20 days
1 7.37(0.16) 23 29(1) 7.92(0.15) 9 23(1)
2 7.26(0.16) 24 20(1) 7.83(0.13) 7 13(2)
1+2+L 7.48(0.16) 27 27(4) 7.98(0.24) 7 24(4)
1+2+SC+L 7.50(0.17) 26 27(3) 8.12(0.12) 7 24(1)
*SRT of 10 days
1 7.48(0.09) 19 28(1) 7.93(0.09) 9 25(3)
2 6.99(0.27) 29 23(2) 7.71(0.17) 9 19(3)
1+2+L 7.59(0.09) 28 26(1) 8.17(0.07) 7 26(1)
1+2+SC+L 7.68(0.10) 28 26(1) 8.20(0.15) 7 26(1)
*SRT: sludge retention time. Data represent the arithmetic mean of 74 replicates for 20-d SRT, and
38 replicates for 10-d SRT, collected during steady state (standard deviation)
†Derived using effect of pH on the carbonate alkalinity of the liquid and the carbon dioxide content
(Grady et al., 1999)

67
Ammonia is generated by biodegradation of nitrogenous matter (i.e. proteins and urea)
during digestion and high amounts of ammonia could inhibit methanogenic bacteria (Demirel
and Scherer, 2008). Due to this concern, ammonia monitoring was done during this study
(Tables 4.6-4.7). Higher ammonia was generated in thermophilic digesters compared to
mesophilic digesters based on the data. Anaerobic treatment ammonia toxicity limit is around
2,000 mg/L (Bouallagi et al., 2009), causing a decrease in biogas production. On the other
hand, there are conflicting studies in the literature reporting that some of the methanogenic
strains are able to tolerate ammonia levels higher than 10,000 mg/L (Jarrel et al., 1987). In
this study, the ammonia levels in all of the digesters during the 20-d SRT were below the
toxicity limit of 2,000 mg/L. On the other hand, for the 10-d SRT, the ammonia levels in all
thermophilic digesters (except T-2) were slightly above the ammonia toxicity limit as
concentrations ranged in 2,100-2,300 mg/L. The fact that single digesters fed with industrial
TWAS (2) did not have alarming ammonia concentrations confirms that the instability of
these digesters observed at an SRT of 10 days was not due to ammonia inhibition.

Grady et al. (1999) explain that alkalinity, pH, and ammonia concentrations are
interconnected in anaerobic digestion. Different total ammonia concentrations can result in a
toxic free ammonia concentration (100 mg/L as N), depending on the pH and temperature.
The influence of pH is largely due to its effect on the equilibrium between dissolved
ammonia gas (free ammonia in more toxic form) and ammonium ions. Table 4.10 describes
the effect of pH and temperature on total ammonia concentrations necessary to release toxic
free ammonia concentration of 100 mg/L in the system. It is clear that mesophilic digesters
were below the maximum total ammonia concentration limits at corresponding digester pH
values, confirming stability of the system, while thermophilic digesters were above the
estimated total ammonia concentration limits for stable operation. However, thermophilic
digesters were able to tolerate ammonia concentrations with no negative effect on biogas or
methane production. This could be due to 3 months of inocula acclimation provided for all
the digesters including thermophilic digesters prior to actual digester set-up.

68
Table 4.10 Comparison between theoretical total ammonia toxicity limit with measured total
ammonia concentrations

Total ammonia concentration (mg/L as N)

Mesophilic (35oC) Thermophilic (55oC)

pH Maximum† Experimental pH Maximum† Experimental

*SRT of 20 days
1 7.37(0.16) 4,400 1,476 ± 392 7.92(0.15) 1,800 1,588 ± 542
2 7.26(0.16) 5,900 772 ± 184 7.83(0.13) 2,000 1,057 ± 355
1+2+L 7.48(0.16) 3,600 1,161 ± 258 7.98(0.24) 1,500 1,475 ± 465
1+2+SC+L 7.50(0.17) 3,600 1,235 ± 342 8.12(0.12) <500 1,406 ± 422
*SRT of 10 days
1 7.48(0.09) 3,600 1,764 ± 342 7.93(0.09) 1,800 2,368 ± 413
2 6.99(0.27) 11,000 849 ± 102 7.71(0.17) 900 1,475 ± 196
1+2+L 7.59(0.09) 2,950 1,485 ± 262 8.17(0.07) <500 2,178 ± 261
1+2+SC+L 7.68(0.10) 2,500 1,641 ± 194 8.20(0.15) <500 2,171 ± 260
*SRT: sludge retention time
†Total ammonia concentration necessary to give a toxic, free ammonia concentration of 100 mg N/L
This is calculated based on dissociation of ammonia as a function of digester pH and temperature
(Grady et al., 1999)

4.6 Land application of digested biosolids according to regulations

Agriculture is not possible without nutrients present in the soils. As previously mentioned,
digestate may have significant nutrient values that can make it an ideal fertilizer. However,
agencies such as Environmental Protection Agency (EPA) or the BC Ministry of
Environment continue to create strict regulations for the land application of biosolids. These
regulations are selective according to the methods for processing, reuse and disposal of
biosolids. In the Province of BC, waste producers and users follow the Land Application
Guidelines for the Organic Matter Recycling Regulation (OMMR) and the Soil Amendment
Code for Practice established by BC Ministry of Environment (OMRR, 2008). Biosolids are
classified in the OMRR as either Class A or Class B, depending on the extent to which
quality criteria in terms of fecal coliforms, trace heavy metals and vector attraction are met.
Vector attraction represents the characteristics related to attraction of rodents, mosquitos, or
other organisms capable of transporting infectious agents. Satisfactory vector attraction can

69
be demonstrated if treatment processes applied to waste sludge can reduce the VS content by
a minimum of a certain percentage, i.e. 38%. In this study, digested biosolids were quantified
in terms of coliforms and dewaterability characteristics, another important factor for easier
handling.

Although, heavy metals presences are the major restriction that prevents the agricultural use
of some sludges (Wang et al., 2006; OMMR 2008), heavy metals were not tested for the
digested biosolids for the following reasons. Both City of Kelowna and BCTTP monitor the
heavy metals in their waste streams (dewatered sludge cake, industrial TWAS and landfill
leachate) to comply with OMRR. The average metal concentrations listed for the waste
streams in Appendix D allowed us to set-up mass balances for metal concentrations entering
to the digesters. As metals do not undergo biodegradation during anaerobic digestion, and
also are not volatile, there will not be any decrease in concentrations during biological or
physiochemical reactions. As digesters showed around 40-50% volume reductions during the
digestion, it is expected that the concentrations of metals will be accumulated by 40-50% in
the digested biosolids samples. The calculated concentrations tabulated in Appendix D along
with the Class A and Class B criteria indicated that digested biosolids are expected to meet
Class A criteria in terms of metal contents (OMMR, 2008).

4.6.1 Dewaterability

In order to follow OMRR regulation, biosolids should be dewatered for land application. It is
expected that biosolids could be up to 25% of dry matter (OMRR, 2008). Dewatering reduces
water content in biosolids, reducing final volumes for better handling (Radaideh et al., 2010).
One of the methods to measure dewaterability is CST, which provides a quantitative measure
of how readily sludge releases its water. Dewaterability results provide information such as
sludge conditioning, coagulation effects and settleable solids.

