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DEVELOPMENT OF AN ANAEROBIC TREATMENT SCREENING
PROTOCOL FOR FRUIT AND VEGETABLE PROCESSING
WASTEWATER

presented by

ERIN HENDERSON SZCZEGIELNIAK

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DEVELOPMENT OF AN ANAEROBIC TREATMENT SCREENING PROTOCOL
FOR FRUIT AND VEGETABLE PROCESSING WASTEWATER

By

Erin Henderson Szczegielniak

A THESIS
Submitted to
Michigan State University
in partial fulfillment of the requirements
for the degree of
MASTER OF SCIENCE
Department of Biosystems and Agricultural Engineering

2008

ABSTRACT

DEVELOPMENT OF AN ANAEROBIC TREATMENT SCREENING PROTOCOL
FOR FRUIT AND VEGETABLE PROCESSING WASTEWATER

By

Erin Henderson Szczegielniak

Fruit and vegetable processors commonly produce large volumes of high
strength wastewater that may be inadequately treated by land application.
Anaerobic digestion reduces or eliminates the need for soil treatment and
produces biogas which has the potential to provide the processor with a
renewable energy resource. A novel screening protocol was developed to help
food processors determine the economic feasibility of instituting an anaerobic
digester. The protocol assesses a processing waste stream’s pretreatment

requirement (e.g. pH buffering or nutrient limitations), biogas potential using an

anaerobic respirometer, and biogas quality (% CH4). Processor needs,

wastewater parameters and respirometer results are considered in tandem to
conclude whether the processor should further pursue anaerobic treatment in a
pilot-scale study. The protocol was tested under three conditions including one
in replicate, one blended substrate and one failed condition, with distinguishing
results indicating appropriate or inappropriate substrates for anaerobic treatment.
For each case study, the substrates were characterized by common wastewater
parameters and tested in an anaerobic respirometer. Gas samples from the
respirometer flasks’ headspace were collected and analyzed in a gas

chromatograph for methane and carbon dioxide.

This work is dedicated to the food processors of Michigan.
Here’s to a brighter, cleaner future.

ACKNOWLEDGEMENTS

I wish to acknowledge and thank the following people: my major professor,
Dr. Steven Saffennan, for his patience, guidance and endless support; my
committee members, Dr. Timothy Harrigan and Dr. William Bickert, for their
insight; Mr. Steve Miller for his invaluable assistance, and weathering a
harrowing trip home from Milwaukee; the rest of the GREEEN project advisory
team, especially Mr. Gerald Wojtala, for helping to facilitate the project, and the
Michigan food processors who shared their time, their facilities and their
wastewater to make this work possible; Mr. James Wallace for his time and effort
in supplying the digestate for the respirometer, without which there would be no
data; my fellow students, Ms. Isis Femandez-Torres and Ms. Rebecca Larson,
for providing support and laughter through the frustration; the department staff,
Ms. Barb DeLong, Ms. Cheryl Feldkamp and Ms. Priscilla Gardner, for tirelessly
ordering lab supplies, ensuring I received some payment, and providing rescue
the numerous times I looked my keys in the lab; the rest of the department faculty
and staff who each imparted knowledge and/or support in their own way; my
parents and in-laws for their love, concern and support; my cat, Eddie, for his
companionship throughout the writing process; and most especially my husband,

Mike, whom words would not do justice.

TABLE OF CONTENTS

List of Tables ....................................................................................... vii
List of Figures ....................................................................................... ix
Key to Abbreviations and Acronyms .......................................................... x
Chapter 1: Introduction ........................................................................... 1
Chapter 2: Literature Review .................................................................... 4
2.1 Anaerobic Treatment Applications ............................................... 4

2.2 Microbiology ........................................................................... 4

2.3 pH and Alkalinity ..................................................................... 5

2.4 Temperature .......................................................................... 6

2.5 Nutrient Availability .................................................................. 7

2.6 Toxicity ................................................................................. 9
2.7 Estimating Biogas Production ................................................... 10

2.8 Digester Start-up, Operation and Acclimation .............................. 11

2.9 Biogas Products .................................................................... 13

2.10 Economic and Environmental Considerations ............................ 14

2.11 Advantages and Disadvantages ............................................. 15
Chapter 3: Materials and Methods ........................................................... 17
3.1 Overview ............................................................................. 17

3.2 Substrate Sources ................................................................. 17

3.3 Substrate Characterization ...................................................... 18

3.4 Anaerobic Respirometery ........................................................ 19

3.5 Gas Chromatography ............................................................. 24
Chapter 4: Results and Discussion .......................................................... 26
4.1 Substrate Characterization ...................................................... 26

4.2 Anaerobic Respirometery ........................................................ 29

4.2.1 Case A .................................................................... 29

4.2.2 Case B-1 .................................................................. 31

4.2.3 Case B-2 .................................................................. 33

4.2.4 Case C .................................................................... 36

4.3 Biogas Analysis ..................................................................... 39

4.4 Summary ............................................................................. 43

4.5 Discussion ............................................................................ 45
Chapter 5: Anaerobic Digestion Feasibility Protocol ..................................... 47
5.1 Protocol Overview ................................................................. 47

5.2 Plant Profile ......................................................................... 48

5.3 Energy Potential .................................................................... 48

5.4 Substrate Characterization ....................................................... 49
5.5 Anaerobic Respirometery ........................................................ 50
Chapter 6: Conclusions ......................................................................... 51
6.1 Conclusions ......................................................................... 51
6.2. Future Applications ............................................................... 51
Appendix A: Anaerobic Respirometer Components .................................... 54
Appendix B: Substrate Characterization Analyses - Raw Data ..................... 61
Appendix C: Case C Substrate Allocation Calculations ................................ 66
Appendix D: Respirometer Data ............................................................. 69
Appendix E: Gas Chromatograph Calibration Curves ................................ 121
Appendix F: Gas Chromatography Data ................................................. 124
Appendix G: Quality Assurance and Quality Control .................................. 131
Appendix H: Anaerobic Digestion Feasibility Protocol ................................ 133
H.1 Processor’s Goals and Objectives .......................................... 134
H.2 Plant Profile ....................................................................... 136
H.3 COD Conversion to Heat and Electric Potential ......................... 139
HA Substrate Characterization Tests ............................................ 141
H.5 Anaerobic Respirometery ...................................................... 146
H.6 Toxicity Test ....................................................................... 150
H.7 Interpretation ...................................................................... 151
Appendix I: Respirometer Set-up Procedure ............................................ 152
L1 Flask Allocation .................................................................... 153
l.2 Nutrient and Metal Solutions ................................................... 154
L3 Flask Set-up ........................................................................ 156
Appendix J: Processing Plant Assessment Worksheets .............................. 158
References ....................................................................................... 164

vi

LIST OF TABLES

Table 2.1 Biogas Production from Various Commodities and Reactor Types 13

Table 3.1 Case A Respirometer Flask Allocations ...................................... 21
Table 3.2 Case 8-1 Respirometer Flask Allocations .................................... 22
Table 3.3 Case 8-2 Respirometer Flask Allocations .................................... 22
Table 3.4 Case C Respirometer Flask Allocations ....................................... 23
Table 4.1 Substrate Characteristics ......................................................... 28
Table 4.2 Case A Biogas Analysis .......................................................... 40
Table 4.3 Case 81 Biogas Analysis ........................................................ 41
Table 4.4 Case 82 Biogas Analysis ........................................................ 42
Table 4.5 Case C Biogas Analysis .......................................................... 43
Table 8.1 Case A Substrate Characterization Raw Data .............................. 62
Table 8.2 Case B Substrate Characterization Raw Data .............................. 63
Table 8.3 Case C Wastewater Characterization Raw Data ........................... 64
Table 8.4 Case C Manure Characterization Raw Data ................................ 65
Table 0.1 Respirometer Raw Data: Case A Cumulative Gas ........................ 71
Table 0.2 Respirometer Calculated Data: Case A Gas Production Rate ......... 77
Table 0.3 Respirometer Raw Data: Case 8-1 Cumulative Gas ..................... 84

Table 0.4 Respirometer Calculated Data: Case 8-1 Gas Production Rate ....... 88
Table 0.5 Respirometer Raw Data: Case 8—2 Cumulative Gas ...................... 91
Table 0.6 Respirometer Calculated Data: Case 8-2 Gas Production Rate ....... 98

Table 0.7 Respirometer Raw Data: Case C Cumulative Gas ...................... 103

vii

Table 0.8 Respirometer Calculated Data: Case C Gas Production Rate ........ 114

Table E.1 Gas Chromatograph Calibration Data — Methane ........................ 122
Table E.2 Gas Chromatograph Calibration Data — Carbon Dioxide ............... 123
Table F .1 Gas Chromatography Data: Case A ......................................... 126
Table F .2 Gas Chromatography Data: Case 8-1 ....................................... 127
Table F.3 Gas Chromatography Data: Case 8-2 ....................................... 128
Table F.4 Gas Chromatography Data: Case C ......................................... 129
Table 6.1 Percent Relative Range for Duplicates ..................................... 132
Table 6.2 Percent Recovery for Standards ............................................. 132
Table H.1 Types of Anaerobic Digesters ................................................. 140
Table H.2 Substrate Characterization Analyses ........................................ 142

viii

LIST OF FIGURES

Figure 4.1 Case A Gas Production Rate ................................................... 30
Figure 4.2 Case A Cumulative Gas Production .......................................... 31
Figure 4.3 Case 8-1 Gas Production Rate ................................................ 32
Figure 4.4 Case 8-1 Cumulative Gas Production ....................................... 33
Figure 4.5 Case 8-2 Gas Production Rate ................................................ 35
Figure 4.6 Case 8-2 Cumulative Gas Production ....................................... 36
Figure 4.7 Case C Gas Production Rate ................................................... 38
Figure 4.8 Case C Cumulative Gas Production .......................................... 39
Figure A.1 Stir Plate ............................................................................. 55
Figure A.2 Rear View of Water Bath on Stir Plate ....................................... 55
Figure A.3 Water Bath Hose Connections to Heating/Cooling Unit ................. 56
Figure A.4 Heating/Cooling Unit Set for 35°C ............................................ 57
Figure A.5 Empty Reaction Flask with Syringe and Gas Collection Line .......... 58
Figure A.6 Individual Flow Measuring Cell ................................................. 59
Figure A.7 Flow Measuring Cells ............................................................. 60
Figure A.8 Case A Flasks in Water Bath ................................................... 60
Figure E.1 Methane Calibration Curve ................................................... 122
Figure E.2 Carbon Dioxide Calibration Curve .......................................... 123

8MP
COD
HRT
MDEQ
Rep.
SCOD
TMP
TS
VFA
VS

KEY TO ABBREVIATIONS AND ACRONYMS

biological methane potential

chemical oxygen demand

hydraulic retention time

Michigan Department of Environmental Quality
replicate

soluble chemical oxygen demand

theoretical methane potential

total solids

volatile fatty acids

volatile solids

CHAPTER 1: INTRODUCTION

Fruit and vegetable processors face technical challenges and potential
costs in treating the large volumes of high strength wastewater resulting from
production. All processors face rising fuel costs. Processors with access to a
municipal treatment plant must often meet volume and quality restrictions and
pay a base amount for flow and surcharges for high solids, biochemical oxygen
demand and nutrients. Often a pretreatment system is needed prior to discharge
to the sewer. Processors in rural areas commonly employ lagoon systems and
land application which incorporates soil treatment. While minimally regulated in
the past, land application may soon face more stringent regulations.

One possible solution is anaerobic digestion which reduces or eliminates
the need for municipal or soil treatment and would provide the processor with an
energy resource from the biogas. Anaerobic biogas consists primarily of
methane and thus can be burned as natural gas or transformed into electricity.

While anaerobic digestion offers an attractive solution, not all waste
streams are appropriate for anaerobic treatment. If the wastewater has a
significant concentration of sanitizers, a non-neutral pH or a nutrient deficiency,
then biodegradation and methane production will be inhibited. The high capital
investment of such a treatment system necessitates preliminary screening to
ensure that the waste is anaerobically biodegradable.

Anaerobic biodegradability is typically reported in terms of percent

chemical oxygen demand (COD) removed. More advanced testing to determine

the biogas potential is often desired, which can be achieved using anaerobic
respirometry. A respirometer study measures the individual gas production from
multiple reaction flasks.

Thus far, respirometers have commonly been used to study aerobic
treatment methods, a trend which mirrors the predominance of conventional
aerobic treatment methods in the wastewater treatment field. As anaerobic
digestion and its advantages are becoming better understood and appreciated,
the respirometer has been utilized for anaerobic studies in municipal wastewater
applications. Conversely, many anaerobic studies have focused on food
processing wastewater over the past two decades, but none have been found to

use respirometers.

The first objective was to develop a protocol to pre-screen fruit and
vegetable processing waste streams for anaerobic treatment by determining the
biogas potential using an anaerobic respirometer. Employing anaerobic
respirometry provides a cost effective and efficient means for a processor to
investigate anaerobic treatment options prior to investing significant time and
money in a pilot-scale test or a full-scale system. The purpose of the protocol
was to provide a step by step methodology for the determination of anaerobic
biodegradability. This required general guidelines to apply this method to any
waste stream, the parameters of which could fall within wide ranges. These
parameters affect how long the respirometer trial must run and the net biogas

produced.

The second objective was to test the protocol under three conditions: an
ideal substrate, a low-COD substrate and a blended substrate. ‘ldeal’ and ‘low-
000’ substrates were defined as suggested by supporting literature. A fourth
case of interest involved a failed condition, which happened to be incorporated in
the blended substrate case. Observing a failed substrate was important in
demonstrating that the respirometer results did not produce false positives.
Testing these conditions served to develop and check the utility of the protocol,
which was then revised based on these test results. The purpose of this
research was not to compare specific waste streams.

As the protocol employs a small-scale apparatus, its results are not
directly representative of a full-scale operation nor do they guarantee full-scale
success. Flasks smaller than a liter, such as the respirometer uses, do not
accurately reflect the mixing effects in a full-scale digester. The purpose of the

protocol is to verify if a pilot-scale study is a worthy investment.

CHAPTER 2: LITERATURE REVIEW

2.1 Anaerobic Treatment Applications

Anaerobic digestion is most widely established as a waste treatment
method in Western Europe (Angelidaki et al., 1999). Regulations there require
strict abatement of greenhouse gases including methane and carbon dioxide
(Carucci et al., 2005). As a treatment technology, anaerobic digestion is unique
in that it both reduces waste and produces an energy resource in the biogas.
Potential anaerobic feed substrates include manure (AI-Masri, 2001; Demirer and
Chen, 2005), crop residues (Stewart et al., 1984; Weiland, 1993), organic
municipal solid waste (i.e. solid food wastes) from restaurants or markets
(Bouallagui et al., 2003; Han et al., 2005; Xu et al., 2002; Kiely et al., 1996), and
wastewater from food processing plants (T ekin and Dalgic, 2000; Alvarez et al.,

2005; Lepisto and Rintala, 1997; \flswanath et al., 1992).

2.2 Microbiology

There are four processing steps defined in anaerobic digestion, each
attributed to different trophic groups. The first three steps are hydrolysis,
acidogenesis, and aoetogenesis, which are each performed by different bacterial
groups. The final step is methanogenesis, performed by a type of archaea aptly
termed methanogens (Bouallagui et al., 2004a).

In studying anaerobic digestion it is important to recognize that

methanogens are archaea and still often mislabeled as bacteria. Archaea make

up a domain separate from bacteria and eukarya, and include methanogens,
therrnophiles, and halophiles (Schiraldi et al., 2002). Woese and Fox (1977)
distinguished the domain by noting that archaea evince stark biochemical and
genetic differences from bacteria.

Anaerobic bacteria have different optimal pH and nutrient levels from
methanogens and exhibit different growth kinetics and stress responses
(Bouallagui et al., 2004a). Methanogens are generally more sensitive than
bacteria to environmental fluctuations. It is common for anaerobic digesters to
manifest an unstable methanogen population: methane production may fluctuate
significantly while bacterial volatile fatty acid (VFA) productions remain consistent
(Bouallagui et al., 2005). The rate-controlling step is often acetogenisis though,
as evidenced by VFA accumulation (Speece, 1996; Bouallagui et al., 2005).

Optimal environmental needs include pH and alkalinity, temperature,
macronutrients (C/N/P), bioavailable micronutrients, and a lack of toxicity
(Speece, 1996). Adequate conditions for all parameters must exist for a digester

to flourish, as discussed below.

2.3 pH and Alkalinity

Optimal alkalinity and pH, between 6.5 and 8.2 (Speece, 1996), are critical
for stable methanogensis, and yet confounded by the proceeding process steps
that produce 002 and other acids. If acetogens are slowed by environmental
stressors, then acids go unprocessed and pH will quickly drop, inhibiting

methanogenesis entirely (Bouallagui et al., 2005; Speece, 1996). To counter this

acidifying effect, alkalinity in the digester must be balanced with VFA levels
relative to organic loading rate and hydraulic retention times (HRT) (Borja et al.,
2004). A two-stage digester system, with separate sections for acid and
methane formation, was found to quell rising acid levels (Bouallagui et al., 2005).
Biodegradation can also be limited by high pH though (Penaud et al. 1999), as

ammonia is un-ionized above a pH of 8 and thus toxic (Speece, 1996).