During anaerobic digestion, there is an agglomeration of particles resulting in a disturbance


in the particle size distribution. When the anaerobic digestion process is completed, particles
are destroyed, with a removal of small sizes (Lin et al., 1997), leading to the presence of
created biopolymer colloids (Radaideh et al., 2010). Hence, anaerobic digestion reduces the
dewatering rate of sludge. In this study, the dewaterability of digestate was measured at the

70
end of each SRT period when the digesters were at the steady-state by a capillary suction
timer at room temperature (21 ± 1oC). The CST results (in seconds) normalized by the TS
concentrations in digested biosolids (Figure 4.6) showed that digesters fed with industrial
TWAS (2) needed the lowest time in releasing its water, indicating the best dewaterability
among different digester scenarios under both mesophilic and thermophilic conditions. Also,
mixed sludge dewaterability was lower compared to digesters fed with dewatered municipal
sludge cake only due to the presence of industrial TWAS. This could be caused by the
presence of cellulose and polymers in the industrial TWAS stream. Organic polymers are
widely used as sludge conditioners, improving dewaterability. These polymers generate less
solid cake volume after dewatering (Lee and Liu, 2001). Furthermore, these results are in
agreement with previous studies that observed better dewaterability from sludge generated in
extended aerated biological treatment units, similar to one at BCTTP. Literature indicates
that extended aeration sludge with low food to microorganism rations may produce better
flocculated particles that result in smaller fraction of finer than anaerobically digested sludge
(Radaideh et al., 2010).

The SCOD results had the same pattern as dewatering. The presence of soluble inorganic
materials interferes easily with the dewatering of digestates. These inorganic small particles
had higher contact surface area, slowing the dewatering process. As is shown in Figure 4.7,
higher SCOD content was present in the thermophilic digesters, specifically in digesters fed
with diluted municipal sludge cake (1). It is well established in the literature that
thermophilic digestates are harder to dewater due to the presence of small particles having a
higher specific surface area (Lin et al., 1997). The results generated as part of this study were
in agreement with the literature, consistently yielding in better dewaterability for the
mesophilic digesters than those of thermophilic at both SRTs except the single digester fed
with industrial TWAS (2) at SRT of 10 days. Overall, the results indicate that the addition of
industrial TWAS to other waste streams can enhance the dewaterability by acting as a
conditioner polymer.

71
Mesophilic Thermophilic

10000
Capillary suction time (s/g TS)

1000

100

10

1
1 2 1+2 1+2+SC 1 2 1+2 1+2+SC
Single digestion Co-digestion Single digestion Co-digestion
SRT = 20 d SRT = 10 d

Figure 4.6 Dewaterability analysis results of single and co-digested samples (data represent the
mean and error bars represent the standard deviation of 9 replicates, SRT: sludge retention
time, TS: total solids)

Mesophilic Thermophilic
7000
SCOD present in digestate (mg/L)

6000

5000

4000

3000

2000

1000

0
1 2 1+2 1+2+SC 1 2 1+2 1+2+SC
Single digestion Co-digestion Single digestion Co-digestion
SRT = 20 d SRT = 10 d

Figure 4.7 SCOD analysis results of single and co-digested samples (data represent the mean
and error bars represent the standard deviation of 74 and 38 replicates for 20 and 10 days SRT,
respectively, SRT: sludge retention time, SCOD: soluble chemical oxygen demand)

72
4.6.2 Pathogens

Biosolids are known to contain pathogens; therefore, digestates must be tested for the safety
of both people and animals. According to OMRR (2008), Class A biosolids contain lower
counts of fecal coliforms (<1,000 Most probable number or MPN fecal coliforms/g dry
weight), meaning that they are higher quality biosolids with more liberal distribution
allowance. Class B biosolids are allowed to contain more fecal coliforms (<2,000,000 MPN
fecal coliforms/g dry weight). Therefore, Class B biosolids are subjected to more land
application and distribution restrictions.

Table 4.11 summarizes previous studies of coliform presents in different sources of


digestates. Based on the source of the substrate, digestates may have higher or lower coliform
content, an important factor for inactivation of pathogens. Also, temperature of treatment is
another important factor for the decay rate of pathogens. Other critical factors of decay rate
of pathogenic bacteria are: pH, VFA concentration, bacterial species, nutrients concentration,
and treatment time (Salström, 2003).

For anaerobic digestion, digester temperature and retention time are the factors that
determine pathogen inactivation. The time required for pathogen inactivation is known as
decimation reduction time. For many bacteria in thermophilic environment, their reduction
time could be hours while for a mesophilic environment, the reduction time could be days
(Salström, 2003). Since temperature helps to decrease the decimation reduction time, it is
expected that the thermophilic digestates will contain lower coliforms. Table 4.11 shows that
thermophilic digestions were the ones with lower coliform content in most of the previous
studies. Overall the results from literature indicated that higher SRTs and elevated digester
temperature lower pathogens concentrations in digested samples for land application.

73
Table 4.11 Summary of different substrates and digestion techniques with their total fecal
coliform presence

Total fecal
Type of
Author Type of feed SRT* coliforms
digestion
(MPN/g TS†)
Primary and
Aitken et al., Anaerobic-
waste activated 6d 81.3-1905
2005 thermophilic
sludge
Anaerobic- 20 d >1×108
Primary sludge mesophilic 10 d >1×108
Coelho et al.,
and activated Anaerobic-2-
2011 20 d <100
sludge stage
10 d >1×104
thermophilic
Anaerobic-
Primary and 1.1×104-2×106a
Kabrick & mesophilic
waste activated 20 d
Jewell, 1982 Aerobic-
sludge 1×103-7×104a
thermophilic
Anaerobic-
1×104-1×105
Rojas Oropeza Municipal mesophilic
16 d
et al., 2001 sludge Anaerobic-
<103
thermophilic
Sahlström et al., Municipal Anaerobic-
20 d 174,463-35,258a
2004 sludge mesophilic
*SRT: Sludge retention time
†MPN/100mL, SRT: sludge retention time, TS: total solids, MPN: most probable number
a
Total coliforms

This study had the same pattern, as it is shown in Figure 4.8, where mesophilic digesters had
consistently higher total coliform content (8,838 to 37,959 MPN/g TS) compared to
thermophilic digesters (41 to 1,090 MPN/g TS) at both SRT of 20 and 10 days. The lowest
total coliform content (41 MPN/g TS) was in the thermophilic digester fed with the industrial
TWAS (2), due to its source (free of human residuals). The coliform content in all the

74
mesophilic digestates were above the Class A biosolids; therefore, they could be classified as
Class B biosolids (OMRR, 2008).

For thermophilic digesters, except the digester fed with a mixture of 1+2+SC+L, all
digestates could be qualified as Class A biosolids even at an SRT of 10 days. These results
are in agreement with the literature indicating that an SRT of 10 days could provide adequate
pathogen destruction under thermophilic temperatures (Salström, 2003). Furthermore, these
coliform results confirmed that the mesophilic temperature of 35oC is not effective in
pathogens reduction. Hence, a minimum of SRT for mesophilic should be 20 d (Salström et
al., 2004). It is important to note that OMRR (2008) regulations are based on fecal coliform
(associated with human or animal waste) and not total coliform content. However, in this
study, the method used was able to quantify total coliforms as well as E. coli, part of the
group of fecal coliforms. Thus, the assessment made based on the total coliforms, displayed
in Figure 4.8, is conservative as fecal coliforms are expected to be lower than the total
coliforms in digestate samples. If this point is taken into account, there is a higher level of
confidence that regardless of the digestion scenario implemented at the full-scale, digested
biosolids will be qualified either under Class A or Class B, therefore, will be suitable for land
application.

75
Mesophilic Thermophilic

2000000 MPN/g dry weight, Class B biosolids (OMRR 2008)

1000000
1000 MPN/g dry weight, Class A biosolids (OMRR 2008)
Total coliforms (MPN/g TS)

100000

10000

1000

100

10

1
1 2 1+2 1+2+SC 1 2 1+2 1+2+SC
Single digestion Co-digestion Single digestion Co-digestion
SRT = 20 d SRT = 10 d

Figure 4.8 Coliform content of effluents from anaerobic digesters, at 20 d and 10 d SRT with
Class A limit regulation (data represent the mean and error bars represent the standard
deviation of 8 replicates, SRT: sludge retention time, MPN: most probable number, TS: total
solids)

4.7 Approximate cost functions for single and co-digestion treatment facilities

Planning municipal and industrial solid waste management systems requires quantitative
estimates of capital and operational costs. Cost estimation for anaerobic digestion facility is
complex and requires design by engineers from different disciplines (environmental,
structural, mechanical and electrical). In order to evaluate the cost analysis, the facility is
viewed as a system, consisting of components or subsystems (Tsilemou, 2002).

Although cost analysis was initially not within the scope of this study, it was decided to
attempt to calculate potential savings in both capital as well as long term (25 years)
operational cost if City of Kelowna and Sun-Rype Beverage Ltd. decided to build a co-
digester utilizing all municipal and industrial streams. This was made possible by the capital

76
and operational cost functions suggested by Tsilemou and Panagiotakopoulus (2006) as a
function of anaerobic digester design capacity. The cost functions are shown in Figure 4.9.
A B
0,5 10000

Operating cost (€/ton )


Initial cost (106 € )

0,4 8000

0,3 6000
y = 0,0342x0,55 y = 16722x-0,61
0,2 4000
R2= 0.92 2000 R2= 0.94
0,1
0 0
0 50 100 150 0 50 100 150
Design capacity (103 tons/year) Capacity (inflow 103 tons/yeat)

Figure 4.9 A) Initial and B) operating cost functions of anaerobic digestion facilities (adapted
from Tsilemou and Panagiotakopoulus, 2006)

In this study, cost components such as facility size, inflowing waste composition, operational
conditions, number of employees, quantities of recovered material, compost and energy,
recovery coefficients, number and size of equipment units, land area, among other
parameters, are studied for different solid waste management systems, including anaerobic
digestion (Tsilemou and Panagiotakopoulus, 2006). Assumptions made by Tsilemou and
Panagiotakopoulus (2006) for cost functions were as follows.

Cost functions were based on thermophilic dry one-stage digestion.

Digesters receive source-separated biodegradable waste (i.e. source-separated


municipal solids waste, bio-waste with sludge, bio-waste mixed with garden waste or
food industry waste.

Initial (capital cost) includes predevelopment costs (site characterization,


environmental assessment, hydrogeological investigation, land acquisition,
engineering design) + construction costs (land cleaning, excavation, buildings/other
construction works), equipment and furnishing of facilities, technical equipment for
waste transport and energy recovery, connecting networks (access roads, water &
energy supply, sewerage system).

77
Operating cost includes expenses for raw materials, laboratory tests (reagent,
chemicals, etc.), energy and other utilities, wastewater disposal, labor, supervision,
maintenance, insurance, overheads, training programs.

The operating cost does include capital recovery cost via biogas or fertilizer.

The results are displayed in Table 4.12. Methane production was calculated based on
experimental methane yield obtained in this study (L/g VSadded, Table 4.6). Preliminary cost
analysis results indicated an overall saving of $10.52 million ($2 million in capital and $8.52
million in operational) over 25 years period for co-digestion scenario utilizing all waste
streams over building/operating two separate digesters for municipal and industrial waste
streams. In addition, the, unit operation cost ($/ton) for only industrial TWAS +SC will be
almost 5 times ($272.02 to $54.29, respectively) higher than the co-digester utilizing all the
waste streams due to much lower digester capacity utilizing the industrial streams. Therefore,
the results from this study confirm that co-digestion has lower unit cost due to sharing of
facility and operation. It is important to emphasize that due to the cost functions based on
European sites, it is expected that the capital and operational costs will vary for Canada. For
anaerobic digesters, the cost is influenced by the pretreatment/characteristics of waste,
volume and quality (energy content) of biogas that are determined by regulations in different
countries. Therefore it is difficult to estimate the uncertainty of using European cost
functions in the cost analysis for the Canadian waste treatment sector.

78
Table 4.12 Estimated cost items for single and co-digestion reactors*

Single digesters Co-digesters Two single digesters


(one for municipal
Sludge Industrial Industrial Industrial TWAS Sludge cake Sludge cake + sludge cake and one
cake TWAS* SC + SC + TWAS TWAS + SC for industrial TWAS
combined with SC)
Sludge production rate
60.0 25.5 0.14 25.6 85.50 85.6 85.6
(wet ton/d)
Total solids (%, w/w) 17.4 2.8 21.0 2.9 13.1 13.1
Total solids produced (dry
10.44 0.71 0.03 0.74 11.15 11.21 (10.44) + (0.74)
ton/d)
Volatile solids (%, w/w) 15.0 2.4 19.0 2.5 11.2 11.23
Volatile solids produced
9.00 0.61 0.03 0.64 9.61 9.64 (9.00) + (0.64)
(dry ton/d)
Digester volume† (m3) 3,214 218 9.5 228 3,433 3,442 (3,214) + (228)
Annual CH4 production
722,700 35,741 not tested not tested 806,927 879,522
(m3/year)a
Design capacity (ton/year) 19,053 1,303 1,357 20,356 20,410 (19,053) + (1,357)
Capital cost (million $)c 10.24 2.34 2.39 10.62 10.63 (10.24) + (2.39) = 12.63
Unit operation cost ($/ton)c 54.29 278.83 272.02 52.14 52.06
Operating cost (million
1.03 0.36 0.37 1.06 1.06 (1.03) + (0.37) = 1.4
$/year)

Total operating cost (25


25.85 9.08 9.23 26.53 26.56 (25.85)+ (9.23)= 35.08
years, million $)

Total capital & operating (36.10) + (11.62) =


36.10 11.42 11.62 37.15 37.19
cost (25 years, million $) 47.72
Gas purification (million
1.5 1.5 1.5 1.5 1.5
$)² optional