2.4 Temperature

Anaerobic digestion can occur in three distinct temperature ranges:
psychrophilic at 15°C to 25°C, mesophilic at 30°C to 37°C, and thermophilic at
50°C to 65°C (Bouallagui et al., 2004b; Speece, 1996). It should be noted that
thermophilic digestion is unrelated to the therrnophile archaea that inhabit more
extreme locales such as geysers and ocean heat vents. A distinct transition
region between mesophilic and thermophilic digestion is evinced around 45°C
where methane production notably decreases (Converti et al., 1999; Speece,
1996). Methanogens are also sensitive to abrupt temperature change
(Bouallagui et al., 2004b). A 5°C drop resulted in a 34% decrease in methane
production (Speece, 1996).

Thermophilic biomass has a higher metabolic rate than mesophilic and
thus higher gas production (Speece, 1996; Converti et al., 1999) and protein
assimilation (Speece, 1996). Thermophilic systems also exhibit greater
pathogen elimination (Bouallagui et al., 2004b; Duran, 2006). Methanogens

exhibited improved activity with higher temperatures (Converti et al., 1999). The

optimal temperature for acetoclastic methanogens was found to be 56°C to 59°C
(Speece, 1996).

Thermophilic digestion requires disproportionately higher metal nutrients
(Speece, 2006) and has a significantly slower growth rate than mesophiles and
consequently a longer start-up period (Speece, 1996). A two-stage system with
therrnophlic and mesophilic in series utilized the advantages of both (Bouallagui
et al., 2005).

A digester’s temperature range is often selected to compliment the
climatic region, as to avoid excessive heating demands (Bouallagui et al.,
2004b). It follows then that as Europe is the prevailing region in anaerobic
research and development and of a temperate clime, mesophilic systems are
most commonly studied and pursued (Borja et al., 2004; Penaud et al., 1999;
Al-Masri, 2001; Bouallagui et al., 2003). An underlying reason may also be that
acetogens and methanogens are equally active at a mid temperature range
(Speece, 1996); acetogen activity dominates at lower temperatures where

methanogens are more active a higher temperatures.

2.5 Nutrient Availability

Methanogenesis is very sensitive to nutrient availability. Basic
macronutrients and a library of micronutrients must be properly allotted and
biologically available (Speece, 1996). Like most metabolic processes, anaerobic
digestion requires an adequate C:N:P ratio, where carbon is often accounted for

in terms of COD. One source considered fruit and vegetable waste to be

balanced with a COD/NIP of 100/4.3l0.9 (Bouallagui et al., 2004b). Nitrogen or
phosphorus deficiency may be expressed by VFA accumulation (Speece, 1996).
Ammonium can be used as an indicator of digester performance (Carucci et al.,
2005; Speece, 1996).

Micronutrient availability can play a pivotal role in anaerobic digestion.
When a food waste lacking in trace metals was co-digested with municipal
sludge abundant in iron, manganese, copper and zinc, significantly more
methane was produced than from food waste alone (Carucci et al., 2005). Low
methane production initially attributed to toxicity may often be amended by trace
metal addition, particularly iron, cobalt and nickel (Speece, 1996). To prevent
such limiting conditions in batch digesters and bench-scale studies, researchers
commonly provide bulk nutrient solutions with a host of trace metals (Owen et al.,
1979; Shelton and Tiedje, 1984; DiStefano and Ambulkar, 2006; Aquino and
Stuckey, 2007). Iron, cobalt, nickel, zinc, copper, manganese, molybdenum,
selenium, tungsten and boron have been shown to stimulate methanogenesis
(Speece, 1996; Speece, 2006).

Among required nutrients, sulfide is especially noteworthy. While
microbes require sulfide, it readily precipitates with various trace metals
(especially iron), rendering all biologically unavailable (Speece, 1996; Isa et al.,
1986). Sulfur also plays a role in the multifaceted competition between
methanogens and sulfate reducing bacteria, which produce hydrogen sulfide in

lieu of methane (Speece, 1996). Hydrogen sulfide gas is toxic to both anaerobes

and humans. Sulfate and free sulfide are recognized as methanogen inhibitors

at higher concentrations (lsa et al., 1986).

2.6 Toxicity

Anaerobic digestion can be hindered by certain compounds. At high
concentrations, potassium and other salts can interrupt cell function (Carucci et
al.; 2005; Speece, 1996). Sodium chloride was found to inhibit methanogenic
activity (Dolfing and Bloemen, 1985). It was shown however, that in adding
sodium hydroxide, the hydroxide anions caused the negative effect, not the
sodium cations (Penaud et al., 1999). Surfactants were shown to cause greater
inhibition of anaerobic treatment than aerobic treatment (Mohan et al., 2006). As
mentioned in section 2.3, ammonia is un-ionized above pH 8 and is toxic to

anaerobes. Acetogens are particularly sensitive, and concentrations above 3000

mglL NH4-N are toxic regardless of pH (Calli et al., 2005). While not necessarily

‘toxic’, increased total solids loading have a direct correlation with methanogen
inhibition (Viswanath et al., 1992; Carucci et al., 2005; Tekin and Dalgic, 2000).
General toxicity can be determined by an Anaerobic Toxicity Assay, in which gas
production rates are depressed despite an abundance of acetate (Owen et al.,
1979; Speece, 1996).

Long-chain fatty acids (LCFAs) and polyphenols are natural antimicrobial
compounds. In multiple studies of different phenol-rich substrates, anaerobic
digestion was drastically inhibited unless some form of pre-treatment was

employed, such as ozonation (Alvarez et al., 2005), fungal treatment (Dhouib et

al., 2006), or electro Fenton reaction (Khoufi et al., 2006). Adding sulfate during
treatment can also improve phenol biodegradability (Speece, 1996; lsa et al.,
1986), though the negative affects of sulfate must then be abated. It is important
to note that while a microbe population may express inhibition upon initial
exposure to a compound, anaerobes have a strong ability to acclimate (Speece,
1996). Acclimation to LCFAs could not be achieved and the inhibiting affect was

irreversible (Angelidaki and Ahring, 1992).

2.7 Estimating Biogas Production

Simple anaerobic digestibility is often reported in terms of percent COD
removal. Further testing is often desired to determine the biological methane
potential, reported as volume methane produced per unit COD. Batch tests are
commonly conducted using some variation of the Owen serum bottle method
(Owen et al., 1979; Demirer et al., 2000; Han et al., 2005; Shelton and Tiedje,
1984). Based on preliminary batch test results, studies are often expanded to a
semi-continuous bench scale reactor (Carucci et al., 2005; Hwang and Cheng,
1991). There are respirometers available for anaerobic applications. In
anaerobic mode, a respirometer measures the individual gas production from
multiple flasks, each approximately 500 mL in volume (Mohan et al., 2006). This
combines the benefit of test controls and replicates from the serum bottle
methods with the continuous gas monitoring of bench scale reactors (DiStefano

and Ambulkar, 2006). In a hydrogen production study, the anaerobic

10

respirometer produced 43% more gas than the Owen serum bottle method
(Logan et al., 2002).

Many studies use synthetic substrates to observe the affects of specific
parameters on anaerobic digestion (Converti et al., 1999; Conklin et al., 2006);
Isa et al., 1986; Fitzgerald, 1996). However, to study wastewater
biodegradability in the lab, substrate must be imported from the original
processing waste stream because processing wastewaters often include a
conglomeration of food wastes, disinfectants, anti-scaling and other chemicals,

the interactions of which cannot be synthetically replicated.

2.8 Digester Start-up, Operation and Acclimation

Anaerobes have a relatively slow growth rate compared to their aerobic
counterparts. Organic substrate must be processed through several steps before
reaching simple carbon compounds appropriate for methanogenesis. Thus, a
reactor of any size may require several weeks of acclimation before significant
methane production is observed. A two-liter lab reactor digesting pig slurry
produced minimal biogas for the first 25 days of testing (Kiely et al., 1997). Start-
up time is greatly improved when the reactor is seeded with adequate inoculate
from an acclimated seed source (Totzke, 2006).

Different methanogen species express distinct responses to
environmental stimuli and stressors. Hourly versus daily feeding schedules were

shown to select for methanogens with low and high growth rates, respectively

11

(Conklin et al., 2006). The microbes with a higher growth rate made for a more
stable digester, responding better to peak loads and feed shortages.

Biogas production is also influenced by organic loading, total solids and
hydraulic retention time (HRT) (Viswanath et al., 1992; Tekin and Dalgic, 2000).
HRT is of greater concern for a substrate with a high non-soluble fraction (Tekin
and Dalgic, 2000). Switching feedstock between different fruit wastes evinced
little effect on biogas production (Viswanath et al., 1992). This is significant for
food processing applications as plants often switch seasonal commodities
throughout the year. Table 2.1 includes a brief comparison of various sized

reactors and feed sources and their subsequent methane production.

12

Table 2.1 Biogas Production from Various Commodities and Reactor Types

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Reference Commodlty Reactor Temperature Biogas Methane
Type! Size Production fraction
Bouallagui Raw fruit & Tubular/ Psychrophilic 0.64-1.05 LIL/d 56-58%
et al. 2004b vegetable 18L
waste Mesophilic 0.83-2.34 UUd 54-65 %
(shredded)
Thermophilic 1.7 -3.17 UUd 58-62%
Alvarez et Cherry stillage Sequencing Low mesophilic 58-71 %
al. 2005 Batch (30°C)
Reactor/
1.8 L
Stewart et Bananas Continuous! Mesophilic 497 L/kg T8 53%
al. 1984 (fruit and stem) 20 L
Potatoes 350-410 ng 44-50%
(peelings, TS
rejects)
Oats 227-257 ng 51-54%
TS
Yacob et al. Palm oil mill Closed High 650-1000 kg/d
2006 effluent digester/ mesophilic
500 in3 (37-42°C)
Tekin and Olive pomace Semi- Mesophilic 0.39-0.69 UUd 79.5-84%
Dalgic 2000 continuous!
1 L
Vrswanath et Sequential Semi- Low mesophilic 0.61-1.96 UUd 22-61.2%
al. 1992 feedings: continuous] (30°C)
mango, orange, 45 L
pineapple,
tomato
processing,
jackfruit and
banana waste
Lepisto and Carrot UASBI Thermophilic 7.3 UUd 49%
Rintala 1997 processing 2-3 L (55°C) (315 cm3/g (carrots)
wastewater. COD)
Potato and
swede 347 cm3/g
processing COD
wastewater
2.9 Biogas Products

Methane and carbon dioxide are the main constituents of anaerobic

biogas. The methane fraction can range from 40 to 85% depending on

methanogen vitality, substrate quality and reactor type (Alvarez et al., 2005;

Stewart et al., 1984; Tekin and Dalgic, 2000; Yacob et al., 2006). A large

13

percentage of the carbon dioxide remains in solution (Shelton and Tiedje, 1984).
Being mostly methane, biogas can be collected and burned, like natural gas, for
thermal or electric energy. In Denmark, community digesters produce both heat
for local farms and electricity to the power grid (Angelidaki et al., 1999). Several
engine types are adapted to run on biogas, and emerging technology in high-
temperature fuel cells can convert and store energy from biogas (Bove and
Lunghi, 2006; Serge, 2006). The anaerobic digestion process can also be
manipulated to produce a higher percentage of hydrogen gas, a sought-after
resource for fuel cells (Han et al., 2005; Logan et al., 2002).

There are also minor gas constituents which can be troublesome for
certain applications. Biogas often includes a small fraction of hydrogen sulfide
produced from sulfate-reducing bacteria (Speece, 1996). The specific percent

fraction depends on the substrate components. Digestion of citric acid factory

wastewater with 600 mg/L sulfate resulted in the biogas having 4% H28 (Isa et

al., 1986). Internal combustion engines are especially sensitive to hydrogen
sulfide impurities (Speece, 1996) which can be expensive to purge (Isa et al.,

1986)

2.10 Economic and Environmental Considerations

There are several economic considerations in choosing anaerobic
treatment. While primary attention goes to methane as an energy source, those
with experience in the field have found equal or greater benefit in the stabilized

sludge end product (T ekin and Dalgic, 2000). There is also the opportunity to

14

apply for carbon credits through such organizations as the Chicago Climate
Exchange, for actively reducing methane and carbon dioxide emissions (Jensen,
2006).

There are various operating costs associated with an anaerobic digester.
If the influent substrate has a low pH or alkalinity, an alkalinity source must be
metered in to support a neutral pH. To maintain digester stability, it is necessary
to extensively monitor various parameters. There has been recent research to
develop infrared monitoring equipment to measure VFA, COD, alkalinity, sulfate
and nitrogen in-Iine to limit the over-sizing of digesters and lower capital and
operating costs (Spanjers et al. 2006). There had been some trouble of the

monitoring equipment clogging with higher solids content though.

2.11 Advantages and Disadvantages

Anaerobic treatment allows for higher organic loading rates and requires
lower nutrient levels than traditional aerobic treatment (Speece, 1996). There is
no aeration required. While an anaerobic digester requires heating to maintain a
mesophilic (or thermophilic) environment, this can often be met by reapplying
25% of the biogas as a heat source. Overall, anaerobic treatment can provide an
energy resource while reducing a waste product. Due to the anaerobe’s low
growth kinetics, an anaerobic reactor can remain viable in a dormant state during
periods of low flow or plant shut-down.

There are disadvantages to anaerobic wastewater treatment. It does not

achieve significant nutrient treatment such as denitrification or phosphorus

15

removal (Speece, 1996). If effluent discharge regulations require lower limits
than can be met by anaerobic treatment, secondary or tertiary treatment such as
aerobic polishing or phosphorus treatment would need to be considered. While a
low growth rate can provide some advantages, it also equates to a slow start-up

period and arduous recoveries from organic overloading or biomass washout.

16

CHAPTER 3: MATERIALS AND METHODS

3.1 Overview

Development of the screening protocol required a correlation between the
conclusions drawn from the substrate characterization results and the
respirometer results. Testing consisted of collecting and analyzing wastewater
samples from various fruit and vegetable processing plants, and digesting the
samples in an anaerobic respriometer. Respirometry tests included the analysis
of gas samples from the headspace to verify significant methane production.

The substrates were characterized based on parameters of known
relevance to anaerobic digestion. Respirometry testing was conducted at 35°C
based on full-scale operating norms in the region. Quality assurance and quality
control was observed in all aspects by the use (as applicable) of field duplicates,

lab duplicates, standards, blanks and controls.

3.2 Substrate Sources

Wastewater was sampled from three fruit and vegetable processing
plants. Coincidentally, all three plants were processing only fruit at the
respective times at which wastewater was sampled. At the time of sampling,
plant A was producing apple juice and dried cherries; plant 8 was processing
apple slices; plant C was processing whole cherries. The subsequent studies of
each sample are referred to as Case A, 8 and C, respectively. Two respirometer

trials were conducted with sample B, denoted Case 8-1 and 8-2. In Case C,

17

liquid manure was sampled from a local dairy farm for a blended substrate of
manure and wastewater. Manure was collected following a cyclone sand-
manure separator. The substrate constituents for Case C were analyzed
separately and blended later based on these results. 8qu samples for
respirometer testing were stored at 4°C until the respirometer was available to

set up.

3.3 Substrate Characterization

Several parameters were tested, of which pH, COD, soluble COD
(SCOD), total solids, volatile solids and total phosphorus were tested in-house at
Michigan State University. Ammonia, nitrate + nitrite, TKN, sulfide and sulfate
testing was conducted by a commercial laboratory, A&L Labs (Fort Wayne, IN).
Immediately after being collected, these samples were packed on ice and
shipped overnight to A&L Labs. Samples for COD, SCOD and total phosphorus
were collected in glass containers, adjusted with sulfuric acid to a pH <2, stored
at 4°C and analyzed within 28 days. Samples for pH, total and volatile solids
were stored at 4°C and analyzed within seven days.

The pH was measured by a pH meter (accumet Excel XL60, Fisher Scientific)
and electrode (accuCap, Fisher Scientific). COD was determined according to
USEPA approved Hach Method 8000 (0 to 1500 mg COD/L) (Hach Company,
Loveland, Col.). Total phosphorus was determined according to USEPA
accepted Hach Method 8190 (Hach Company). TKN and nitrate plus nitrite were

determined according to EPA methods 351.3 and 353.2, respectively. Sulfide

18

was determined according to EPA method 376.2. Wastewater samples were
analyzed for ammonia according to EPA method 350.2, and digested according
to method SW846-3010A and then analyzed for sulfate according to EPA method
200.7. The liquid manure was analyzed for ammonia according to method
SM(20th)-4500-NH38,C. Sulfate was determined according to EPA method
375.4.

3.4 Anaerobic Repirometery

Respirometer testing was conducted with an AER 200 model (Challenge
Technology, Springdale, Ark.) in anaerobic mode. The system consisted of eight
nominal 500 mL reaction flasks maintained at 35°C in a constant temperature
water bath and mixed via magnetic stir plate at approximately 100 rpm. Gas
production resulted in a slight pressure buildup and dissipated in discrete
bubbles, measured through calibrated flow measuring cells. A computer
processed and stored the data, calculating the gas production rate and
cumulative volume for each individual flask.

To minimize any lag in degradation due to microbial acclimation, seed was
collected from a bench-scale reactor actively digesting ethanol processing
byproducts. Both pH and COD were analyzed at the time of sample collection
and, if stored, again at the time the respirometer set up, as these parameters
may change in unpreserved samples during storage.