79
Two single digesters
(one for municipal
Sludge Industrial Industrial Industrial TWAS Sludge cake Sludge cake +
sludge cake and one
cake TWAS* SC + SC + TWAS TWAS + SC
for industrial TWAS
combined with SC)
Revenue calculated from digestate to be sold as Ogogrow© fertilizer
Annual Ogogrow
11,677.63 1,491.06 12,634.52 12,175.63
production (wet ton/year)
Revenue gained ($/year)2 346, 479 44,240 374,870 361,255
Revenue gained (25 yrs.,
8.66 1.11 9.37 9.03
million $)
Revenue calculated from biogas assuming biogas is purified to bio-methane quality (96% methane)
Energy (GJ/year) 24,692 1,221 27,570 30,049
3
Energy value ($/GJ) 11 11 11 11
Revenue gained ($/year) 271,610 13,432 303,265 330,548 287,378
Revenue gained (25 yrs.,
6.79 0.34 7.58 8.26 7.18
million $)
Revenue calculated from biogas generation assuming biogas is NOT purified to bio-methane quality (60-70% methane)
Energy (GJ/year) 24,692 1,221 27,570 30,049
Energy value ($/GJ)3 2.5 2.5 2.5 2.5
Revenue gained ($/year) 61,729 3,053 68,924 75,124 65.313
Revenue gained (25 yrs.,
1.54 0.08 1.72 1.88 1.63
million $)
*TWAS: thickened waste activated sludge, SC: screen cake, TS: total solids, VS: volatile solids, SRT: sludge retention time
†Digester volume is calculated based on organic loading rate (OLR) of 2.80 kg VS/m3 × day
a
Based on the experimental specific methane yields obtained in Table 4.15 for thermophilic digesters at SRT of 20 days
c
Digester capital and operational cost functions are based on Tsilemou and Panagiotakopoulus (2006). Currency conversion rate: 1.3249 CAD/Euro (March
26th, 2013)
2
Ogogrow selling price of $13.5 per cubic yard at total solid concentration of 20-30% by weight (City of Kelowna, 2013)
3
Personal communication (Fortis BC, 2013)

80
Chapter 5: Conclusions and recommendations

5.1 Conclusions

This research explored the potential of using co-digestion for sewage sludge cake, fruit juice
thickened waste activated sludge and screen cake, diluted with landfill leachate. The study
started with acclimation of mesophilic and thermophilic inocula to a mixture of waste
streams. Upon achieving steady state during acclimation phase, eight lab-scale digesters were
set-up with acclimatized inocula to assess performances from different single and co-
digestion scenarios. Total duration of digestion studies was 7 months. Upon experimental
work, organic loading rates and methane yields obtained were used to calculate full-scale
digester volumes and revenue to be generated from methane recovered from waste streams.
Based on the experimental data and analysis, the following conclusions were drawn:

1. Among the single digestion scenarios, fruit-juice TWAS achieved the lowest
biodegradation efficiency, and therefore lowest methane yield due to higher level of
refractory compounds present. This was highly likely linked to the extended aeration
(long SRT & Hydraulic retention time) operation regime of the activated sludge
process at BCTTP.
2. Specific biogas yields from waste streams were close or higher than literature values
reported for similar substrates (~1 L/ g VS removed). All single and co-digestion
scenarios achieved steady state at SRTs of 20 and 10 days, corresponding to OLRs of
1.41-4.38 g COD/L × d, except for the fruit-juice TWAS. The steady state was
achieved after 15 and 5 days of operation, for 20 and 10 days SRT, respectively. SRT
is fixed value for a certain operation condition. At an SRT of 10 days, the biogas
production from TWAS digesters started declining after 20 days of digestion at both
mesophilic and thermophilic temperatures.
3. On the other hand, addition of municipal sludge cake and particularly landfill leachate
to fruit-juice waste streams enhanced the co-digestion due to additional buffering
capacity and less refractory organics provided by landfill leachate and municipal
sludge cake, respectively. Due to this feature, co-digestion digesters were stable even
at the higher organic loadings without accumulation of VFA leading to pH drop.

81
4. Single and co-digestion scenarios presented statistically significant differences (p <
0.05 for TS and p ≤ 0.05 for VS removals, respectively), suggesting that co-digestion
has a better performance than the single digestion in terms of solid removal
efficiencies. However, the effects of digestion temperature (mesophilic or
thermophilic) and SRT (20-d or 10-d) were not significantly different.
5. Thermophilic digesters yielded total ammonia concentrations higher than the
maximum limit to release toxic free ammonia of 100 mg/L at corresponding reactor
pH and temperature. However, thermophilic digester did not experience any
inhibition possibly due to adequate acclimation period.
6. Despite the low biodegradability, fruit-juice TWAS indicated the fastest
dewaterability, therefore enhanced the dewaterability of digestates from co-digesters
utilizing mixture of municipal/industrial streams. These results are in agreement with
previous studies that observed better dewaterability from sludge generated in
extended aerated biological treatment units, similar to one at BCTTP.
7. According to OMRR of BC, all mesophilic digestate coliform concentrations were
under Class B biosolids limits. However, all thermophilic digestates could be
categorized under Class A biosolids.
8. Preliminary cost analysis indicated an overall saving of $10.52 million ($2 million in
capital and $8.52 million in operational) over 25 years period for co-digestion
scenario utilizing all waste streams over building/operating two separate digesters for
municipal and industrial waste streams. Therefore, the results from this study confirm
that co-digestion has lower unit cost due to sharing of facility and operation.

5.2 Recommendations for future work

To verify the conclusions presented in this study, it is recommended that the following
additional research be undertaken in the future:

1. Application of pretreatment methods such as ultrasound, alkaline, microwave, before


anaerobic digestion can be tested to increase the degradation of waste-streams.

82
2. In this study, metal concentrations in digestate samples were calculated based on the
data provided by the City of Kelowna and BCTTP for the influent waste streams. It is
recommended that these concentrations are experimentally verified.
3. Due to seasonal variation in the industrial waste streams, it is recommended to verify
the biogas and methane yields obtained from this study (performed during spring and
fall months) with future set of digesters utilizing waste sampled during winter
months.
4. Concentration of H2S in the biogas should be measured to assess the suitability of the
biogas for energy utilization and risk of corrosion for the biogas recovery system.
5. A pilot plant study should be conducted to simulate the actual plant process condition
(e.g. to avoid mixing by shaker) and for better economic analysis of the process to
reduce the effect of scale-up from shake flask to real digester.

83
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Appendices

Appendix A: Calibration curves

450
400
Air volume in manometer (mL)

350
300
y = 0,8051x + 0,8204
250 R² = 0,9999

200 Volume

150 Lineal (Volume)

100
50
0
0 100 200 300 400 500 600
Injected air volume(mL)

Figure A.1 Calibration curve for biogas measurement via manometer (STP)

0,6

0,5
Concentration (mg/L)

0,4
y = 0,0007x
R² = 0,9998
0,3
COD
Lineal (COD)
0,2

0,1

0
0 200 400 600 800
Absorbance (600nm)

Figure A.2 Calibration curve for COD determination

95
NH3 probe reading (mV)
0
0 2 4 6 8
Concentration (lnC, mg/L)

-50
y = -24,038x - 26,609
R² = 0,9999
-100 Ammonia
Lineal (Ammonia)
-150

-200

-250

Figure A.3 Calibration curve for ammonia (NH3-N) determination

2,5

2
Absorbance at 420nm

1,5
y = 0,0136x
R² = 0,9908
Series1
1
Lineal (Series1)

0,5

0
0 50 100 150 200
concentration of TN (mg/L)

Figure A.4 Calibration curve for total nitrogen (TN) determination

96
Appendix B: Results summary of digesters fed with leachate

Table B.1 Results for semi-continuous digesters at 20d SRT

Parameter Mesophilic Thermophilic

Daily biogas production


25 ± 13† 23 ± 9
(mL/d)

TS (%w/w) 99 ± 24* 97 ± 21*

VS (%w/w) 54 ± 21* 52 ± 6*

TCOD (mg/L) 6,566 ± 3105 7,041 ± 3392

SCOD (mg/L) 1,108 ± 735 1,593 ± 659

CH4 (%) 33 ± 6 32 ± 2

pH 7.8 ± 0.1 8.3 ± 0.2

Ammonia (mg/L) 588 ± 361 726 ± 430

Alkalinity (mg CaCO3/L) 3,725 ± 399 4,106 ± 563

TVFA 2.4 ± 0.3 12.5 ± 0.2

*Total and volatile solids majority content were coming from inoculum. TS: total solids, VS: volatile
solids, TCOD: Total chemical oxygen demand, SCOD: soluble chemical oxygen demand, TVFA:
total volatile fatty acids
† Data represent the arithmetic mean of minimum of duplicates for loading rates and 20 replicates for
the remaining parameters collected during steady state (standard deviation)

97
Appendix C: ANOVA Analyses

C.1 TS % removal efficiency

Table C.1.1 TS% removal ANOVA analyses results for temperature and sludge retention time

Scenarios Mesophilic Thermophilic


1 (20-d) 36.75 ± 4.18 39.06 ± 5.78
2 (20-d) 27.66 ± 3.94 33.25 ± 5.77
1+2+L (20-d) 40.42 ± 6.71 40.95 ± 4.28
1+2+SC+L (20-d) 40.03 ± 3.66 43.21 ± 3.16
1 (10-d) 38.56 ± 4.12 42.02 ± 4.38
2 (10-d) 29.67 ± 4.13 39.78 ± 4.58
1+2+L (10-d) 42.28 ± 5.02 40.57 ± 3.59
1+2+SC+L (10-d) 43.71 ± 6.80 40.69 ± 3.55

Table C.1.2 ANOVA: two-factor with replication TS% removal results for temperature and
sludge retention time

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 136.43 149.59 286.02
Average 34.11 37.40 35.75
Variance 101.11 56.91 70.82

Count 4 4 8
Sum 148.09 163.06 311.14
Average 37.02 40.76 38.89
Variance 85.65 0.87 41.08

Count 8 8
Sum 284.51 312.65
Average 35.56 39.08
Variance 82.46 27.99

98
Table C.1.3 ANOVA analysis TS% removal results for temperature and sludge retention time

Source of variation SS df MS F P-value F-critic


Sample 39.44 1 39.44 0.65 0.44 4.75
Columns 49.48 1 49.48 0.81 0.39 4.75
Interaction 0.20 1 0.20 0.003 0.95 4.75
Within 733.59 12 61.13
Total 822.72 15

Table C.1.4 TS% removal ANOVA analyses results for sludge retention time and temperature

Scenarios 20-d 10-d


M-1 36.75 ± 4.18 38.56 ± 4.12
M-2 27.66 ± 3.94 29.67 ± 4.13
M-1+2+L 40.42 ± 6.71 42.28 ± 5.02
M-1+2+SC+L 40.03 ± 3.66 43.71 ± 6.80
T-1 39.06 ± 5.78 42.02 ± 4.38
T-2 33.25 ± 5.77 39.78 ± 4.58
T-1+2+L 40.95 ± 4.28 40.57 ± 3.59
T-1+2+SC+L 43.21 ± 3.16 40.69 ± 3.55

Table C.1.5 ANOVA: two-factor with replication TS% removal results for sludge retention
time and temperature

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 136.43 148.09 284.51
Average 34.11 37.02 35.56
Variance 101.11 85.65 82.46

Count 4 4 8
Sum 149.59 163.06 312.65
Average 37.40 40.76 39.08
Variance 56.91 0.87 28.00

Count 8 8
Sum 286.02 311.14
Average 35.75 38.89
Variance 70.82 41.08

99
Table C.1.6 ANOVA analysis removal results for sludge retention time and temperature

Source of variation SS df MS F P-value F-critic


Sample 49.48 1 49.48 0.81 0.39 4.75
Columns 39.44 1 39.44 0.65 0.43 4.75
Interaction 0.20 1 0.20 0.003 0.95 4.75
Within 733.59 12
Total 822.72 15

Table C.1.7 TS% removal ANOVA analyses results for single to co-digestion, and sludge
retention time

Scenarios Single Co-digestion


M-1 / M-1+2 +L (20-d) 36.75 ± 4.18 40.42 ± 6.71
M-2 / M-1+2+SC+L (20-d) 27.66 ± 3.94 40.03 ± 3.66
T-1 / T-1+2+L (20-d) 39.06 ± 5.78 40.95 ± 4.28
T-2 / T-1+2+SC+L (20-d) 33.25 ± 5.77 43.21 ± 3.16
M-1 / M-1+2 +L (10-d) 38.56 ± 4.12 42.28 ± 5.02
M-2 / M-1+2+SC+L (10-d) 29.67 ± 4.13 43.71 ± 6.80
T-1 / T-1+2+L (10-d) 42.02 ± 4.38 40.57 ± 3.59
T-2 / T-1+2+SC+L (10-d) 39.78 ± 4.58 40.69 ± 3.55

Table C.1.8 ANOVA: two-factor with replication TS% removal results for single to co-
digestion, and sludge retention time

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 121.41 164.61 286.02
Average 30.35 41.15 35.75
Variance 85.47 2.03 70.82

Count 4 4 8
Sum 143.89 167.25 311.14
Average 35.97 41.81 38.89
Variance 70.89 2.22 41.08

Count 8 8
Sum 265.30 331.86
Average 33.16 41.48
Variance 76.03 1.95

100
Table C.2 ANOVA analysis removal results for single to co-digestion, and sludge retention time

Source of variation SS df MS F P-value F-critic


Sample 39.44 1 39.44 0.98 0.34 4.75
Columns 276.90 1 276.90 6.90 0.02 4.75
Interaction 24.57 1 24.57 0.61 0.45 4.75
Within 481.80 12 40.15
Total 822.72 15

101
C.2 VS % removal efficiency

Table C.2.1 VS% removal ANOVA analyses results for temperature and sludge retention time

Scenarios Mesophilic Thermophilic


1 (20-d) 43.01 ± 2.26 46.62 ± 3.64
2 (20-d) 36.81 ± 6.80 41.04 ± 5.25
1+2+L (20-d) 50.21 ± 2.64 51.02 ± 4.12
1+2+SC+L (20-d) 44.20 ± 4.41 49.22 ± 2.60
1 (10-d) 47.39 ± 3.67 49.07 ± 4.29
2 (10-d) 39.05 ± 6.35 40.96 ± 5.57
1+2+L (10-d) 47.32 ± 3.00 48.25 ± 2.27
1+2+SC+L (10-d) 46.28 ± 2.82 47.24 ± 4.31

Table C.2.2 ANOVA: two-factor with replication VS% removal results for temperature and
sludge retention time

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 159.24 177.90 337.14
Average 39.81 44.47 42.14
Variance 153.85 83.46 107.92

Count 4 4 8
Sum 175.04 195.52 370.57
Average 43.76 48.88 46.32
Variance 42.13 2.48 26.61