Several studies with nutrient solutions were considered (Owen et al.,

1979; ASTM E, 1996; Shelton and Tiedje, 1984; DiStefano and Ambulkar, 2006;

19

Aquino and Stuckey, 2007). Shelton and Tiedje (1984) offered an improvement
on the proposed ASTM standard and a detailed methodology that minimized
precipitation. Though intended for serum bottle tests, this nutrient solution was
similar to mediums described in respirometer literature (DiStefano and Ambulkar,
2006; Logan et al., 2002; Mohan et al., 2006).

Measured amounts of microbial seed, nutrient solution and wastewater
substrate were added to multiple reaction flasks. Contents were stirred and
maintained at a constant 35°C via a water bath. When filled to the lip of the
bottle, nominal 500 mL Wheaton reaction flasks hold approximately 715 mL.
Following the respirometer manufacturer’s recommendations, a 10% headspace
was allowed with a working volume of 650 mL. A 4:1 ratio of nutrient solution to
seed as described by Mohan et al. (2006) was chosen as the study used
comparable substrate and equipment.

Resazurin, an oxidation-reduction indicating dye, was added to each flask
for an approximate concentration of 1 mglL. This indicator changes color
depending on the level of oxidation or reduction: from blue when fully oxidized,
pink when partially oxidized/reduced, and colorless when fully reduced (see
Figure A.8, Appendix A). It allowed for the determination of oxygen
contamination in the anaerobic respirometer flasks. Color change was
discemable even with dark, opaque seed in the flasks.

Tables 3.1, 3.2, 3.3 and 3.4 outline the reaction flask constituents for

Cases A, 8-1, 8-2 and C respectively. Case A had seven reaction flasks; Cases

20

8-1, 8-2 and C each had eight flasks. In all cases a seed control provided the
background biogas produced without substrate.

For Case A (see Table 3.1) two wastewater/seed flasks served as
duplicates. Nutrient solution was omitted from these flasks to evince the effect of
nutrient amendment. The half-strength dilution flask (1/2 [wastewater] seedl
nutrientsj) served as both a scale-duplicate and, if it were to produce
proportionally more biogas than the full-strength flask, a toxicity indicator. Seed
was omitted from the wastewater/nutrients flask to test the microbial activity of
the wastewater itself. Seeding a full-scale digester can incur significant cost. A
blank flask of de-ionized water served to establish the noise level in gas readings
due to pressure changes. During set-up, an eighth flask was broken and so
could not be included.

Table 3.1 Case A Respirometer Flask Allocations

 

 

 

 

 

 

 

 

 

Flask m substrate Seed Nutrient Solution “$223“

(mL) (mL) (mL) (mL)
Wastewater, Seed, Nutrients 50 120 480 0

Wastewater, Seed (repA) 50 120 0 480
Wastewater, Seed (rep 8) 50 120 0 480
Seed 0 120 0 530
‘/2 (Wastewater, Seed, Nutrients) 25 60 240 325
Wastewater, Nutrients 50 0 480 120
Blank 0 0 0 650

 

 

 

 

 

 

For Case 8-1 (Table 3.2) a flask was tested with half the volume of
nutrient solution to further investigate the effect and need for nutrient
amendment. As in Case A, two wastewater/seed flasks served as duplicates; a

half-strength dilution, wastewater/nutrients flask and blank were also included.

21

Table 3.2 Case 8-1 Respirometer Flask Allocations

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Flask ID Substrate Seed Nutrient Solution 0963;?“

(mL) (mL) (mL) (mL)
Wastewater, Seed, Nutrients 50 120 480 0

Wastewater, Seed, 1/2 Nutrients 50 120 240 240
Wastewater, Seed (rep A) 50 120 0 480
Wastewater, Seed (rep 8) 50 120 0 480
Seed 0 120 0 530
1/2 (Wastewater, Seed, Nutrients) 25 60 240 325
Wastewater, Nutrients 50 0 480 120
Blank 0 0 0 650

 

The seed and substrate samples from Case 8-1 were stored at 4°C and

used 4 weeks later in Case 8-2 (Table 3.3). For Case 8-2, two wastewater/

substrate! nutrients flasks were designated as duplicates to confirm the results

from Case 8-1. Two seed controls were tested, one with nutrients and one

without, to determine if a nutrient solution would affect the background gas

production. As in Cases A and 8-1, two wastewater/seed flasks served as

duplicates; a half-strength dilution, wastewater/nutrients flask and blank were

also included.

Table 3.3 Case 8-2 Respirometer Flask Allocations

 

 

 

 

 

 

 

 

 

 

Flask ID Substrate Seed Nutrient Solution 096322;?“

(le (le (le (mL)
Wastewater, Seed, Nutrients (rep A) 50 120 480 0
Wastewater, Seed, Nutrients (rep 8) 50 120 480 0

Wastewater, Seed, 1/2 Nutrients 50 120 240 240

‘/z (Wastewater, Seed, Nutrients) 25 60 240 325
Seed, Nutrients 0 120 480 50

Wastewater, Seed 50 120 0 480

Seed 0 120 0 530

Blank 0 0 0 650

 

 

 

 

 

Case C (Table 3.4) tested a blended wastewater/manure substrate and

thus wastewater and manure separately, each with and without nutrients. The

seed control included nutrients for comparability with the substrate/nutrient

22

 

 

flasks. Because of the multiple scenarios the same controls in Cases A, 8-1 and
8-2 could not all be utilized in Case C due to the restricted number of flasks in
the respirometer.

Substrates were allocated differently with Case C to increase the net
biogas, i.e. the biogas differential between the seed controls and substrate
flasks. The wastewater and manure were apportioned based on COD rather
than volume and blended based on their combined weight-based COD-to-
nitrogen ratio (see Appendix C).

Manure is known to have a high microbial activity; a seed source is not
traditionally used in such anaerobic digestion applications. For comparability,
manure was tested both with the common seed source and as a full volume of
manure alone. In this way, manure was tested as a seed source itself.

Table 3.4 Case C Respirometer Flask Allocations

 

Nutrient De-ionized

 

 

 

 

 

 

 

 

 

Flask ID wastwa‘" "3"“ 3”" Solution Water
(mL) (mL) (mL) (Ml-I (mL)
Wastewater, Manure, Seed,
Nutrients 170 30 90 360 0
Wastewater, Seed, Nutrients 1 70 0 90 360 30
Manure, Seed, Nutrients 0 30 90 360 170
Manure, N utrients 0 120 0 360 170
Seed, Nutrients 0 0 90 360 200
Wastewater, Manure, Seed 170 30 90 0 360
Wastewater, Seed 170 0 90 0 390
Manure, Seed 0 30 90 0 530

 

 

 

 

 

 

Setting up the respirometer was typically a two day process. During the
first day, the nutrient solution was blended, the de-ionized water for the flask
mixtures and the nutrient solution were autoclaved to drive out dissolved oxygen
and the water bath was cleaned. On the second day, the seed sample was

collected (with the exception of Case 8-2 for which stored seed from 8-1 was

23

 

used), the flask filled with the apportioned constituents, the water bath was filled,
the flasks were connected to the gas counting cells and the respirometer
software was set up for data collection. See Appendix H for the respirometer set-
up protocol used.

Respirometer tests were continued until gas production in all flasks
ceased. A flask without nutrient media illustrated to what degree nutrient
amendment was required relative to the flask of substrate, seed and nutrients. A
flask without seed showed to what degree biodegradation, if any, may occur
without seed. The half-strength dilution served as a scale-duplicate and a toxicity
indicator if it were to produce proportionally more biogas than the full-strength

flask.

3.5 Gas Chromatography

Gas samples of 100 pL were collected from the head space of the reaction
flasks and analyzed for methane and carbon dioxide composition by a gas
chromatograph (GC-8, Shimadzu Co., Kyoto, Japan) equipped with a thermal
conductivity detector (TCD) and 6.1 m nickel columns packed with HayeSep D
(100l120 mesh) (Supelco, Bellefonte, Pen.). Two identical columns were
installed; the second served as a reference column into which gas was never
injected. Helium served as the carrier gas. The column temperature was
ramped from 40°C to 110°C at 20°C per minute and the injection port was

maintained at 120°C.

24

Gas tight syringes with push button valves (Series A-2, Fisher Scientific)
were used to collect the gas samples. Originally, 1 mL volume syringes were
used. These were later changed to 250 pL volume syringes for more precise
sample collection. Sampling syringes was purged several times with ambient air
before drawing gas samples from the reaction flasks or standard gas cylinders.

Using methane (99.0%) and carbon dioxide (99.8%) gas standards,
calibration curves were established for the gas chromatograph column (see
Appendix E). Samples of 25, 50, 75 and 100 uL standard gas were analyzed for
each calibration curve (methane and carbon dioxide). From this calibration, the
composite methane and carbon dioxide fractions, was found. Prior to any
sampling event, 50 or 75 uL standard samples of methane and carbon dioxide
were analyzed to conflrrn the calibration. The calibration was considered valid if
were acceptable if the gas standard reading’s reported percent value
(determined from the calibration) was within ten percentage points of the injected
value, e.g. a peak area equivalent to 40% for a 50 uL standard methane sample,

or a peak area equivalent to 65% for a 75 uL standard carbon dioxide sample.

25

CHAPTER 4: RESULTS AND DISCUSSION

4.1 Substrate Characterization

Table 4.1 outlines the characterization analysis of each substrate
(wastewaters A, B and C and manure C). The test parameters and
corresponding recommended ranges from the literature serve as guidelines by
which to screen a substrate’s suitability for anaerobic digestion. This provides a
starting point from which to consider financial implications such as the cost of
nutrient amendment.

Wastewater A had an ideal pH, adequate COD, and a low sulfate
concentration which should produce a clean biogas free of hydrogen sulfide. The
decision to measure SCOD was made after testing case A, so this information is
not available. Like the others fruit processing wastewaters (8 and C) it was low
in nitrogen, phosphorus and sulfide. It was also low in alkalinity. These would
need to be supplemented in a full-scale operation. Wastewater 8 had a
marginally acceptable pH and a low sulfate concentration, but low COD and
alkalinity levels which would not be cost effective for anaerobic digestion.
Wastewater C had an adequate COD level, especially considering the high
percent SCOD which is a measure of COD readily available to the microbial
population. Alkalinity was not tested for wastewater C due to the limited sample
volume collected. The low pH may require the addition of substantial alkalinity to
a full scale system. Manure C had well proportioned nitrogen (CODzN) and

adequate sulfide. The precise phosphorus level was unknown: readings were

26

over the detection limit even at 0.025 dilution factor. This at least indicates that
the phosphorus level was greater than 136 mg/L P. The low percent SCOD and
VS could make for unstable digestion while the remaining insoluble COD (and
solids) are slowly broken down. Marginally high ammonia could cause some
inhibition and the higher sulfate levels could produce a biogas with a notable
hydrogen sutfide component. Alkalinity could not be tested as the manure

sample was too opaque for reliable results.

27

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28

4.2 Anaerobic Respirometery
Figures 4.1 through 4.8 illustrate the respirometer results: the gas
production rate and cumulative gas production for each of the four different

cases, A, 8-1, 8-2 and C.

4.2.1 Case A

Data points were recorded every 3 hours. Gas production lasted for 34
days. Nearly all biodegradation was completed in 14 days in the wastewater/
seed/nutrients flask, where the nutrient-limited (wastewater/seed) flasks took
twice as long. Duplicate flasks exhibited very little relative variation in gas
production rate.

The two wastewater/seed flasks, replicates A and 8, produced the same
amount of gas as the wastewater/seed/nutrients flask but at a slower rate,
showing that digestion was nutrient limited A half-strength dilution of the
wastewater, seed and nutrients produced nearly half the biogas of the full-
strength mixture, evincing no relative toxicity at the full-strength concentration.
There was a relative lag in gas production from this half-strength flask and the
resazurin dye was pink for the first day following set-up, which both point low
seed activity, though maximum gas production rate was as high as the seed and
wastewater/seed replicates. The wastewater/nutrients flask had a distinct pink
color (see Figure A.8) which indicates some microbial activity, though there was
no difference in cumulative gas compared to the de-ionized water. This showed

there to be no significant anaerobic activity from the substrate.

29

 

 

41)

 

35 -~ w__

 

)-

 

b’
or

 

 

 

 

3
r.
I“
FL

 

 

 

.3
O
1

Gas Production Rate (mLIhr)
. r3 .
l

  

 

'I .
O 0 ;.,§’ . I’V‘I'H". ' 1 (\WVV‘r/«x/‘h I” “9 y

O 1 2 3 4 5 6 7 8 9 1O 11 12 13 14 15 18 17 18 19 20 21 22 23 24 25 28 27 28 29 30 31 32 33

 

 

Tlme (days)
—+—Wastewater, Seed. Nutrients -—I—Wastewater, Seed (rep. A) --—s-—— Wastewater, Seed (rep. 8)
——+— Seed +1I2 (Wastewater, Seed, Nutrients) - . - — Wastewater, Nutrients

— — - Deionized Water

 

Figure 4.1 Case A Gas Production Rate

30

 

700

 

 

     
 

 

/*

/. ,
........ _
H-n-"-"MMMMW
.. .- - _ - - - - V'.‘-R'fl-

012 3 4 s e 7 s 9101112131415181718192021222324252627282930313233
Tlmeldays)

§

 

&
8
I

 

 

 

300 «~—

 

 

Cumulative Gas (m L)

200

 

100

 

 

 

 

O

 

—+— Wastewater, Seed, Nutrients ——I—— Wastewater Seed (rep. A) «at—w Wastewater, Seed (rep. 8)
~0— Seed —-x— 112 (Wastewater, Seed, Nutrients) - - - — Wastewater, Nutrients
— — - Deionized water

 

 

 

Figure 4.2 Case A Cumulative Gas Production

4. 2.2 Case B-1

Data points were recorded every 4 hours. Gas production essentially
lasted for 14 days. The wastewater/seed/nutrients flask completed nearly all
biodegradation in 11 days. Duplicate flasks exhibited very little relative variation
in gas production rate. Both Case 8-1 and 8-2 (see Figure 4.5 below) exhibited
a very low gas production rate at less than 1 mUhr. This must be attributed to a
low activity in the seed sample as the seed controls produced a much lower
biogas volume (120 to 130 mL) compared to Case A (over 500 mL).

The two wastewater/seed flasks, A and 8, produced the same amount of

gas as the wastewater/seed] 1/2 nutrients flask though at a slightly slower rate.

31

From this it appears the reaction was less nutrient limited than in Case A. The
waste/seedlnutrients flask produced approximately the same gas volume as the
seed, and less than twice as much as the half-strength dilution. This is probably
due to oxygen contamination or other situational upset rather than a toxic
response to the full-strength nutrient solution concentration, as the same
constituents responded favorably in Case 8-2 (section 4.2.3). The
wastewater/nutrients flask produced less gas than the de-ionized water, again

evincing no active anaerobe population in the substrate.

4.0

 

 

9"
or

9°
0

 

 

 

 

N
or

 

 

4
0|

.3
O

 

Gas Production Rate (mLIhr)
N
O

 

 

 

P
or

 

 

 

Time (days) -
—-o—Wastewater, Seed, Nutrients -,,, ~ Wastewater, Seed, 172 Nutrients -—I——Wastewater, Seed (rep. A)
--s—— Wastewater, Seed (rep. 8) —--0— Seed —-x—- 1I2 (Wastewater, Seed, Nutrients)
- - - - Wastewater, Nutrients - — - Deionized Water

 

 

 

Figure 4.3 Case 8-1 Gas Production Rate

32

160

 

140 —— -= °:° ---'-' "

120 If. , :-::--: - - - ---:-----

 

§
3.

 

 

Cumulative Gas (mL)
8
a“

40 f7
20 1 . ' ”Eff '1 E

.....

 

 

 

—__-_---—_———_——_———————
.—I‘
‘I'
‘—
___..——-—-- ..‘.p-IO-UG“CI—-l—-D—ID—I.-OU’DI-IO—OIU
AF

 

 

o _r—- _ I— _ — T - - F ‘1 T f I r I l I 1' T T I T ‘l 1 Y I T I
o 1 2 3 4 5 6 7 8 9 1o 11 12 13 14 15 16
Time (days)
——0— Wastewater, Seed. Nutrients ~ r -_ Wastewater, Seed, 1/2 Nutrients -I-— Wastewater, Seed (rep. A)
-—-—t—— Wastewater, Seed (rep. 8) -~+— Seed —x-— 1/2 (Wastewater, Seed, Nutrients)
- - - - Wastewater, Nutrients - - - Deionized Water

 

 

Figure 4.4 Case B-1 Cumulative Gas Production

4.2.3 Case B-2

Data points were recorded every 4 hours. Gas production lasted for 27
days. The two wastewater/seed/nutrients flasks, replicates A and 8, completed
biodegradation in 20 days. These duplicate flasks exhibited very little relative
variation in gas production rate. The nutrient solution corresponded with a higher
gas production rate: the wastewater/seed/nutrients flasks had a peak rate of 0.9
mL/hr, where the wastewater/seed flask had a lower rate at 0.6 mL/hr but more
sustained for 4 days longer. There was no significant gas production from the

wastewater] seed/ 1/2 nutrients flask, which was attributed to a loose cap.