Count 8 8
Sum 334.28 373.42
Average 41.78 46.68
Variance 88.45 42.38

102
Table C.2.3 ANOVA analysis VS% removal results for temperature and sludge retention time

Source of variation SS df MS F P-value F-critic


Sample 69.83 1 69.83 0.99 0.34 4.75
Columns 95.74 1 95.74 1.36 0.27 4.75
Interaction 0.21 1 0.21 0.003 0.95 4.75
Within 845.77 12 70.48
Total 1011.55 15

Table C.2.4 VS% removal ANOVA analyses results for sludge retention time and temperature

Scenarios 20-d 10-d


M-1 43.01 ± 2.26 47.39 ± 3.67
M-2 36.81 ± 6.80 39.05 ± 6.35
M-1+2+L 50.21 ± 2.64 47.32 ± 3.00
M-1+2+SC+L 44.20 ± 4.41 46.28 ± 2.82
T-1 46.62 ± 3.64 49.07 ± 4.29
T-2 41.04 ± 5.25 40.96 ± 5.57
T-1+2+L 51.02 ± 4.12 48.25 ± 2.27
T-1+2+SC+L 49.22 ± 2.60 47.24 ± 4.31

Table C.2.5 ANOVA: two-factor with replication VS% removal results for sludge retention
time and temperature

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 159.24 175.04 334.28
Average 39.81 43.76 41.79
Variance 153.85 42.13 88.45

Count 4 4 8
Sum 177.90 195.52 373.42
Average 44.47 48.88 46.68
Variance 83.46 2.48 42.38

Count 8 8
Sum 337.14 370.57
Average 42.14 46.32
Variance 107.92 26.61

103
Table C.2.6 ANOVA analysis results for sludge retention time and temperature

Source of variation SS df MS F P-value F-critic


Sample 95.74 1 95.74 1.36 0.27 4.75
Columns 69.83 1 69.83 0.99 0.34 4.75
Interaction 0.21 1 0.21 0.003 0.95 4.75
Within 845.77 12 70.48
Total 1011.55 15

Table C.2.7 VS% removal ANOVA analyses results for single to co-digestion, and sludge
retention time

Scenarios Single Co-digestion


M-1 / M-1+2 +L (20-d) 43.01 ± 2.26 50.21 ± 2.64
M-2 / M-1+2+SC+L (20-d) 36.81 ± 6.80 44.20 ± 4.41
T-1 / T-1+2+L (20-d) 46.62 ± 3.64 51.02 ± 4.12
T-2 / T-1+2+SC+L (20-d) 41.04 ± 5.25 49.22 ± 2.60
M-1 / M-1+2 +L (10-d) 47.39 ± 3.67 47.32 ± 3.00
M-2 / M-1+2+SC+L (10-d) 39.05 ± 6.35 46.28 ± 2.82
T-1 / T-1+2+L (10-d) 49.07 ± 4.29 48.25 ± 2.27
T-2 / T-1+2+SC+L (10-d) 40.96 ± 5.57 47.24 ± 4.31

Table C.2.8 ANOVA: two-factor with replication VS% removal results for single to co-
digestion, and sludge retention time

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 142.49 188.01 330.50
Average 35.62 47.00 41.31
Variance 129.06 6.25 94.99

Count 4 4 8
Sum 181.47 195.73 377.20
Average 45.37 48.93 47.15
Variance 59.02 2.59 30.03

Count 8 8
Sum 323.96 383.74
Average 40.49 47.97
Variance 107.74 4.85

104
Table C.2.9 ANOVA analysis results for single to co-digestion, and sludge retention time

Source of variation SS df MS F P-value F-critic


Sample 136.31 1 136.31 2.77 0.12 4.75
Columns 223.39 1 223.39 4.54 0.05 4.75
Interaction 61.07 1 61.07 1.24 0.29 4.75
Within 590.77 12 49.23
Total 1011.55 15

105
C.3 TCOD % removal efficiency

Table C.3.1 TCOD% removal ANOVA analyses results for temperature and sludge retention
time

Scenarios Mesophilic Thermophilic


1 (20-d) 54.89 ± 4.58 58.06 ± 4.93
2 (20-d) 50.49± 14.13 55.57 ± 10.79
1+2+L (20-d) 56.58 ± 7.58 58.51 ± 6.81
1+2+SC+L (20-d) 58.54 ± 10.22 61.27 ± 7.94
1 (10-d) 45.95 ± 7.21 42.67 ± 5.01
2 (10-d) 31.62 ± 7.29 40.45 ± 10.07
1+2+L (10-d) 50.34 ± 3.34 46.90 ± 9.13
1+2+SC+L (10-d) 57.43 ± 4.38 50.76 ± 5.84

Table C.3.2 ANOVA: two-factor with replication TCOD% removal results for temperature and
sludge retention time

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 220.50 233.41 453.91
Average 55.13 58.35 56.74
Variance 11.79 5.45 10.37

Count 4 4 8
Sum 185.34 180.78 366.12
Average 46.34 45.19 45.76
Variance 118.64 20.92 60.18

Count 8 8
Sum 405.84 414.19
Average 50.73 51.77
Variance 77.98 60.77

106
Table C.3.3 ANOVA analysis TCOD% results for temperature and sludge retention time

Source of variation SS df MS F P-value F-critic


Sample 481.76 1 481.76 12.29 0.004 4.75
Columns 4.35 1 4.35 0.11 0.74 4.75
Interaction 19.08 1 19.08 0.49 0.49 4.75
Within 470.41 12 39.20
Total 975.61 15

Table C.3.4 TCOD% removal ANOVA analyses results for sludge retention time and
temperature

Scenarios 20-d 10-d


M-1 54.89 ± 4.58 45.95 ± 7.21
M-2 50.49± 14.13 31.62 ± 7.29
M-1+2+L 56.58 ± 7.58 50.34 ± 3.34
M-1+2+SC+L 58.54 ± 10.22 57.43 ± 4.38
T-1 58.06 ± 4.93 42.67 ± 5.01
T-2 55.57 ± 10.79 40.45 ± 10.07
T-1+2+L 58.51 ± 6.81 46.90 ± 9.13
T-1+2+SC+L 61.27 ± 7.94 50.76 ± 5.84

Table C.3.5 ANOVA: two-factor with replication TCOD% results for sludge retention time and
temperature

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 220.50 185.34 405.84
Average 55.13 46.33 50.73
Variance 11.79 118.64 77.98

Count 4 4 8
Sum 233.41 180.78 414.19
Average 58.35 45.19 51.77
Variance 5.45 20.92 60.77

Count 8 8
Sum 453.91 366.12
Average 56.74 45.76
Variance 10.37 60.18

107
Table C.3.6 ANOVA analysis results for sludge retention time and temperature

Source of variation SS df MS F P-value F-critic


Sample 4.35 1 4.35 0.11 0.74 4.75
Columns 481.76 1 481.76 12.29 0.004 4.75
Interaction 19.08 1 19.08 0.49 0.49 4.75
Within 470.41 12 39.20
Total 975.61 15

Table C.3.7 TCOD% removal ANOVA analyses results for single to co-digestion, and sludge
retention time

Scenarios Single Co-digestion


M-1 / M-1+2 +L (20-d) 54.89 ± 4.58 56.58 ± 7.58
M-2 / M-1+2+SC+L (20-d) 50.49± 14.13 58.54 ± 10.22
T-1 / T-1+2+L (20-d) 58.06 ± 4.93 58.51 ± 6.81
T-2 / T-1+2+SC+L (20-d) 55.57 ± 10.79 61.27 ± 7.94
M-1 / M-1+2 +L (10-d) 45.95 ± 7.21 50.34 ± 3.34
M-2 / M-1+2+SC+L (10-d) 31.62 ± 7.29 57.43 ± 4.38
T-1 / T-1+2+L (10-d) 42.67 ± 5.01 46.90 ± 9.13
T-2 / T-1+2+SC+L (10-d) 40.45 ± 10.07 50.76 ± 5.84

Table C.3.8 ANOVA: two-factor with replication TCOD% results for single to co-digestion, and
sludge retention time

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 182.95 222.89 405.84
Average 45.74 55.72 50.73
Variance 101.95 13.51 77.98

Count 4 4 8
Sum 196.75 217.44 414.19
Average 49.19 54.36 51.77
Variance 79.44 44.53 60.77

Count 8 8
Sum 379.70 440.
Average 47.46 55.04
Variance 81.14 25.41

108
Table C.3.9 ANOVA analysis results for single to co-digestion, and sludge retention time

Source of variation SS df MS F P-value F-critic


Sample 4.35 1 4.35 0.07 0.79 4.75
Columns 229.79 1 229.79 3.84 0.07 4.75
Interaction 23.18 1 23.18 0.39 0.54 4.75
Within 718.29 12 59.86
Total 975.61 15

109
C.4 Methane %

Table C.4.1 CH4% ANOVA analyses results for temperature and sludge retention time

Scenarios Mesophilic Thermophilic


1 (20-d) 66.82 ± 1.79 62.42 ± 2.12
2 (20-d) 63.02 ± 2.59 67.48 ± 2.59
1+2+L (20-d) 66.43 ± 3.90 62.62 ± 10.82
1+2+SC+L (20-d) 66.30 ± 4.86 66.02 ± 0.58
1 (10-d) 68.94 ± 2.36 69.82 ± 5.04
2 (10-d) 64.52 ± 1.61 67.74 ± 3.71
1+2+L (10-d) 68.00 ± 1.35 67.54 ± 1.30
1+2+SC+L (10-d) 69.09 ± 1.23 65.65 ± 1.96

Table C.4.2 ANOVA: two-factor with replication CH4%results for temperature and sludge
retention time

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 262.57 258.55 521.12
Average 65.64 64.64 65.14
Variance 3.10 6.33 4.33

Count 4 4 8
Sum 270.54 270.75 541.29
Average 67.64 67.69 67.66
Variance 4.55 2.89 3.19

Count 8 8
Sum 533.12 529.30
Average 66.64 66.16
Variance 4.42 6.61

110
Table C.4.3 ANOVA analysis CH4% results for temperature and sludge retention time

Source of variation SS df MS F P-value F-critic


Sample 25.43 1 25.43 6.02 0.03 4.75
Columns 0.91 1 0.91 0.22 0.65 4.75
Interaction 1.11 1 1.11 0.26 0.62 4.75
Within 50.65 12 4.22
Total 78.10 15

Table C.4.4 CH4% ANOVA analyses results for sludge retention time and temperature

Scenarios 20-d 10-d


M-1 66.82 ± 1.79 68.94 ± 2.36
M-2 63.02 ± 2.59 64.52 ± 1.61
M-1+2+L 66.43 ± 3.90 68.00 ± 1.35
M-1+2+SC+L 66.30 ± 4.86 69.09 ± 1.23
T-1 62.42 ± 2.12 69.82 ± 5.04
T-2 67.48 ± 2.59 67.74 ± 3.71
T-1+2+L 62.62 ± 10.82 67.54 ± 1.30
T-1+2+SC+L 66.02 ± 0.58 65.65 ± 1.96

Table C.4.5 ANOVA: two-factor with replication CH4% results for sludge retention time and
temperature

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 262.57 270.54 533.12
Average 65.64 67.64 66.64
Variance 3.10 4.55 4.42

Count 4 4 8
Sum 258.55 270.75 529.30
Average 64.64 67.69 66.16
Variance 6.33 2.90 6.61

Count 8 8
Sum 521.12 541.29
Average 65.14 67.66
Variance 4.33 3.19

111
Table C.4.6 ANOVA analysis results for sludge retention time and temperature

Source of variation SS df MS F P-value F-critic


Sample 0.91 1 0.91 0.22 0.65 4.75
Columns 25.43 1 25.43 6.02 0.03 4.75
Interaction 1.12 1 1.12 0.26 0.62 4.75
Within 50.65 12 4.22
Total 78.10 15

Table C.4.7 CH4%ANOVA analyses results for single to co-digestion, and sludge retention time

Scenarios Single Co-digestion


M-1 / M-1+2 +L (20-d) 66.82 ± 1.79 66.43 ± 3.90
M-2 / M-1+2+SC+L (20-d) 63.02 ± 2.59 66.30 ± 4.86
T-1 / T-1+2+L (20-d) 62.42 ± 2.12 62.62 ± 10.82
T-2 / T-1+2+SC+L (20-d) 67.48 ± 2.59 66.02 ± 0.58
M-1 / M-1+2 +L (10-d) 68.94 ± 2.36 68.00 ± 1.35
M-2 / M-1+2+SC+L (10-d) 64.52 ± 1.61 69.09 ± 1.23
T-1 / T-1+2+L (10-d) 69.82 ± 5.04 67.54 ± 1.30
T-2 / T-1+2+SC+L (10-d) 67.74 ± 3.71 65.65 ± 1.96

Table C.4.8 ANOVA: two-factor with replication CH4% results for single to co-digestion, and
sludge retention time

Summary Mesophilic Thermophilic Total

Count 4 4 8
Sum 259.74 261.38 521.12
Average 64.94 65.35 65.14
Variance 6.67 3.32 4.33

Count 4 4 8
Sum 271.01 270.28 541.29
Average 67.75 67.57 67.66
Variance 5.38 2.05 3.19

Count 8 8
Sum 530.75 531.66
Average 66.34 66.46
Variance 7.43 3.71

112
Table C.4.9 ANOVA analysis results for single to co-digestion, and sludge retention time

Source of variation SS df MS F P-value F-critic


Sample 25.43 1 25.43 5.84 0.03 4.75
Columns 0.05 1 0.05 0.01 0.91 4.75
Interaction 0.35 1 0.35 0.08 0.78 4.75
Within 52.27 12 4.36
Total 78.10 15

113
Appendix D: Heavy metals in substrates
Table D.1 Comparison of OMRR heavy metals criteria with calculated concentration for single and co-digested thermophilic effluents at
10-d SRT

Influenta Effluent

Class A Class B 1+2+SC+


1 2† 1+2+L 1 2 1+2+L 1+2+SC+L
biosolids* biosolids* L

Results (mg/kg dry weight)