33

 

Overall, gas production rates for Case B-2 were comparable to Case 8-1.
Gas production was limited during the first week. This lag was attributed to seed
inactivity due to storage: the same seed sample was used in both 8-1 and 8-2
but was stored at 4°C for 30 days prior to Case 8-2. These results are consistent
with previous observations which corresponded length of storage to lag time
(Shelton and Tiedje, 1984)

There was similar cumulative gas production from the wastewater/seed
flask and the two wastewater/seed/nutrients flasks, replicates A and 8. Flasks
without nutrients had a shorter lag time, suggesting that digestion was less
nutrient-limited than Case A.

The marginal net biogas from Cases 8-1 and B-2 illustrated the
importance of testing substrates based on COD per flask rather than by volume,
and perhaps allocating less seed, in order to ensure significant differentials in
gas production between the substrate and seed control flasks. As discussed in

section 3.3, Case C was set up differently based on this observation.

34

 

 

 

 

 

 

 

 

 

 

 

Gas Production Rate (mLIhr)

 

 

 

 

2 3 4 5 8 7 8 8101112131415181718192021222324

I T v r I

Time (days)

 

 

+ Wastewater. Seed, Nutrients (rep. A) -+-— Wastewater, Seed, Nutrients (rep. 8)
Wastewater, Seed, 112 Nutrients +112 (Wastewater, Seed, Nutrients)
——.-—- Seed. Nutrients +Wastewster, Seed

+ Seed — - — Deionized Water

 

 

Figure 4.5 Case 8-2 Gas Production Rate

35

 

 

25282728

 

180

 

 

140 1

120

 

100‘

 

 

 

 

 

 

 

 

Cumulative Gas (m L)
8

40‘

 

 

20

 

 

 

 

 

 

 

o 1
012 3 4 5 e 7 s 910111213141518171819202122232425282728

Time (days)

 

-+-Wastewater, Seed, Nutrients (rep. A) “—0 —- Wastewater, Seed, Nutrients (rep 8)
Wastewater. Seed, 172 Nutrients ~+- 1/2 (Wastewater, Seed, Nutrients)
-O—- Seed. Nutrients + Wastewater, Seed

+ Seed - - — Deionized Water

 

 

 

 

Figure 4.6 Case 8-2 Cumulative Gas Production

4. 2.4 Case C

Data points were recorded every 4 hours. A larger quantity of substrate,
both in terms of volume and COD, and a smaller quantity of seed were allocated
to each flask. This was done to increase the relative net biogas production, but
also inherently resulted in a longer digestion time. Gas production lasted for 54
days.

Gas production was considerably unstable for Case C compared to the
previous cases, with multiple peaks in the gas production rate for each active
flask. This may be attributed to several factors. The seed sample may have

been of poor quality, as the seed control was itself unstable, as seen by the

36

fluctuations in the gas production rate. To compound the effect of the unstable
seed, the manure/nutrients flask also went through fluctuations in productivity
with multiple gas production rate peaks. This suggests that the manure
presented a more complex substrate, which is supported by its low percent
SCOD. Another factor is the low pH of the cherry wastewater. The
wastewater/seed flask had no significant gas production, a fact which could not
be attributed to oxygen contamination in this case as evinced by the consistent
colorless resazurin dye throughout the trial. The poor results must be due to
inhibition or a lack of essential nutrients or alkalinity to offset the low pH.
Cherries do contain polyphenols which are known to inhibit microbial activity.
However, the cherry wastewater/seedlnutrients flask was not notably inhibited,
which suggests polyphenol inhibition was not the main factor.

The blended substrate (wastewater and manure) performed better than
either substrate individually. Each substrate reached equilibrium faster when
mixed with the nutrient solution, though the nutrient solution did not correlate to a
higher total gas volume. A given 30 mL of manure produced more gas when

combined with 90 mL of seed than with another 90 mL of manure.

37

Gas Production Rate (m Uhr)

 

8.0

 

9'
o

 

:8
o

 

9’
o
1

 

.N
o

 

 

.5
O

 

0.0

 

0 2 4 6 810121418182022242828303234383840424448485052

 

Time (days)
+ Wastewater, Manure, Seed, Nutrients + Wastewater, Seed, Nutrients
A ~ Manure, Seed, Nutrients —+— Manure, Nutrients
-x— Seed, Nutrients ~9- Wastewater, Manure, Seed
+Wastewater, Seed ~o Manure. Seed

 

 

 

Figure 4.7 Case C Gas Production Rate

38

2000

 

é

 

 

i

 

 

é

 

 

é

 

 

 

 

§

 

 

Cumulative Gas (mL)
é

a
8

 

 

400

 

 

 

§

 

 

 

 

 

o rrrfr l I 1'ij I ITTTIil l Uirl

O 2 4 8 810121418182022242828303234383840424448485052

 

Time (days)
+ Wastewater, Manure, Seed, Nutrients +Wastewater, Seed, Nutrients
+ Manure, Seed, Nutrients —+— Manure, Nutrients
+ Seed. Nutrients we Wastewater, Manure, Seed
+Wastewater, Seed >e~ Manure, Seed

 

 

 

Figure 4.8 Case C Cumulative Gas Production
Note: Data were recorded every four hours. For clarity, points are only shown for
every eight hours.

4.3 Biogas Analysis

Tables 4.2, 4.3, 4.4 and 4.5 present the biogas analyses for Case A, 8-1,
8-2 and C, respectively. “COD from Substrate” is the amount of COD available
from the substrate in each given flask, based on the volume of substrate added
and its measured COD. The theoretical methane potential (T MP) is determined

by the following stoichiometric conversion (Speece, 1996):

1 g COD = 395 mL CH4 at 35°C [4.1]

TMP is calculated at 35°C so as to be comparable to the measured data. From

this, the theoretical biogas potential (T 8P) was calculated by assuming 70%

39

methane composition. The total biogas reported is the cumulative volume
measured by the respirometer. Net biogas was calculated as the difference
between the substrate flask and its respective seed control.

An effort was made to analyze gas samples at a period in the trial when
the gas production rate was maximized for a majority of the flasks, barring any
equipment maifunctions. It was assumed this point in the trial best represented
the ideal operating conditions of a full scale reactor when methane production
should also be maximized.

Gas sampling for Case A (Table 4.2) was conducted just as the gas
chromatograph was being set up and the respirometer trial was ending (day 33
and 34). Due to equipment malfunctions and time constraints there was not an
opportunity to analyze a sample from the wastewater/seed/nutrients flask. A
significant background level of methane appeared in sample from the de-ionized
water flask. The syringe-flushing method was revised due to this cross-
contamination.

Table 4.2 Case A Biogas Analysis

 

COD from

TBP

Total

Net

 

 

 

 

 

 

 

 

 

 

 

 

 

 

o
Flask ID Substrate (mL at Biogas Biogas “la-LEV: d % CH 4
(mg) 35°C) (mL) (mL)
Seed - - 512.01 - - 64.5
Wastewater, a
Seed, Nutrients 54.5 130.46 605.7 93.69 71.8 /o n/a
Wastewater, 0
Seed (rep. A) 231.2 130.46 592.3 80.29 61.5 /o 65.6
Wastewater, 0
Seed (rep. 8) 231.2 130.46 618.85 106.84 81.9 A 73.0
‘/2 (Wastewater, 0
Seed, Nutrients) 115.6 65.23 275.75 19.75 30.3 /o 47.0
Wastewater,
Nutrients 231.2 130.46 45.82 45.82 35.1% 37.6
De-ionized water - - 31.21 31.21 - 25.8

 

 

For Case 8-1 (Table 4.3) gas samples were collected and analyzed on

day 6 from wastewaterlseed/nutrients, wastewater/seed (rep. 8) and

wastewater/nutrients) and day 12 from all flasks. Wastewater/seed (rep. A) was

left un-sampled as a control to ensure that the act of gas sampling did not

impose any negative affect on the gas flow measurements. Active flasks with

full-strength wastewater all exhibited methane fractions over 60%. The half-

strength flask (‘/2(wastewater/seed nutrients» achieved over 90% of its TBP,

though with an average methane fraction of 32%, the %T8P may be skewed by

background noise considering the de-ionized water had a reported 10 mL biogas.

Unseeded wastewater produced negligible biogas and methane.

Table 4.3 Case 8-1 Biogas Analysis

 

 

 

 

 

 

 

 

 

COD from TBP Total Net "/ TBP
Flask ID Substrate (mL at Biogas Biogas “awed % cr-r4
(mgL 35°C) (mL) (mL)
Seed - - 122.74 - - 68.5
Wastewater, 54 2
Seed, 54.5 30.75 115.44 0 0.0% 652
Nutrients '
Wastewater,
Seed, 54.5 30.75 143.08 20.34 66.1% 70.9
1l2 Nutrients
Wastewater, 0
Seed (rep. A) 54.5 30.75 143.65 20.91 68.04 n/a
Wastewater, o 47.8,
Seed (rep. 8) 54.5 30.75 146.79 24.05 78.2 /o 68.1
‘/2 (Wastewater, o 19.6,
Seed, Nutrients) 27.3 15.38 75.40 14.03 91.2/e 44.6
Wastewater, o
Nutrients 54.5 30.75 3.14 0 O/o 4.8
De-ionized water - - 10.19 10.19 - 5.7

 

 

 

 

 

 

 

 

For Case 8-2 (Table 4.4) gas samples were collected and analyzed on

day 20. The wastewater/seed/Vz nutrients flask was not sampled, as the gas

production was negligible. Though Including nutrients with the seed control had

no affect on total gas production, net biogas was calculated from each flask’s

41

 

corresponding seed control (i.e. with or without nutrients). The half-strength flask

(‘/2(wastewaterlseed nutrients» had low biogas production and correspondingly

low methane of 39%, comparable to its 8-1 counterpart at an average 32%

Table 4.4 Case B-2 Biogas Analysis

 

COD from

TBP

Total

Net

 

 

 

 

 

 

 

 

0
Flask ID Substrate (mL at Blogas Biogas a $12,; 7, CH4
(m9) 35°C) (le (mL)
Seed, Nutrients - - 121.12 - - 68.5
Wastewater,
Seed, Nutrients 54.5 30.75 137.71 16.59 53.9% 59.3
(rep. A)
Wastewater,
Seed, Nutrients 54.5 30.75 135.44 14.32 46.6% 74.8
(rep. 8)
Wastewater,
Seed, 1/2 54.5 30.75 3.88 0 0.0% n/a
Nutrients
1/2 (Wastewater, a
Seed, Nutrients) 27.3 15.38 63.31 2.75 17.9 /o 38.7
Seed - - 129.51 - - 56.7
we???“ 54.5 30.75 134.49 4.98 16.2% 28.2
De-ionized water - 11.60 11.6 - 5.6

 

 

 

 

 

 

 

 

For Case C (Table 4.5) gas samples were collected and analyzed on days

11 and 14. The methane fraction varied significantly for some of the flasks. A

manure/seed lab duplicate had a difference of 12% methane and average value

of 71.8%. This suggests that the variance between sampling days may reflect

this same resolution.

The blended substrate (wastewater and manure) produced significantly

more gas than either individually, though gas production from the blended

substrate was less than the sum of that from wastewater plus that from the

manure. Interestingly, the individual substrates (wastewater or manure)

achieved a higher %TBP with nutrient amendment at approximately 100% for

 

each, where the blended substrate reached a higher %T8P without nutrient

 

 

 

 

 

 

 

 

 

addition.
Table 4.5 Case C Biogas Analysis
COD from TBP Total Net ./ TBP
Flask ID Substrate (mL at Biogas Biogas a ciii ev ed % CH4
(m9) 35°C) (mL) (mL)
Seed, Nutrients - - 983.6 - - 211%
Wastewater, 40 0
Manure, Seed, 1647 929.5 1632.4 648.8 69.8% 57' 9’
Nutrients '
Wastewater, 27.3,
Seed, Nutrients 783 441.7 1440.1 456.5 103.4% 62.8
Manure, Seed, 63.3,
Nutrients 865 487.8 1467.0 483.4 99.1% 77.3
Manure, 63.7,
Nutrients 3458 1951.4 1173.1 1173.1 60.1% 70.5
Wastewater, 58.8,
Manure, Seed 1647 929.5 1725.7 742.1 79.8% 62.2
Wastewater, 5.2,
Seed 783 441.7 110.0 0 0.0% 17.5
Manure, Seed 865 487.8 1292.5 308.9 63.3% #3,;

 

 

 

 

 

 

 

 

 

*averaged value from lab duplicates

4.4 Summary

All three case studies had respective correlating substrate
characterizations and respirometer gas analyses. Substrate analyses for the
Case A wastewater sample suggested a decent candidate for anaerobic
treatment, with a neutral pH and a mid-range COD level with a high SCOD,
though it would require nutrient amendment including nitrogen, phosphorus and
alkalinity. This was confirmed by the respirometer results, achieving roughly
72% theoretical biogas potential (assuming 70% methane) and an average
methane fraction of 69% from the wastewater/seed replicates. The difference in
gas production rates between the wastewater/seed flasks and that with nutrients

confirmed the benefit of nutrient amendment.

43

Substrate characterizations for Case 8 suggested a poor candidate for
anaerobic treatment, mainly due to the dilute COD level in addition to low
alkalinity and nutrient levels. Respirometer results were poor for both Case 8-1
and B-2. Percent TBP recovered was higher for B-1 than B-2, though these
values may not be significant considering the background level from the de-
ionized water were in the same range as the net biogas from wastewater.
Though biogas production was limited, the average methane fraction (for the
seeded wastewater flasks with and without nutrients) was 63% for 8-1 and 67%
for 8-2.

Wastewater and manure substrates were blended in Case C to optimize
anaerobic treatment potential. The blended substrate had a near optimal COD/N
ratio, compared with the nitrogen deficient wastewater and the nitrogen rich
manure. Respirometer and gas chromatography test results were complex and
inconsistent in this case. Based on the net biogas, biodegradation was improved
by blending. While the manure/nutrients flask produced the highest net biogas, it
had a lower volume than the manure/seed/nutrients per 30 mg COD of manure
added. The percent TBP recovery suggests that manure was the better
candidate, followed by the blended substrate and then the wastewater. Manure
alone also had the highest methane fraction with an average of 70%, where the
blended substrate had an average of 55% methane and the wastewater an
average of 28% methane. Considering just the fruit processing wastewater C,
anaerobic biodegradability was significantly improved by blending with liquid

dairy manure.

44

4.5 Discussion

Screening wastewater for anaerobic biogas potential is important because
substrate characterization alone may not identify sources of inhibition. This was
illustrated in Case C where manure exhibited an unstable gas production rate
and cherry wastewater completely inhibited biogas production in the
respirometer, for which there were no definitive indication from the substrate
characterizations. This is especially true for the blended substrates which did not
exhibit the explicit improvement in gas production as anticipated by the
characterization results.

Case C does not represent conditions as they would likely occur in the
case of proposed blending circumstances. All processors (A, B and C), from
whom samples were collected for testing, added their storm water to their plant
wastewater and land applied this mixture. This may be acceptable practice for
land application, but in pursuing anaerobic digestion storm water would be kept
separated and other water minimization practices would likely be implemented to
further concentrate the COD loading. Blending manure with a highly soluble
COD waste stream could then potentially stabilize gas production. Wasted food
product that does not meet specifications would also be much more concentrated
and appropriate for supplemental blending perhaps.

The experiments conducted to support this protocol development yielded
interesting findings regarding the characteristics of fruit processing wastewater.
For Cases A, 8-1 and 8-2, the cumulative gas curves from the optimized flasks

(wastewater/seed/nutrients) exhibited a classic batch-system growth curve, i.e.

45

an initial lag period followed by a log inverse increase. Without nutrient
amendment (wastewater/seed), the lag was increased in the slope of the growth
curve was decreased.

From the varied seed gas production rates among the respriometer trials,
it is clear that anaerobic digestate activity can vary greatly (even from the same
digester processing the same substrate over time). Therefore, it is important to
note the relative seed activity so that inaccurate conclusions are not drawn
regarding the substrate’s biodegradability.

In developing the protocol, several procedural techniques were found that
can impact results. This includes the ratio of substrate to seed in the
respirometer flasks. There is little precedent set by previous literature as the
majority of studies concern the treatment of municipal sludge or manure in which
case the substrate being treated provides its own seed source. Cases A, 8-1
and 8-2 illustrate one option in which a set volume of substrate is added in
proportion to a set volume of seed. The specific ratio may be adjusted to model
a plug-flow anaerobic digester. Case C offers an alternative in which a substrate
volume is selected to provide a specific amount of COD to each flask. This
option allows more control in insuring an ample net biogas potential and the
respirometer trial length. A subsequent question is whether to ration the nutrient

solution in relation to the seed volume, the substrate volume or both.

46

CHAPTER 5: ANAEROBIC DIGESTION FEASIBILITY PROTOCOL

5.1 Protocol Overview

Based on the lab results (Chapter 4) and several processing plant tours
and interviews this protocol was revised to its current edition. Step-by-step
instructions for the protocol are provided in Appendix H with supporting material
in Appendices l and J.

This protocol is intended to serve fruit and vegetable processors by
analyzing a waste stream (substrate) to determine the applicability of anaerobic
digestion as a treatment method and/or energy source. Food processors and
area farmers pursuing a regional digester may also test wastewater-manure
blends. An individual processor may be interested in installing a digester for the
plant’s wastewater treatment or a group of processors and/or farmers may be
organizing a regional digester. The protocol includes methods to assess a waste
stream’s pretreatment and operating requirements, estimate biogas production
using an anaerobic respirometer and analyze the subsequent methane fraction
with gas chromatography. It provides recommendations for suitable methane
applications. Processor objectives, wastewater parameters and respirometer
results are considered to determine if further investigation such as a pilot-scale
digester is appropriate. To facilitate the collection of pertinent information from
the processor, assessment worksheets were developed based on literature and
site-specific experience (see Appendix J). Conclusions for an individual

processor may include a recommendation to consider a regional digester.

47

5.2 Plant Profile

Several fruit and vegetable processors were interviewed to gain insight to
important considerations for this screening procedure. Due to the seasonality of
fruit and vegetables, processors commonly handle a variety of commodities
throughout the year. Wastewater may widely fluctuate in flow, pH, COD strength
and nutrient concentration, all of which can impact the stability of anaerobic
digestion. Therefore, a critical step is to profile these changes throughout the
year as accurately as possible. For the purpose of regulatory compliance, many
processors keep record of monthly wastewater flows and its characteristics such
as pH, BOD, macronutrients and some minerals. Wastewater regulations often
require processors to monitor BOD, which reflects aerobic biodegradability;
however, COD is easier to analyze and more appropriate for anaerobic
applications and thus the reference test for this protocol as with most anaerobic
literature.

Once the wastewater profile is established, multiple samplings may be .
needed for testing to represent high, low and average wastewater conditions. To
maintain representative results, waste stream samples should be analyzed and

set up in the respirometer as soon as possible.

5.3 Energy Potential
Other important considerations for anaerobic treatment often include
energy potential. Rough estimates of methane production and heating potential

can be calculated based on the wastewater COD content. The theoretical

48

methane equivalence of 1 g COD is 395 mL CH4 at 35°C (or 350 mL CH4 at

STP) (Speece, 1996). This converts to 12.66 GJ (12 MM Btu) per 1000 kg COD
destroyed. Actual methane production will vary with reactor efficiency. Given a
processor’s current cost for natural gas, and assumed reactor and boiler
efficiencies, rough cost offsets from potential methane production can be
calculated. This represents the maximum energy potential. If energy recovery is
important to the processor and this value is too low, the opportunity for anaerobic

digestion will be limited.

5.4 Substrate Characterization

The COD to energy conversions described above do not account for
variability in substrate biodegradability. To properly assess the potential for
anaerobic treatment of a specific waste stream, several other parameters must
be analyzed.

In considering anaerobic treatment for a nutrient-deficient waste stream,
the cost for nutrient amendment in full-scale operation should be weighed against
potential cost offset by biogas production. Most food processing wastes may be
lacking in trace metals such as iron, nickel, zinc and cobalt, which are known to
be highly limiting of methanogenesis. If nutrient amendment is too costly, the
opportunity to blend the waste stream in a regional digester should be

considered and tested using this protocol.

49

5.5 Anaerobic Respirometer

The ultimate step in the protocol is respirometer testing to analyze biogas
potential and methane production. Testing different combinations of wastewater
or blended substrate with seed and/or nutrient solution can provide information
about the biodegradability of the wastewater. Comparison of the cumulative gas
and gas production rate curves can show signs of inhibition, nutrient limitation
and seeding requirements. Gas chromatography analysis of headspace samples
can confirm the degree of biodegradation and methane production. From these
considerations an educated assessment to pursue anaerobic treatment can be

garnered.

50

CHAPTER 6: CONCLUSIONS

6.1 Conclusions

The objectives of the project were successfully met. A general protocol
was developed to pre-screen fruit and vegetable processing waste streams for
anaerobic treatment using anaerobic respirometry. This protocol was tested
under three conditions with distinguishing results indicating appropriate or

inappropriate substrates for anaerobic treatment.

6.2 Future Applications

There are several opportunities to improve and streamline the screening
protocol for future applications. Characterizing the seed sample prior to
respirometer testing including COD and volatile suspended solids would provide
better insight to the seed biogas potential, as the experiments in this study
showed great variability in the seed activity over time even from the same
digester. A standard seed source maintained in the lab may provide the most
benefit. A validation study of the protocol with a full-scale system is imperative
and may incite further improvements in the protocol. It may be of interest to
compare the respirometer method to the conventional serum bottle method.

If an expanded respirometer of 16 or more reaction flasks were available,
then it should be possible to run flask duplicates in which CO; is scrubbed out

from one of each pair. This could allow for the gas counter to directly measure

51

methane production. Gas chromatography analyses would still be advisable to

ensure carbon dioxide was fully removed and to confirm methane concentrations.

52

APPENDICES

53

APPENDIX A

ANAEROBIC RESPIROMETER COMPONENTS

54

Figures A-1 through A-8 show the various components of the respirometer
equipment. In Figure A-1 the stir plate is shown, upon which the water bath is
placed in Figure A-2. The gap in the water bath lid provides space for the gas

transport lines which connect the reaction flasks to the flow measuring cells. The

heating/cooling unit is not yet connected to the water bath in this view.

 

Figure A.2 Rear View of Water Bath on Stir Plate

55

Hose connections at the water bath are shown in Figure A-3. The left hose
is the inlet line to the water bath; the right hose is the gravity return line to the

heating/cooling unit.

 

Figure A.3 Water Bath Hose Connections to Heating/Cooling Unit

Flow rate through the water bath was adjusted by the blue handle seen on
the heating/cooling unit’s left side (Figure A-4). The valve on top allows for the
unit to be filled or drained. The water bath must be elevated above the unit to

accommodate the gravity return line.

56

 

Figure A.4 Heating/Cooling Unit Set at 35°C

Figures A-5 through A-7 illustrate the gas collection components. Arrows
indicate the direction of gas flow. In Figure A-5, a syringe connected to the gas
collection line is shown inserted into an empty reaction flask septum cap. The
syringe is inserted into the septum cap at the thicker edge and at an angle to

prevent strain, as per the manufacturer’s instructions.

57

 

Figure A.5 Empty Reaction Flask with Syringe and Gas Collection Line

From the reaction flasks, gas flowed through the syringe and gas
collection line to flow measuring cells. An individual flow measuring cell is shown
removed from the base in Figure A-6. Gas flows from the reaction flask up the
left tube, then through the cell oil in discrete bubbles of calibrated volume where
they interrupt a laser counter (labeled in Figure A-6). The bubbles then flow out
of the cell through the right tube to a common manifold and out the exhaust port.
Figure A-7 shows all eight flow measuring cells connected to the center manifold.
Tubing can be seen (as labeled in Figure A-7) connected to the exhaust port
which led to a gas collection bag (not pictured) for safety.

In Figure A-8, the reactions flasks are shown being stirred while in the

water bath and connected to the flow measuring cells. An oxidation-reduction

58

 

Figure A.6 Individual Flow Measuring Cell

indicator, resazurin, was added to each flask to indicate aerobic conditions. With
no microbial activity in the de-ionized water, the resazurin is fully oxidized and a
dark indigo color. Resazurin transitions to bright pink when minimal reduction
occurs. This can be seen in flask 6 (top right corner, Figure A-8) containing
wastewater and nutrients, which shows there is limited microbial activity though
not fully anaerobic conditions. When fully reduced, the indicator is colorless as
seen in the seeded flasks (1 through 5, the five flasks to the left in Figure A-8). If
oxygen were present in the seeded flasks, the indicator would be oxidized and

turn the solution a dark maroon color.

59

Exhaust tubing to
gas collection bag

n—m...
-M “W... . W“.-. . _--... .

 

Figure A.8 Case A Flasks in Water Bath

60

APPENDIX B

SUBSTRATE CHARACTERIZATION ANALYSES — RAw DATA

61

Table 8.1 Case A Substrate Characterization Raw Data

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Dilution Original Reported Reporting
Parameter Sample No. Factor Reading Value leit
H 1 7.41
9 LD 1 7.20
Alkalinity 1 1 66 66
(mg/L CaCO3) ,
Blank 0.025 L 0.000 g 0
Total Solids (glL) 1 0.025 L 2.341;; 93.64
LD 1 0025 L 1.8881: 75.52
Standard
COD (m 9M (1000 mglL) 1.00 1050 1050
2 0.25 1156 4624
Standard
(392 m gIL P) 0.20 0.85 4.25
Total Phosphorus 1 025 OR OR 1 _10+
(mg/L P) 2 0.25 1.11 4.44
LD 2 0.25 1.00 4.00
Ammonia
A&L BDL 0.10*
(mg/L NH4-N)
Nitrate + Nitrite
[m /L N) A&L 0.40
TKN (rm/L N) A&L 24
Sulfide (mg/L) A&L BDL 1*
Sulfate (mg/L S04) A&L 3
LD = Lab Duplicate OL = Over Limit BDL = Below Detection Limit
1: Liquid left in dish after 6 hours “ Upper limit * Lower limit

62

Table 8.2 Case 8 Substrate Characterization Raw Data

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Dilution Ori inal Re rted Re ortin
Parameter Sample No. Factor Reagcang VZTue Eimit g
1 6.42
pH 2 6.52
3 6.62
Alkalinity 2
(mg/L CaCO3) 4 0. 0 11 55
Blank 0.025 L 0.0000 g 0.00
1 0.025 L 0.0251 g 1.00
Total Solids (g/L) 2 0.025 L 0.0255 9L 1.02
LD 2 0.025 L 0.0269 g 1.08
3 0.025 L 0.0261 g 1.04
Blank 0.025 L 0.00143 0.06
1 0.025 L 0.0198 g 0.79
Volatile Solids (glL) 2 0.025 L 0.0205 g 0.82
LD 2 0.025 L 0.0217 g 0.87
3 0.025 L 0.0215 5 0.86
Standard 1.00 1044 1044
(1000 mglL)
COD ("'9“) 1 0.25 265 1060
2 0.25 280 1120
1 0.25 224 896
SCOD (mg/L) 2 0.25 239 956
L0 2 0.25 226 904 f f
Standard
(392 m g/L P) 0.20 0.73 3.65
Total Phosphorus 1 0.25 0.52 2.08
(mg/L P) LD 1 0.25 0.57 2.28
2 0.25 0.51 2.04
3 0.25 0.52 2.08
Ammonia '
A&L BDL 0.10*
(mg/L NH4-N)
Nitrate + Nitrite .
(mg/L N) A&L BDL 0.05
TKN (mg/L N) A&L 6
Sulfide (rrig/L) A&L BDL 1*
Sulfate (mg/L $04) A&L 28
L0 = Lab Duplicate OL = Over Limit BDL = Below Detection Limit
+ Upper limit * Lower limit

63

Table 8.3 Case C Wastewater Characterization Raw Data

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Dilution Ori inal Re rted
Parameter Sample No. Factor Reagdin v2?“
pH 1 5.17
Blank 0.025 L 00006 -o,02
Total Solids (glL) 1 0.025 L 0,1223 4.89
LD 1 0.025 L 0.12319 4,95
Blank 0.025 L 0.0004 g 0.02
Volatile Solids (g/L) 1 0.025 L 01143 9 4,59
LD 1 0.025 L 0.1167 g 4.68
Standard
coo (mg/L) (1000 mg IL) 1.00 1014 1014
1 0.25 1160 4640
2 0.25 1 142 4568
1 0.25 1047 4188
SCOD (mg/L) LD 1 0.25 1077 4308
Standard
Total Phosphorus (3.92 mglL P) 0'20 ”5 3'25
(mg/L P) 2 0.25 0.92 3.68
. LD2 , 0.25 0.98 3.92
Ammonia
A&L 2.02
(mg/L NH4-N)
Nitrate + Nitrite ' ‘
(mg IL N) A&L 0.68 .
T KN (mgL N) A&L 22
Sulfide (mg/L) A&L 1
Sulfate (mg/L $04) A&L 11

 

 

 

 

LD = Lab Duplicate

Note: sample 1 was un-preserved; sample 2 was preserved with H2804 to pH < 2.

64

Table 8.4 Case C Manure Characterization Raw Data

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Dilution Original Reported Reporting
Parameter Sample No. Factor Readin Value Limit
. Blank See Case C Wastewater
ma" S°"ds (9M 1 0.025 L [ 0.6665 9 1 26.66
. . Blank See Case C Wastewater
V°'at"e S°"ds (9M 1 0.025 L 0.4111 g 16.44
Standard (a)
(1000 mg@ 1.0 1014 1014
1 (a) 0.04 563 14,075
1 (a) 0.02 637 31.850
LD 1 (a) 0.02 566 28.300
Standard (0)
COD (mg/L) (1000 mglL) 1.0 1024 1024
1 (b) 0.05 CL CL 1500+
LD1 (b) 0.05 1374 27,480
(33333333 1.0 1019 1019
1 (C) 0.05 1382 27,640
1 0.05 537 10,740
SCOD (mg/L) LD 1 0.05 546 10.920
Standard 7
Total phosphorus (3.92 mg/L P) 02° 0'65 3'25
(mg/L P) 1 0.10 CL CL 1.10+
1 0.025 CL CL 1.10+
Ammonia
A&L 1004
(mg/kg NH4-N)
Nitrate (mg/kg N) A&L 2
TKN (mg/kg N) A&L 1673
Sulfide (mg/L) A&L 1 3
Sulfate (mg/L $04) A&L 681
L0 = Lab Duplicate OL = Over Limit " Upper limit

(a), (b), (c) Corresponds given standard to sample(s).

65

APPENDIX C

CASE C SUBSTRATE ALLOCATION CALCULATIONS

66

The Objective for Case C was to blend the cherry wastewater and dairy
manure to an approximate COD/N Of 100/4.5 (approximated from Bouallagui et
al., 2004b). In this case, only SCOD was considered, representing substrate
readily available tO the microorganisms. TKN was considered for the nitrogen
fraction, following Bouallagui et al. (2004b).

From the SCOD and TKN values given in Table 4.1, the COD:N ratios are:

Wastewater C (COD/N): 4248 l 23 100l0.517

Manure C (COD/N): 10830 / 1673 100/15.45
In the original blending calculations, the Wastewater C ratio was rounded to
100/0.52 and Manure C was rounded to 100l15.

A target Of 1000 mg COD per flask was chosen to provide a significant net
biogas volume when compared with the seed flask. TO achieve an approximate
ratio of 100l4.5 from a blended substrate would require 720 mg Of Wastewater C

and 280 mg Of Manure C.

Wastewater: 720 mg COD *0.52 mg N I100 mg COD = 3.74 mg N

Manure: 280 mg COD *15 mg N I 100 mg COD = 42. mg N

Blended: (720 + 280) mg COD I (3.74 + 42.) mg N = 1000/45.74
COD/N = 100l4.57

67

TO set up the respirometer flasks, the wastewater and manure was
measured out volumetrically. The fractions of milligrams COD were simply

converted to milliliters.

Wastewater: 720 mg COD / 4248 mg COD/L = 170 mL

Manure: 280 mg COD / 10,830 mg COD/L = 26 mL

The manure volume was rounded to 30 mL for ease Of measurement. This
provided a blended substrate volume of 200 mL. The remaining flask volume
was then 450 mL. At a seed to nutrient solution Of 4:1, this gave a seed volume

of 90 mL and 360 mL Of nutrient solution.

68

APPENDIX D

RESPIROMETER DATA

69

For Tables 0.1 through 0.8, the flask contents are abbreviated as follows:
wastewater (W), manure (M), seed (8), nutrients (N), de-ionized water (DI) and
replicate (rep). The ‘Cumulative Gas’ tables (Tables D1, D3, 05 and 0.7)
contain data stored directly by the respirometer software. The ‘Gas Rate’ tables
(Tables 0.2, DA, 06 and 0.8) contain the gas rate (mL/hr) calculated from the
change in total gas (mL) over the given time count Of three or four hours. While
the respirometer software updates and plots the gas production rate every ten
seconds, it does not store this data, so this had to be recalculated from the
stored cumulative gas data which was recorded in multiple-hour time steps.

In Case A, the gas counter was reset at 13 hours when the water bath
temperature and gas fluctuation had equilibrated, and data collection was
changed from every 4 hours to every 3 hours. In Cases B-1, B-2 and C, the
cumulative gas totals were recalculated after the acclimation period. This period
was defined by a noted common decrease in the gas production rate consistent
among all the flasks after an initial spike. Cumulative gas totals were

recalculated from zero, and trial durations were retimed, starting at this point.