Aluminum n/r n/r 918.39 0 796.17 794.17 2,185.37 0 1,962.74 1,951.60


Antimony n/r n/r 0.38 0 0.79 0.79 0.90 0 1.94 1.94
Arsenic 75 75 0.36 0.70 2.15 2.15 0.85 1.76 5.29 5.27
Barium n/r n/r 31.95 0 67.31 67.26 76.02 0 165.94 165.28
Beryllium n/r n/r 0.01 0 0.01 0.01 0.02 0 0.03 0.03
Bismuth n/r n/r 4.05 0 3.62 3.61 9.63 0 8.93 8.88
Cadmium 20 20 0.20 1.10 0.29 0.28 0.47 2.76 0.70 0.70
Calcium n/r n/r 2250.88 0 32,325.43 32,332.89 5,356.13 0 79,692.26 79,454.66
Chromium 1,060² 1,060 3.17 14.90 9.91 9.90 7.54 37.46 24.43 24.33
Cobalt 150 150 0.46 0.60 1.49 1.49 1.10 1.51 3.67 3.65
Copper 2,200² 2,200 134.22 46.40 144.16 143.87 319.39 116.65 355.41 353.56
Iron n/r n/r 831.16 0 781.63 779.87 1977.80 0 1,926.97 1,916.46
Lead 500 500 2.89 2 3.13 3.13 6.89 5.03 7.72 7.68
Lithium n/r n/r 0.49 0 5.68 5.68 1.17 0 14.00 13.96
Magnesium n/r n/r 1,197.75 0 32,057.58 32,067.56 2,850.12 0 79,031.93 78,802.65

114
1 2† 1+2+L 1+2+SC+L 1 2 1+2+L 1+2+SC+L

Results (mg/kg dry weight)


Manganese n/r n/r 23.73 0 90.99 90.97 56.47 0 224.32 223.54
Mercury 5 15 0.12 0.05 0.11 0.11 0.30 0.13 0.28 0.28
Molybdenum 20 20 1.46 4 1.82 1.82 3.48 10.06 4.51 4.48
Nickel 180 180 2.34 8.30 5.27 5.27 5.57 20.87 13.02 12.96
Phosphorus n/r n/r 5,019.75 0 4,537.93 4,537.93 11,944.85 0 11,213.77 11,151.48
Potassium n/r n/r 1,490.94 0 18,597.21 18,597.21 3,547.79 0 45,838.53 45,700.66
Selenium 14 14 0.71 1.00 1.22 1.22 1.68 2.51 3.01 3.00
Silver n/r n/r 0.58 0 0.50 0.50 1.38 0 1.24 1.24
Sodium n/r n/r 130.05 0 130,874.3 130,926.9 309.46 0 322,645.9 321,739.13
Strontium n/r n/r 17.57 0 849.73 850.03 41.81 0 2,094.85 2,088.86
Thallium n/r n/r 0 0 0 0 0.01 0 0.01 0.01
Tin n/r n/r 2.71 0 2.49 2.49 6.46 0 6.15 6.12
Titanium n/r n/r 9.91 0 13.42 13.40 23.59 0 33.09 32.94
Uranium n/r n/r 1.74 0 1.96 1.96 4.15 0 4.84 4.82
Vanadium n/r n/r 1.24 0 3.58 3.58 2.95 0 8.83 8.80
Zinc 1,850 1,850 66.05 51.00 67.33 67.18 157.18 128.22 166.00 165.09
Zirconium n/r n/r 1.49 0 3.20 3.20 3.56 0 7.89 7.86
*OMRR (2008)
a
Analysis made in CARO commercial laboratories (Kelowna, BC)
†SunRype internal report: Brandt’s Creek Biosolids Analysis, November 2009, TWAS: thickened waste activated sludge
²Although not specified in OMRR (2008), should be lower than the Class B limits (BC Ministry of Environ., personal communication)

115
Table D.2 Comparison of OMRR heavy metals criteria with calculated concentration for single and co-digested mesophilic effluents at 10-
d SRT

Influenta Effluent
Class A Class B
1 2† 1+2+L 1+2+SC+L 1 2 1+2+L 1+2+SC+L
biosolids* biosolids*
Results (mg/kg dry weight)

Aluminum n/r n/r 918.39 0 796.17 794.17 2,381.70 0 1,882.87 1,816.72


Antimony n/r n/r 0.38 0 0.79 0.79 0.98 0 1.86 1.80
Arsenic 75 75 0.36 0.70 2.15 2.15 0.92 2.98 5.07 4.91
Barium n/r n/r 31.95 0 67.31 67.26 82.85 0 159.19 153.86
Beryllium n/r n/r 0.01 0 0.01 0.01 0.03 0 0.03 0.03
Bismuth n/r n/r 4.05 0 3.62 3.61 10.50 0 8.57 8.27
Cadmium 20 20 0.20 1.10 0.29 0.28 0.51 4.68 0.67 0.65
Calcium n/r n/r 2,250.88 0 32,325.43 32,332.89 5,837.34 0 23.44 73,963.34
Chromium 0 1060 3.17 14.90 9.91 9.90 8.22 63.33 76,449.46 22.65
Cobalt 150 150 0.46 0.60 1.49 1.49 1.20 2.55 3.52 3.40
Copper 0 2200 134.22 46.40 144.16 143.87 348.09 197.22 340.95 329.12
Iron n/r n/r 831.16 0 781.63 779.87 2,155.49 0 1,848.56 1,784.01
Lead 500 500 2.89 2 3.13 3.13 7.51 8.50 7.41 7.15
Lithium n/r n/r 0.49 0 5.68 5.68 1.27 0 13.43 12.99
Magnesium n/r n/r 1197.75 0 32,057.58 32,067.56 3,106.18 0 75,816.00 73,356.39
Manganese n/r n/r 23.73 0 90.99 90.97 61.55 0 215.19 208.09
Mercury 5 15 0.12 0.05 0.11 0.11 0.32 0.21 0.27 0.26

116
Influenta Effluent
Class A Class B
1 2† 1+2+L 1+2+SC+L 1 2 1+2+L 1+2+SC+L
biosolids* biosolids*
Results (mg/kg dry weight)
Molybdenum 20 20 1.46 4 1.82 1.82 3.80 17.00 4.32 4.17
Nickel 180 180 2.34 8.30 5.27 5.27 6.07 35.28 12.49 12.07
Phosphorus n/r n/r 5,019.75 0 4,537.93 4,537.93 13,017.99 0 10,757.46 10,380.78
Potassium n/r n/r 1,490.94 0 18,597.21 18,597.21 3,866.53 0 43,973.29 42,542.18
Selenium 14 14 0.71 1.00 1.22 1.22 1.83 4.25 2.89 2.79
Silver n/r n/r 0.58 0 0.50 0.50 1.51 0 1.19 1.15
Sodium n/r n/r 130.05 0 130,874.3 130,926.95 337.26 0 309,517.0 299,502.91
Strontium n/r n/r 17.57 0 849.73 850.03 45.56 0 2,009.61 1,944.50
Thallium n/r n/r 0 0 0 0 0.01 0 0.01 0.01
Tin n/r n/r 2.71 0 2.49 2.49 7.04 0 5.90 5.70
Titanium n/r n/r 9.91 0 13.42 13.40 25.70 0 31.75 30.66
Uranium n/r n/r 1.74 0 1.96 1.96 4.52 0 4.65 4.49
Vanadium n/r n/r 1.24 0 3.58 3.58 3.21 0 8.47 8.19
Zinc 1,850 1,850 66.05 51.00 67.33 67.18 171.30 216.77 159.24 153.68
Zirconium n/r n/r 1.49 0 3.20 3.20 3.88 0 7.57 7.31
*OMRR (2008)
a
Analysis made in CARO commercial laboratories (Kelowna, BC)
†SunRype internal report: Brandt’s Creek Biosolids Analysis, November 2009, TWAS: thickened waste activated sludge.

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