70

Table D1 Respirometer Raw Data: Case A Cumulative Gas

 

Cumulative Gas from Flasks (mL)

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Da Time ws WS .
V (m) wsu V:(WSN) s (rep A) (rep 6) WM DI Date
0 0.00 0.00 0.00 0.00 0.00 0.00 0.00 4/5/07
0 0.00 0.04 0.13 0.09 0.13 0.00 0.09 4/5/07
4 9.36 7.55 9.28 10.37 11.23 5.28 6.31 4/6/07
6 12.06 6.22 10.08 12.41 13.54 5.67 6.40 4/6/07
12 14.19 6.56 11.77 14.54 15.65 5.96 6.56 4/6/07
13 14.64 6.67 12.22 14.99 16.34 5.96 6.62 4/6/07
0.00 16 1.62 0.40 1.47 1.45 1.65 0.00 0.16 4/6/07
0.13 19 3.26 0.76 2.94 2.65 3.11 0.00 0.36 4/6/07
0.25 22 4.69 0.96 4.24 4.06 4.44 0.00 0.40 4/6/07
0.36 25 6.51 1.16 5.53 5.30 5.77 0.00 0.40 4/6/07
0.50 26 7.95 1.43 6.73 6.57 7.33 0.00 0.40 4/7/07
0.63 31 9.47 1.66 6.16 6.11 6.97 0.00 0.49 4/7/07
0.75 34 10.96 2.41 9.59 9.60 10.61 0.18 0.63 4/7/07
0.66 37 12.39 2.66 10.93 10.67 11.94 0.27 0.67 4/7/07
1.00 40 13.69 3.22 12.13 11.67 13.10 0.27 0.67 4/7/07
1.13 43 15.31 3.67 13.60 13.05 14.21 0.27 0.67 4/7/07
1.25 46 16.79 3.64 14.65 14.04 15.41 0.27 0.67 4/7/07
1.36 49 16.32 3.96 16.01 14.68 16.56 0.27 0.67 4/7/07
1.50 52 20.03 4.20 17.35 16.04 17.60 0.27 0.67 4/8/07
1.63 55 21.91 4.60 16.73 17.35 19.23 0.27 0.67 4/6/07
1,75 56 23.60 4.67 19.96 16.57 20.60 0.27 0.67 4/6/07
1.88 61 25.66 5.19 21.23 19.60 21.69 0.27 0.67 4/8/07
2.00 64 27.64 5.54 22.52 21.11 23.31 0.27 0.67 4/6/07
2,13 67 29.66 5.99 23.62 22.42 24.76 0.27 0.67 4/8/07
2.25 70 32.10 6.39 25.15 23.76 26.24 0.27 0.67 4/6/07
2.36 73 34.30 6.75 26.40 25.05 27.57 0.27 0.67 4/6/07
2.50 76 36.62 7.24 27.74 26.46 28.95 0.27 0.67 4/9/07
2.63 79 39.29 7.76 29.03 27.66 30.41 0.27 0.67 4/9/07
2.75 62 41.65 6.31 30.37 29.06 31.97 0.27 0.67 4/9/07
2.88 85 44.41 6.90 31.71 30.53 33.43 0.27 0.67 4/9/07
3.00 66 47.06 9.57 33.09 32.03 34.90 0.27 0.67 4/9/07
3.13 91 50.06 10.55 34.70 33.70 36.67 0.27 0.67 4/9/07
3.25 94 53.03 11.44 36.22 35.24 36.32 0.27 0.67 4/9/07
3.36 97 55.72 12.11 37.51 36.65 39.60 0.27 0.67 4/9/07
3.50 100 56.55 12.92 39.03 36.10 41.25 0.27 0.67 4/10/07
3.63 103 61.33 13.66 40.45 39.55 42.76 0.27 0.67 4/10/07
3.75 106 64.21 14.39 41.66 40.91 44.16 0.27 0.67 4/10/07
3.66 109 66.66 15.11 43.26 41.90 45.47 0.27 0.67 4/10/07
4.00 112 69.62 16.00 44.62 43.53 47.02 0.27 0.76 4/10/07
4,13 115 73.10 17.03 46.61 45.16 46.75 0.27 1.12 4/10/07
4.25 116 76.29 16.10 46.44 46.79 50.39 0.27 1.39 4/10/07
4.36 121 79.43 19.09 50.16 46.34 51.99 0.27 1.57 4/10/07
4.50 124 62.57 20.03 51.91 49.69 53.46 0.27 1.71 4/11/07

71

 

Table D1 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

4,63 127 86.03 21.14 53.88 51.32 55.19 0.27 2.02 4/11/07
4.75 130 89.53 22.26 55.88 52.87 56.61 0.27 2.25 4/11/07
4,88 133 93.21 23.47 58.07 54.54 58.30 0.27 2.56 4/11/07
5.00 136 97.34 24.99 60.52 56.44 60.25 0.27 3.10 4/11/07
5.13 139 101.56 26.51 62.93 58.35 62.25 1.05 3.64 4/11/07
5.25 142 105.65 27.89 65.34 60.11 64.11 1.55 4.09 4/11l07
5,38 145 109.96 29.32 67.75 61.88 65.89 1.96 4.49 4/11/07
5,50 148 114.41 30.80 70.29 63.65 67.80 2.46 4.98 4/12/07
5,63 151 118.76 32.14 72.74 65.32 69.49 2.78 5.25 4/12/07
5.75 154 122.85 33.35 75.11 66.77 70.55 2.87 5.34 4/12/07
5,88 157 126.62 34.33 77.29 68.00 72.11 2.87 5.34 4/12/07
6.00 160 130.48 35.49 79.66 69.40 73.53 2.87 5.34 4/12/07
6.13 163 134.25 36.56 82.02 70.62 74.86 2.87 5.34 4/12/07
6.25 166 137.89 37.59 84.38 71.85 76.15 2.87 5.34 4/12/07
6.38 169 141.61 38.75 86.79 73.11 77.48 2.87 5.34 4/12/07
6.50 172 145.70 40.19 89.56 74.61 79.21 2.87 5.34 4/13/07
6,63 175 149.83 41.62 92.41 76.19 80.99 2.87 5.34 4/13/07
675 178 154.01 43.09 95.27 77.73 82.67 2.87 5.34 4/13/07
6.88 181 158.23 44.61 98.12 79.32 84.36 2.87 5.34 4/13/07
7,00 184 162.94 46.35 101.29 81.18 86.36 2.87 5.34 4/13/07
7,13 187 168.06 48.37 104.85 83.31 88.36 2.87 5.34 4/13/07
7,25 190 172.51 50.24 108.47 85.48 90.89 2.87 5.34 4/13/07
7,38 193 177.62 52.08 112.08 87.52 93.20 2.87 5.34 4/13/07
7,50 196 183.15 54.13 115.96 89.88 95.77 2.87 5.34 4/14/07
7,63 199 188.80 56.32 119.97 92.37 98.43 2.87 5.34 4/14/07
7,75 202 194.46 58.56 124.03 94.86 101.14 2.87 5.34 4/14/07
7,88 205 200.16 60.84 128.18 97.35 103.94 2.87 5.34 4/14/07
8,00 208 205.87 63.07 132.37 100.02 106.78 2.87 5.34 4/14/07
8,13 211 212.06 65.80 137.10 103.24 110.20 2.87 5.34 4/14/07
8,25 214 217.94 68.26 141.56 106.23 113.31 2.87 5.34 4/14/07
8,38 217 223.60 70.58 146.02 109.22 116.15 2.87 5.34 4/14/07
8,50 220 229.39 73.00 150.66 112.30 119.39 2.87 5.34 4/15/07
8,63 223 234.83 75.41 155. 30 115.38 122.59 2.87 5.34 4/15/07
875 226 240.66 77.82 160.02 118.50 126.05 2.87 5.34 4/15l07
8.88 229 246.37 80.15 164.71 121.63 129.29 2.87 5.34 4/15/07
900 232 252.29 82.56 169.48 124.94 132.93 2.87 5.70 4/15/07
9.13 235 258.44 85.15 174.61 128.52 136.75 3.64 6.47 4/15/07
9.25 238 264.60 87.57 179.60 132.05 140.39 4.14 6.96 4/15/07
9,38 241 270.70 89.80 184.42 135.49 143.99 4.46 7.23 4/15/07
9,50 244 277.03 92.13 189.33 138.98 147.72 4.82 7.54 4/16/07
9,63 247 283.63 94.59 194.41 142.69 151.49 5.19 7.95 4/16/07
9.75 250 290.28 96.95 199.32 146.27 155.31 5.46 8.17 4/16/07
9.88 253 297.10 99.41 204.40 149.99 159.31 5.73 8.49 4/16/07
10.00 256 304.11 101.96 208.33 153.61 163.48 6.10 8.85 4/16/07
10,13 259 311.43 104.69 212.83 157.69 168.01 6.60 9.34 4/16/07
10,25 262 318.92 107.41 217.51 161.77 172.45 6.96 9.70 4/16/07
10,38 265 326.24 110.01 221.89 165.71 176.76 7.14 9.88 4/16/07

72

 

Table D1 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

10.50 268 333.74 112.69 226.30 169.74 181.20 7.42 10.15 4/17/07
10.63 271 341.82 115.68 231.07 174.13 185.95 7.83 10.51 4/17/07
10.75 274 349.50 118.63 235.62 178.39 190.65 8.10 10.78 4/17/07
10,88 277 357.31 121.58 239.99 182.60 195.27 8.24 10.96 4/17/07
11,00 280 365.53 124.85 244.41 187.13 200.20 8.69 11.40 4/17/07
11.13 283 373.97 128.24 248.82 191.80 205.31 9.15 11.85 4/17/07
11,25 286 382.50 131.73 253.60 196.42 210.23 9.60 12.26 4/17/07
11,38 289 391.08 135.17 258.55 201.04 215.21 9.87 12.57 4/17/07
11,50 292 399.88 138.70 263.41 205.48 220.22 10.19 12.84 4/18/07
11,63 295 409.08 142.46 268.31 210.06 225.42 10.60 13.20 4/18/07
11.75 298 418.33 146.30 273.09 214.50 230.44 10.92 13.51 4/18/07
11,88 301 427.63 150.15 277.81 218.80 235.32 11.15 13.74 4/18/07
12,00 304 437.15 154.13 282.76 223.01 240.20 11.38 14.01 4/18/07
12,13 307 446.75 158.19 287.89 227.36 245.09 11.78 14.41 4118/07
12.25 310 456.45 162.31 292.62 231.62 249.71 12.06 14.68 4l18/07
12,38 313 466.20 166.42 297.30 235.88 254.19 12.29 14.91 4/18/07
12,50 316 475.98 170.66 301.90 240.18 258.76 12.60 15.22 4/19/07
12,63 319 485.95 175.09 306.58 244.57 263.34 12.92 15.49 4/19/07
12.75 322 495.74 179.56 311.13 248.88 267.91 13.20 15.76 4/19/07
12.88 325 505.35 184.03 315.55 253.27 272.35 13.24 15.85 4/19/07
13,00 328 514.91 188.59 319.92 257.80 276.97 13.56 16.16 4119/07
13,13 331 524.61 193.55 324.55 262.60 281.90 14.01 16.57 4/19/07
13,25 334 533.73 198.33 328.93 267.27 285.94 14.24 16.79 4/19/07
13,38 337 542.30 203.16 333.12 271.80 291.00 14.38 16.93 4/19l07
13,50 340 550.34 208.12 337.31 276.42 295.57 14.56 17.11 4/20/07
13,63 343 556.54 213.13 341.50 281.04 300.32 14.79 17.29 4/20/07
13.75 346 560.40 218.14 345.61 285.75 305.12 14.97 17.47 4/20/07
13.88 349 562.46 223.01 349.49 290.06 309.69 14.97 17.47 4/20/07
14,00 352 563.72 228.10 353.59 294.90 314.62 15.29 17.74 4/20/07
14,13 355 564.53 233.29 357.69 299.93 319.72 15.74 18.18 4/20/07
14,25 358 565.20 238.52 361.75 304.96 324.92 16.20 18.59 4/20/07
14,38 361 565.61 243.39 365.54 309.76 329.80 16.47 18.90 4/20/07
14,50 364 566.05 248.26 369.15 314.52 334.78 16.79 19.13 4/21/07
14.63 367 566.50 252.87 372.63 319.23 339.70 17.02 19.35 4/21/07
14.75 370 567.00 257.03 375.84 323.99 344.63 17.24 19.58 4/21/07
14,88 373 567.49 260.38 378.83 328.65 349.47 17.43 19.67 4/21/07
15.00 376 568.39 263.06 381.91 333.59 354.62 17.84 20.12 4/21/07
15.13 379 569.38 265.07 384.76 338.66 359.73 18.38 20.61 4/21/07
15.25 382 570.41 266.64 387.40 343.74 364.92 18.88 21.10 4/21/07
15.38 385 571.22 267.66 389.67 348.54 369.99 19.20 21.37 4/21/07
15.50 388 571.94 268.56 391.81 353.34 375.00 19.47 21.69 4/22/07
15,63 391 572.83 269.36 393.91 358.19 380.06 19.88 22.05 4/22/07
15.75 394 573.51 269.81 395.74 362.67 384.86 20.07 22.23 4/22/07
15,88 397 574.14 270.17 397.48 367.20 389.48 20.07 22.23 4/22/07
16,00 400 575.21 270.84 399.53 372.05 394.63 20.38 22.58 4/22/07
16,13 403 576.47 271.55 401.67 377.03 399.82 20.98 23.17 4/22/07
16,25 406 577.77 272.27 403.76 381.97 404.97 21.57 23.71 4/22/07

 

 

 

 

73

 

 

 

 

 

 

Table 0.1 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

16.38 409 578.94 272.71 405.64 386.64 409.86 21.89 24.02 4/22/07
16,50 412 580.11 273.07 407.47 391.12 414.25 22.25 24.34 4/23/07
16,63 415 581.59 273.56 409.43 395.79 419.09 22.70 24.78 4/23/07
16,75 418 583.03 274.06 411.44 400.32 424.02 23.21 25.19 4/23/07
16,88 421 584.01 274.32 413.17 404.62 428.46 23.30 25.37 4/23/07
17,00 424 584.96 274.64 415.05 408.92 432.99 23.66 25.68 4/23/07
17,13 427 585.36 274.73 416.61 412.86 437.03 23.75 25.82 4/23/07
17,25 430 585.36 274.73 418.08 416.53 440.80 23.75 25.82 4/23/07
17,38 433 585.36 274.73 419.37 419.89 444.27 23.75 25.82 4/23/07
17.50 436 585.36 274.73 420.80 423.19 447.77 23.75 25.82 4/24/07
17.63 439 585.36 274.73 422.36 426.50 451.19 23.75 25.82 4/24/07
17,75 442 585.36 274.73 423.97 429.58 454.35 23.75 25.82 4/24/07
17,88 445 585.36 274.73 425.48 432.39 457.32 23.75 25.82 4/24/07
18.00 448 585.36 274.73 427.18 435.11 460.25 23.75 25.82 4/24/07
18,13 451 585.41 274.73 428.96 437.64 462.96 23.75 25.82 4/24/07
18,25 454 585.54 274.73 430.79 439.95 465.40 23.75 25.82 4/24/07
18,38 457 585.59 274.73 432.53 442.04 467.53 23.75 25.82 4/24/07
18,50 460 585.59 274.73 434.18 443.94 469.62 23.75 25.82 4l25107
18,63 463 585.59 274.73 435.92 445.89 471.66 23.75 25.82 4/25/07
18,75 466 585.59 274.73 437.66 447.79 473.66 23.75 25.82 4/25/07
18,88 469 585.59 274.73 439.27 449.47 475.39 23.75 25.82 4/25/07
19,00 472 585.59 274.73 441.09 451.41 477.48 23.75 25.82 4/25/07
19,13 475 585.63 274.73 442.7 453.09 479.25 23.75 25.82 4/25/07
19.25 478 585.63 274.73 444.35 454.81 481.03 23.75 25.82 4/25/07
19,38 481 585.63 274.73 445.91 456.44 482.76 23.75 25.82 4/25/07
19,50 484 585.63 274.73 447.74 458.3 484.71 23.75 25.82 4/26/07
19,63 487 585.72 274.73 449.48 460.2 486.71 24.02 26.04 4/26/07
19,75 490 585.90 274.73 451.22 462.06 488.67 24.48 26.49 4/26/07
19.88 493 585.99 274.73 452.91 463.78 490.62 24.89 26.9 4/26/07
20,00 496 586.12 274.73 454.65 465.64 492.66 25.34 27.34 4/26/07
20.13 499 586.30 274.73 456.35 467.54 494.66 25.8 27.75 4/26/07
20,25 502 586.39 274.73 458.04 469.4 496.7 26.21 28.11 4/26/07
20,38 505 586.48 274.73 459.42 471.26 498.66 26.57 28.47 4/26/07
20.50 508 586.66 274.73 461.12 473.16 500.7 26.98 28.83 4/27/07
20.63 511 586.75 274.73 462.68 474.97 502.47 27.25 29.1 4/27/07
20.75 514 586.80 274.73 464.11 476.65 504.3 27.44 29.23 4/27/07
20.88 517 586.80 274.73 465.31 478.19 505.76 27.44 29.23 4/27/07
21,00 520 586.80 274.73 466.56 479.68 507.36 27.44 29.23 4/27/07
21,13 523 586.80 274.73 467.76 481.22 509 27.44 29.23 4/27/07
21.25 526 586.80 274.73 468.97 482.81 510.64 27.44 29.23 4/27/07
21.38 529 586.80 274.73 470.13 484.35 512.24 27.44 29.23 4/27/07
21.50 532 586.80 274.73 471.38 485.98 513.97 27.44 29.23 4/28/07
21.63 535 586.80 274.73 472.67 487.7 515.66 27.44 29.23 4/28/07
21.75 538 586.80 274.73 473.88 489.38 517.48 27.44 29.23 4/28/07
21,88 541 586.80 274.73 474.99 491.01 519.17 27.44 29.23 4/28/07
22.00 544 586.80 274.73 476.24 492.77 520.95 27.44 29.23 4/28/07
22.13 547 586.93 274.73 477.58 494.59 522.9 27.44 29.23 4/28/07

 

 

 

 

74

 

 

 

 

 

 

Table 0.1 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

22.25 550 587.02 274.73 478.78 496.31 524.63 27.44 29.23 4/28/07
22.38 553 587.07 274.73 479.9 497.89 526.27 27.44 29.23 4/28/07
22.50 556 587.07 274.86 480.88 499.25 527.74 27.44 29.23 4/29/07
22,63 559 587.07 274.86 481.86 500.7 529.25 27.44 29.23 4/29/07
22,75 562 587.07 274.86 482.88 502.15 530.76 27.44 29.23 4/29/07
22,88 565 587.07 274.86 483.78 503.51 532.09 27.44 29.23 4/29/07
23.00 568 587.29 274.86 484.94 505.14 533.73 27.44 29.23 4/29/07
23.13 571 587.74 274.86 486.36 507.04 535.77 27.44 29.23 4/29/07
23,25 574 588.37 274.99 487.75 508.99 537.82 27.66 29.23 4/29/07
23.38 577 588.86 274.99 488.99 510.8 539.73 28.16 29.23 4l29/07
23.50 580 589.45 274.99 490.24 512.57 541.68 28.71 29.32 4/30/07
23,63 583 589.54 275.04 490.91 513.75 542.88 28.71 29.36 4/30/07
23.75 586 589.76 275.04 491.72 515.02 544.21 28.71 29.36 4/30/07
23.88 589 590.12 275.04 492.52 516.33 545.41 28.71 29.36 4/30/07
24,00 592 590.66 275.04 493.45 517.73 546.96 28.71 29.36 4/30/07
24.13 595 591.38 275.04 494.52 519.36 548.74 28.71 29.36 4/30/07
24.25 598 592.19 275.04 495.68 521.09 550.56 28.71 29.36 4/30/07
24.38 601 592.72 275.04 496.44 522.35 551.85 28.71 29.36 4/30/07
24,50 604 593.62 275.04 497.56 524.03 553.76 28.76 29.36 5l1/07
24.63 607 594.52 275.04 498.67 525.75 555.53 29.3 29.36 5/1/07
24,75 610 595.19 275.04 499.56 527.29 557.13 29.53 29.36 5/1/07
24,88 613 595.82 275.04 500.37 528.74 558.64 29.67 29.36 5/1/07
25.00 616 596.95 275.04 501.3 530.46 560.59 30.17 29.41 5/1/07
25.13 619 597.93 275.13 502.46 532.18 562.46 30.62 29.86 5/1/07
25.25 622 598.74 275.13 503.49 533.82 564.19 30.99 30.13 5/1/07
25,38 625 599.15 275.35 504.16 535.13 565.52 31.03 30.17 5/1/07
25,50 628 599.64 275.35 504.92 536.53 566.99 31.21 30.17 5/2/07
25,63 631 599.95 275.35 505.59 537.85 568.45 31.35 30.17 5/2/07
25.75 634 600.18 275.35 506.17 539.16 569.83 31.44 30.17 5/2/07
25.88 637 600.27 275.35 506.66 540.38 571.07 31.44 30.17 5/2/07
26.00 640 600.36 275.35 507.24 541.74 572.45 31.49 30.17 5/2/07
26.13 643 600.72 275.35 507.86 543.19 574 31.71 30.17 5/2/07
26,25 646 601.03 275.35 508.48 544.69 575.6 32.03 30.17 5/2/07
26,38 649 601.12 275.35 508.93 546 576.67 32.08 30.17 5/2/07
26,50 652 601.17 275.35 509.38 547.36 578.31 32.31 30.17 5/3/07
26,63 655 601.17 275.35 509.78 548.72 579.86 32.53 30.17 5/3/07
26.75 658 601 . 17 275.35 510.09 550.12 581.33 32.76 30.17 5/3/07
26.88 661 601.17 275.35 510.27 551.21 582.66 32.85 30.17 5/3/07
27.00 664 601.17 275.35 510.58 552.8 584.17 33.17 30.17 5/3/07
27.13 667 601.26 275.35 510.94 554.38 585.86 33.58 30.17 5/3/07
27.25 670 601.35 275.35 51 1.25 555.92 587.55 33.99 30.17 5123/07
27.38 673 601.39 275. 35 51 1.38 557.33 588.97 34.22 30.17 5/3/07
27.50 676 601.39 275.35 511.43 558.59 590.34 34.49 30.17 5/4/07
27.63 679 601.39 275.35 511.47 560 591.85 34.81 30.17 5/4l07
27,75 682 601.44 275.35 511.52 561.4 593.36 35.13 30.17 514107
27.88 685 601.44 275.35 511.52 562.67 594.65 35.31 30.17 5/4/07
28.00 688 601.44 275.35 511.56 564.03 595.76 35.72 30.17 5/4/07

 

 

 

 

75

 

 

 

 

 

 

Table D1 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

28.13 691 601.62 275.53 511.7 565.71 597.45 36.31 30.17 5/4/07
28,25 694 601.70 275.53 511.96 567.2 599 36.76 30.17 5/4/07
28,38 697 601.84 275.53 512.01 568.65 600.33 37.04 30.17 5/4/07
28,50 700 601.84 275.53 512.01 569.92 601.66 37.36 30.17 5/5/07
28,63 703 601.84 275.53 512.01 571.28 603.09 37.72 30.17 5/5/07
28.75 706 601.93 275.53 512.01 572.59 604.42 38.08 30.17 5/5/07
28,88 709 601.93 275.53 512.01 573.77 605.44 38.31 30.17 5/5/07
29,00 712 601.93 275.53 512.01 575.04 606.64 38.58 30.17 5/5/07
29,13 715 601.93 275.58 512.01 576.17 607.75 38.86 30.17 5/5/07
29.25 718 601.93 275.75 512.01 577.21 608.77 39.04 30.17 5/5/07
29,38 721 601.93 275.75 512.01 578.16 609.66 39.18 30.17 5/5/07
29.50 724 601.93 275.75 512.01 579.02 610.41 39.22 30.17 5/6/07
29,63 727 601.93 275.75 512.01 579.84 611.08 39.31 30.17 5/6/07
29,75 730 601.93 275.75 512.01 580.93 612.05 39.68 30.17 5/6/07
29,88 733 601.93 275.75 512.01 581.65 612.45 39.72 30.17 5/6/07
30,00 736 601.93 275.75 512.01 582.65 613.25 39.9 30.17 5/6/07
30,13 739 601.93 275.75 512.01 583.74 614.14 40.36 30.17 5/6/07
30.25 742 601.93 275.75 512.01 584.82 614.94 40.81 30.17 5/6/07
30,38 745 601.93 275.75 512.01 585.73 615.43 41.04 30.17 5/6/07
30.50 748 601.97 275.75 512.01 586.32 616.01 41.5 30.17 5/7/07
30,63 751 602.15 275.75 512.01 587.36 616.49 41.86 30.17 5/7/07
30,75 754 602.33 275.75 512.01 588.13 616.94 42.22 30.17 5/7/07
30,88 757 602.33 275.75 512.01 588.54 616.98 42.22 30.17 5/7/07
31,00 760 602.47 275.75 512.01 589.22 617.43 42.68 30.17 5/7/07
31.13 763 602.78 275.75 512.01 590.03 617.91 43.22 30.17 5/7/07
31,25 766 603.05 275.75 512.01 590.62 618.27 43.68 30.17 5/7/07
31,38 769 603.28 275.75 512.01 591.07 618.49 44 30.17 5/7/07
31,50 772 603.37 275.75 512.01 591.35 618.54 44.27 30.17 5/8/07
31,63 775 603.50 275.75 512.01 591.71 618.58 44.64 30.31 5/8/07
31.75 778 603.73 275.75 512.01 591.89 618.85 44.82 30.44 5/8/07
31,88 781 603.73 275.75 512.01 591.94 618.85 44.82 30.44 5/8/07
32,00 784 603.73 275.75 512.01 592.03 618.85 44.95 30.44 5/8/07
32.13 787 603.95 275.75 512.01 592.21 618.85 45.23 30.67 5/8/07
32,25 790 604.22 275.75 512.01 592.3 618.85 45.5 30.89 5/8/07
32.38 793 604.31 275.75 512.01 592.3 618.85 45.59 30.94 5/8/07
32.50 796 604.31 275.75 512.01 592.3 618.85 45.59 30.94 5/9/07
32,63 799 604.49 275.75 512.01 592.3 618.85 45.77 31.07 5/9/07
32.75 802 604.67 275.75 512.01 592.3 618.85 45.82 31.21 5/9l07
32,88 805 604.67 275.75 512.01 592.3 618.85 45.82 31.21 5/9/07
33,00 808 604.71 275.75 512.01 592.3 618.85 45.82 31.21 5/9/07
33.13 811 604.80 275.75 512.01 592.3 618.85 45.82 31.21 5/9/07
33.25 814 604.98 275.75 512.01 592.3 618.85 45.82 31.21 5/9/07
33.38 817 605.21 275.75 512.01 592.3 618.85 45.82 31.21 5/9/07
33.50 820 605.30 275.75 512.01 592.3 618.85 45.82 31.21 5/10/07
33,63 823 605.48 275.75 512.01 592.3 618.85 45.82 31.21 5/10/07
33.75 826 605.57 275.75 512.01 592.3 618.85 45.82 31.21 5/10/07
33,88 829 605.70 275.75 512.01 592.3 618.85 45.82 31.21 5/10/07

 

 

 

 

 

 

 

 

 

 

76

 

Table 0.2 Respirometer Calculated Data: Case A Gas Production Rate

 

Gas Production Rate (mUhr)

 

Time

W8

W8

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Day (h n) WSN ‘lz (WSN) 8 (rep A) (rep 8) WM DI

0 0.00 0.00 0.00 0.00 0.00 0.00 0.00

0 0.00 0.04 0.13 0.09 0.13 0.00 0.09

4 2.34 1.88 2.29 2.57 2.77 1.32 2.05

8 0.68 0.17 0.20 0.51 0.58 0.15 0.02

12 0.53 0.09 0.42 0.53 0.58 0.02 0.04

13 0.47 0.09 0.47 0.47 0.51 0.00 0.04

0.00 16 0.54 0.13 0.49 0.48 0.52 0.00 0.06
0.13 19 0.55 0.12 0.49 0.47 0.52 0.00 0.06
0.25 22 0.54 0.07 0.43 0.41 0.44 0.00 0.01
0.38 25 0.54 0.06 0.43 0.41 0.44 0.00 0.00
0.50 28 0.48 0.09 0.40 0.42 0.52 0.00 0.00
0.63 31 0.51 0.15 0.48 0.51 0.55 0.00 0.03
0.75 34 0.50 0.18 0.48 0.50 0.55 0.06 0.05
0.88 37 0.48 0.15 0.45 0.42 0.44 0.03 0.01
1.00 40 0.43 0.12 0.40 0.33 0.39 0.00 0.00
1.13 43 0.54 0.15 0.49 0.39 0.37 0.00 0.00
1.25 46 0.49 0.06 0.42 0.33 0.40 0.00 0.00
1.38 49 0.51 0.05 0.39 0.21 0.38 0.00 0.00
1.50 52 0.57 0.07 0.45 0.45 0.41 0.00 0.00
1.63 55 0.63 0.13 0.46 0.44 0.48 0.00 0.00
1.75 58 0.63 0.09 0.42 0.41 0.46 0.00 0.00
1.88 61 0.63 0.11 0.42 0.41 0.43 0.00 0.00
2.00 64 0.72 0.12 0.43 0.44 0.47 0.00 0.00
2.13 67 0.67 0.15 0.43 0.44 0.49 0.00 0.00
2.25 70 0.75 0.13 0.44 0.45 0.49 0.00 0.00
2.38 73 0.73 0.12 0.42 0.42 0.44 0.00 0.00
2.50 76 0.84 0.16 0.45 0.47 0.46 0.00 0.00
2.63 79 0.82 0.18 0.43 0.47 0.49 0.00 0.00
2.75 82 0.85 0.18 0.45 0.41 0.52 0.00 0.00
2.88 85 0.85 0.20 0.45 0.48 0.49 0.00 0.00
3.00 88 0.89 0.22 0.46 0.50 0.49 0.00 0.00
3.13 91 1.00 0.33 0.54 0.56 0.59 0.00 0.00
3.25 94 0.99 0.30 0.51 0.51 0.55 0.00 0.00
3.38 97 0.90 0.22 0.43 0.47 0.43 0.00 0.00
3.50 100 0.94 0.27 0.51 0.48 0.55 0.00 0.00
3.63 103 0.93 0.25 0.47 0.48 0.50 0.00 0.00
3.75 106 0.96 0.24 0.48 0.45 0.47 0.00 0.00
3.88 109 0.88 0.24 0.46 0.33 0.43 0.00 0.00
4.00 112 0.99 0.30 0.52 0.54 0.52 0.00 0.03
4.13 115 1.09 0.34 0.60 0.54 0.58 0.00 0.12
4.25 118 1.06 0.36 0.61 0.54 0.55 0.00 0.09
4.38 121 1.05 0.33 0.58 0.52 0.53 0.00 0.06

77

 

Table 02 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

4.50 124 1.05 0.31 0.58 0.45 0.49 0.00 0.05
4.63 127 1.15 0.37 0.66 0.54 0.58 0.00 0.10
4.75 130 1.17 0.37 0.67 0.52 0.47 0.00 0.08
4.88 133 1.23 0.40 0.73 0.56 0.56 0.00 0.10
5.00 136 1.38 0.51 0.82 0.63 0.65 0.00 0.18
5.13 139 1.41 0.51 0.80 0.64 0.67 0.26 0.18
5.25 142 1.36 0.46 0.80 0.59 0.62 0.17 0.15
5.38 145 1.44 0.48 0.80 0.59 0.59 0.14 0.13
5.50 148 1.48 0.49 0.85 0.59 0.64 0.17 0.16
5.63 151 1.45 0.45 0.82 0.56 0.56 0.11 0.09
5.75 154 1.36 0.40 0.79 0.48 0.35 0.03 0.03
5.88 157 1.26 0.33 0.73 0.41 0.52 0.00 0.00
6.00 160 1.29 0.39 0.79 0.47 0.47 0.00 0.00
6.13 163 1.26 0.36 0.79 0.41 0.44 0.00 0.00
6.25 166 1.21 0.34 0.79 0.41 0.43 0.00 0.00
6.38 169 1.24 0.39 0.80 0.42 0.44 0.00 0.00
6.50 172 1.36 0.48 0.92 0.50 0.58 0.00 0.00
6.63 175 1.38 0.48 0.95 0.53 0.59 0.00 0.00
6.75 178 1.39 0.49 0.95 0.51 0.56 0.00 0.00
6.88 181 1.41 0.51 0.95 0.53 0.56 0.00 0.00
7.00 184 1.57 0.58 1.06 0.62 0.67 0.00 0.00
7.13 187 1.72 0.68 1.19 0.71 0.67 0.00 0.00
7.25 190 1.48 0.62 1.21 0.72 0.84 0.00 0.00
7.38 193 1.70 0.61 1.20 0.68 0.77 0.00 0.00
7.50 196 1.84 0.68 1.29 0.79 0.86 0.00 0.00
7.63 199 1.88 0.73 1.34 0.83 0.89 0.00 0.00
7.75 202 1.89 0.75 1.35 0.83 0.90 0.00 0.00
7.88 205 1.90 0.76 1.38 0.83 0.93 0.00 0.00
8.00 208 1.90 0.74 1.40 0.89 0.95 0.00 0.00
8.13 211 2.06 0.91 1.58 1.07 1.14 0.00 0.00
8.25 214 1.96 0.82 1.49 1.00 1.04 0.00 0.00
8.38 217 1.89 0.77 1.49 1.00 0.95 0.00 0.00
8.50 220 1.93 0.81 1.55 1.03 1.08 0.00 0.00
8.63 223 1.81 0.80 1.55 1.03 1.07 0.00 0.00
8.75 226 1.94 0.80 1.57 1.04 1.15 0.00 0.00
8.88 229 1.90 0.78 1.56 1.04 1.08 0.00 0.00
9.00 232 1.97 0.80 1.59 1.10 1.21 0.00 0.12
9.13 235 2.05 0.86 1.71 1.19 1.27 0.26 0.26
9.25 238 2.05 0.81 1.66 1.18 1.21 0.17 0.16
9.38 241 2.03 0.74 1.61 1.15 1.20 0.11 0.09
9.50 244 2.11 0.78 1.64 1.16 1.24 0.12 0.10
9.63 247 2.20 0.82 1.69 1.24 1.26 0.12 0.14
9.75 250 2.22 0.79 1.64 1.19 1.27 0.09 0.07
9.88 253 2.27 0.82 1.69 1.24 1.33 0.09 0.11
10.00 256 2.34 0.85 1.31 1.21 1.39 0.12 0.12

 

 

 

 

 

 

 

 

 

78

 

Table 02 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

10.13 259 2.44 0.91 1.50 1.36 1.51 0.17 0.16
10.25 262 2.50 0.91 1.56 1.36 1.48 0.12 0.12
10.38 265 2.44 0.87 1.46 1.31 1.44 0.06 0.06
10.50 268 2.50 0.89 1.47 1.34 1.48 0.09 0.09
10.63 271 2.69 1.00 1.59 1.46 1.58 0.14 0.12
10.75 274 2.56 0.98 1.52 1.42 1.57 0.09 0.09
10.88 277 2.60 0.98 1.46 1.40 1.54 0.05 0.06
11.00 280 2.74 1.09 1.47 1.51 1.64 0.15 0.15
11.13 283 2.81 1.13 1.47 1.56 1.70 0.15 0.15
11.25 286 2.86 1.17 1.60 1.55 1.65 0.15 0.14
11.38 289 2.86 1.15 1.65 1.54 1.66 0.09 0.10
11.50 292 2.93 1.18 1.62 1.48 1.67 0.11 0.09
11.63 295 3.07 1.25 1.63 1.53 1.73 0.14 0.12
11.75 298 3.08 1.28 1.59 1.48 1.67 0.11 0.10
11.88 301 3.10 1.28 1.57 1.43 1.63 0.08 0.08
12.00 304 3.17 1.33 1.65 1.40 1.63 0.08 0.09
12.13 307 3.20 1.35 1.71 1.45 1.63 0.13 0.13
12.25 310 3.23 1.37 1.58 1.42 1.54 0.09 0.09
12.38 313 3.25 1.37 1.56 1.42 1.49 0.08 0.08
12.50 316 3.26 1.41 1.53 1.43 1.52 0.10 0.10
12.63 319 3.32 1.48 1.56 1.46 1.53 0.11 0.09
12.75 322 3.26 1.49 1.52 1.44 1.52 0.09 0.09
12.88 325 3.20 1.49 1.47 1.46 1.48 0.01 0.03
13.00 328 3.19 1.52 1.46 1.51 1.54 0.11 0.10
13.13 331 3.23 1.65 1.54 1.60 1.64 0.15 0.14
13.25 334 3.04 1.59 1.46 1.56 1.35 0.08 0.07
13.38 337 2.86 1.61 1.40 1.51 1.69 0.05 0.05
13.50 340 2.68 1.65 1.40 1.54 1.52 0.06 0.06
13.63 343 2.07 1.67 1.40 1.54 1.58 0.08 0.06
13.75 346 1.29 1.67 1.37 1.57 1.60 0.06 0.06
13.88 349 0.69 1.62 1.29 1.44 1.52 0.00 0.00
14.00 352 0.42 1.70 1.37 1.61 1.64 0.11 0.09
14.13 355 0.27 1.73 1.37 1.68 1.70 0.15 0.15
14.25 358 0.22 1.74 1.35 1.68 1.73 0.15 0.14
14.38 361 0.14 1.62 1.26 1.60 1.63 0.09 0.10
14.50 364 0.15 1.62 1.20 1.59 1.66 0.11 0.08
14.63 367 0.15 1.54 1.16 1.57 1.64 0.08 0.07
14.75 370 0.17 1.39 1.07 1.59 1.64 0.07 0.08
14.88 373 0.16 1.12 1.00 1.55 1.61 0.06 0.03
15.00 376 0.30 0.89 1.03 1.65 1.72 0.14 0.15
15.13 379 0.33 0.67 0.95 1.69 1.70 0.18 0.16
15.25 382 0.34 0.52 0.88 1.69 1.73 0.17 0.16
15.38 385 0.27 0.34 0.76 1.61 1.70 0.11 0.09
15.50 388 0.24 0.30 0.71 1.60 1.67 0.09 0.11
15.63 391 0.30 0.27 0.70 1.62 1.69 0.14 0.12
15.75 394 0.23 0.15 0.61 1.49 1.60 0.06 0.06
15.88 397 0.21 0.12 0.58 1.51 1.54 0.00 0.00

 

79

 

Table 02 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

10.13 259 2.44 0.91 1.50 1.36 1.51 0.17 0.16
10.25 262 2.50 0.91 1.56 1.36 1.48 0.12 0.12
10.38 265 2.44 0.87 1.46 1.31 1.44 0.06 0.06
10.50 268 2.50 0.89 1.47 1.34 1.48 0.09 0.09
10.63 271 2.69 1.00 1.59 1.46 1.58 0.14 0.12
10.75 274 2.56 0.98 1.52 1.42 1.57 0.09 0.09
10.88 277 2.60 0.98 1.46 1.40 1.54 0.05 0.06
11.00 280 2.74 1.09 1.47 1.51 1.64 0.15 0.15
11.13 283 2.81 1.13 1.47 1.56 1.70 0.15 0.15
11.25 286 2.86 1.17 1.60 1.55 1.65 0.15 0.14
11.38 289 2.86 1.15 1.65 1.54 1.66 0.09 0.10
11.50 292 2.93 1.18 1.62 1.48 1.67 0.11 0.09
11.63 295 3.07 1.25 1.63 1.53 1.73 0.14 0.12
11.75 298 3.08 1.28 1.59 1.48 1.67 0.11 0.10
11.88 301 3.10 1.28 1.57 1.43 1.63 0.08 0.08
12.00 304 3.17 1.33 1.65 1.40 1.63 0.08 0.09
12.13 307 3.20 1.35 1.71 1.45 1.63 0.13 0.13
12.25 310 3.23 1.37 1.58 1.42 1.54 0.09 0.09
12.38 313 3.25 1.37 1.56 1.42 1.49 0.08 0.08
12.50 316 3.26 1.41 1.53 1.43 1.52 0.10 0.10
12.63 319 3.32 1.48 1.56 1.46 1.53 0.11 0.09
12.75 322 3.26 1.49 1.52 1.44 1.52 0.09 0.09
12.88 325 3.20 1.49 1.47 1.46 1.48 0.01 0.03
13.00 328 3.19 1.52 1.46 1.51 1.54 0.11 0.10
13.13 331 3.23 1.65 1.54 1.60 1.64 0.15 0.14
13.25 334 3.04 1.59 1.46 1.56 1.35 0.08 0.07
13.38 337 2.86 1.61 1.40 1.51 1.69 0.05 0.05
13.50 340 2.68 1.65 1.40 1.54 1.52 0.06 0.06
13.63 343 2.07 1.67 1.40 1.54 1.58 0.08 0.06
13.75 346 1.29 1.67 1.37 1.57 1.60 0.06 0.06
13.88 349 0.69 1.62 1.29 1.44 1.52 0.00 0.00
14.00 352 0.42 1.70 1.37 1.61 1.64 0.11 0.09
14.13 355 0.27 1.73 1.37 1.68 1.70 0.15 0.15
14.25 358 0.22 1.74 1.35 1.68 1.73 0.15 0.14
14.38 361 0.14 1.62 1.26 1.60 1.63 0.09 0.10
14.50 364 0.15 1.62 1.20 1.59 1.66 0.11 0.08
14.63 367 0.15 1.54 1.16 1.57 1.64 0.08 0.07
14.75 370 0.17 1.39 1.07 1.59 1.64 0.07 0.08
14.88 373 0.16 1.12 1.00 1.55 1.61 0.06 0.03
15.00 376 0.30 0.89 1.03 1.65 1.72 0.14 0.15
15.13 379 0.33 0.67 0.95 1.69 1.70 0.18 0.16
15.25 382 0.34 0.52 0.88 1.69 1.73 0.17 0.16
15.38 385 0.27 0.34 0.76 1.61 1.70 0.11 0.09
15.50 388 0.24 0.30 0.71 1.60 1.67 0.09 0.11
15.63 391 0.30 0.27 0.70 1.62 1.69 0.14 0.12
15.75 394 0.23 0.15 0.61 1.49 1.60 0.06 0.06
15.88 397 0.21 0.12 0.58 1.51 1.54 0.00 0.00

 

79

 

Table D2 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

21.88 541 0.00 0.00 0.37 0.54 0.56 0.00 0.00
22.00 544 0.00 0.00 0.42 0.59 0.59 0.00 0.00
22.13 547 0.04 0.00 0.45 0.61 0.65 0.00 0.00
22.25 550 0.03 0.00 0.40 0.57 0.58 0.00 0.00
22.38 553 0.02 0.00 0.37 0.53 0.55 0.00 0.00
22.50 556 0.00 0.04 0.33 0.45 0.49 0.00 0.00
22.63 559 0.00 0.00 0.33 0.48 0.50 0.00 0.00
22.75 562 0.00 0.00 0.34 0.48 0.50 0.00 0.00
22.88 565 0.00 0.00 0.30 0.45 0.44 0.00 0.00
23.00 568 0.07 0.00 0.39 0.54 0.55 0.00 0.00
23.13 571 0.15 0.00 0.47 0.63 0.68 0.00 0.00
23.25 574 0.21 0.04 0.46 0.65 0.68 0.07 0.00
23.38 577 0.16 0.00 0.41 0.60 0.64 0.17 0.00
23.50 580 0.20 0.00 0.42 0.59 0.65 0.18 0.03
23.63 583 0.03 0.02 0.22 0.40 0.40 0.00 0.01
23.75 586 0.07 0.00 0.27 0.42 0.44 0.00 0.00
23.88 589 0.12 0.00 0.27 0.44 0.40 0.00 0.00
24.00 592 0.18 0.00 0.31 0.47 0.52 0.00 0.00
24.13 595 0.24 0.00 0.36 0.54 0.59 0.00 0.00
24.25 598 0.27 0.00 0.39 0.58 0.61 0.00 0.00
24.38 601 0.18 0.00 0.25 0.42 0.43 0.00 0.00
24.50 604 0.30 0.00 0.37 0.56 0.64 0.02 0.00
24.63 607 0.30 0.00 0.37 0.57 0.59 0.18 0.00
24.75 610 0.22 0.00 0.30 0.51 0.53 0.08 0.00
24.88 613 0.21 0.00 0.27 0.48 0.50 0.05 0.00
25.00 616 0.38 0.00 0.31 0.57 0.65 0.17 0.02
25.13 619 0.33 0.03 0.39 0.57 0.62 0.15 0.15
25.25 622 0.27 0.00 0.34 0.55 0.58 0.12 0.09
25.38 625 0.14 0.07 0.22 0.44 0.44 0.01 0.01
25.50 628 0.16 0.00 0.25 0.47 0.49 0.06 0.00
25.63 631 0.10 0.00 0.22 0.44 0.49 0.05 0.00
25.75 634 0.08 0.00 0.19 0.44 0.46 0.03 0.00
25.88 637 0.03 0.00 0.16 0.41 0.41 0.00 0.00
26.00 640 0.03 0.00 0.19 0.45 0.46 0.02 0.00
26.13 643 0.12 0.00 0.21 0.48 0.52 0.07 0.00
26.25 646 0.10 0.00 0.21 0.50 0.53 0.11 0.00
26.38 649 0.03 0.00 0.15 0.44 0.36 0.02 0.00
26.50 652 0.02 0.00 0.15 0.45 0.55 0.08 0.00
26.63 655 0.00 0.00 0.13 0.45 0.52 0.07 0.00
26.75 658 0.00 0.00 0.10 0.47 0.49 0.08 0.00
26.88 661 0.00 0.00 0.06 0.36 0.44 0.03 0.00
27.00 664 0.00 0.00 0.10 0.53 0.50 0.11 0.00
27.13 667 0.03 0.00 0.12 0.53 0.57 0.14 0.00
27.25 670 0.03 0.00 0.10 0.51 0.56 0.14 0.00
27.38 673 0.01 0.00 0.04 0.47 0.47 0.08 0.00
27.50 676 0.00 0.00 0.02 0.42 0.46 0.09 0.00
27.63 679 0.00 0.00 0.01 0.47 0.50 0.11 0.00

81

 

Table D2 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

16.00 400 0.36 0.22 0.68 1.62 1.72 0.10 0.12
16.13 403 0.42 0.24 0.71 1.66 1.73 0.20 0.20
16.25 406 0.43 0.24 0.70 1.65 1.72 0.20 0.18
16.38 409 0.39 0.15 0.63 1.56 1.63 0.11 0.10
16.50 412 0.39 0.12 0.61 1.49 1.46 0.12 0.11
16.63 415 0.49 0.16 0.65 1.56 1.61 0.15 0.15
16.75 418 0.48 0.17 0.67 1.51 1.64 0.17 0.14
16.88 421 0.33 0.09 0.58 1.43 1.48 0.03 0.06
17.00 424 0.32 0.11 0.63 1.43 1.51 0.12 0.10
17.13 427 0.13 0.03 0.52 1.31 1.35 0.03 0.05
17.25 430 0.00 0.00 0.49 1.22 1.26 0.00 0.00
17.38 433 0.00 0.00 0.43 1.12 1.16 0.00 0.00
17.50 436 0.00 0.00 0.48 1.10 1.17 0.00 0.00
17.63 439 0.00 0.00 0.52 1.10 1.14 0.00 0.00
17.75 442 0.00 0.00 0.54 1.03 1.05 0.00 0.00
17.88 445 0.00 0.00 0.50 0.94 0.99 0.00 0.00
18.00 448 0.00 0.00 0.57 0.91 0.98 0.00 0.00
18.13 451 0.02 0.00 0.59 0.84 0.90 0.00 0.00
18.25 454 0.04 0.00 0.61 0.77 0.81 0.00 0.00
18.38 457 0.02 0.00 0.58 0.70 0.71 0.00 0.00
18.50 460 0.00 0.00 0.55 0.63 0.70 0.00 0.00
18.63 463 0.00 0.00 0.58 0.65 0.68 0.00 0.00
18.75 466 0.00 0.00 0.58 0.63 0.67 0.00 0.00
18.88 469 0.00 0.00 0.54 0.56 0.58 0.00 0.00
19.00 472 0.00 0.00 0.61 0.65 0.70 0.00 0.00
19.13 475 0.01 0.00 0.54 0.56 0.59 0.00 0.00
19.25 478 0.00 0.00 0.55 0.57 0.59 0.00 0.00
19.38 481 0.00 0.00 0.52 0.54 0.58 0.00 0.00
19.50 484 0.00 0.00 0.61 0.62 0.65 0.00 0.00
19.63 487 0.03 0.00 0.58 0.63 0.67 0.09 0.07
19.75 490 0.06 0.00 0.58 0.62 0.65 0.15 0.15
19.88 493 0.03 0.00 0.56 0.57 0.65 0.14 0.14
20.00 496 0.04 0.00 0.58 0.62 0.68 0.15 0.15
20.13 499 0.06 0.00 0.57 0.63 0.67 0.15 0.14
20.25 502 0.03 0.00 0.56 0.62 0.68 0.14 0.12
20.38 505 0.03 0.00 0.46 0.62 0.65 0.12 0.12
20.50 508 0.06 0.00 0.57 0.63 0.68 0.14 0.12
20.63 511 0.03 0.00 0.52 0.60 0.59 0.09 0.09
20.75 514 0.02 0.00 0.48 0.56 0.61 0.06 0.04
20.88 517 0.00 0.00 0.40 0.51 0.49 0.00 0.00
21.00 520 0.00 0.00 0.42 0.50 0.53 0.00 0.00
21.13 523 0.00 0.00 0.40 0.51 0.55 0.00 0.00
21.25 526 0.00 0.00 0.40 0.53 0.55 0.00 0.00
21 .38 529 0.00 0.00 0.39 0.51 0.53 0.00 0.00
21.50 532 0.00 0.00 0.42 0.54 0.58 0.00 0.00
21 .63 535 0.00 0.00 0.43 0.57 0.56 0.00 0.00
21.75 538 0.00 0.00 0.40 0.56 0.61 0.00 0.00

80

 

Table D2 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

27.75 682 0.02 0.00 0.02 0.47 0.50 0.11 0.00
27.88 685 0.00 0.00 0.00 0.42 0.43 0.06 0.00
28.00 688 0.00 0.00 0.01 0.45 0.37 0.14 0.00
28.13 691 0.06 0.06 0.05 0.56 0.56 0.20 0.00
28.25 694 0.03 0.00 0.09 0.50 0.52 0.15 0.00
28.38 697 0.05 0.00 0.02 0.48 0.44 0.09 0.00
28.50 700 0.00 0.00 0.00 0.42 0.44 0.11 0.00
28.63 703 0.00 0.00 0.00 0.45 0.48 0.12 0.00
28.75 706 0.03 0.00 0.00 0.44 0.44 0.12 0.00
28.88 709 0.00 0.00 0.00 0.39 0.34 0.08 0.00
29.00 712 0.00 0.00 0.00 0.42 0.40 0.09 0.00
29.13 715 0.00 0.02 0.00 0.38 0.37 0.09 0.00
29.25 718 0.00 0.06 0.00 0.35 0.34 0.06 0.00
29.38 721 0.00 0.00 0.00 0.32 0.30 0.05 0.00
29.50 724 0.00 0.00 0.00 0.29 0.25 0.01 0.00
29.63 727 0.00 0.00 0.00 0.27 0.22 0.03 0.00
29.75 730 0.00 0.00 0.00 0.36 0.32 0.12 0.00
29.88 733 0.00 0.00 0.00 0.24 0.13 0.01 0.00
30.00 736 0.00 0.00 0.00 0.33 0.27 0.06 0.00
30.13 739 0.00 0.00 0.00 0.36 0.30 0.15 0.00
30.25 742 0.00 0.00 0.00 0.36 0.27 0.15 0.00
30.38 745 0.00 0.00 0.00 0.30 0.16 0.08 0.00
30.50 748 0.01 0.00 0.00 0.20 0.19 0.15 0.00
30.63 751 0.06 0.00 0.00 0.35 0.16 0.12 0.00
30.75 754 0.06 0.00 0.00 0.26 0.15 0.12 0.00
30.88 757 0.00 0.00 0.00 0.14 0.01 0.00 0.00
31.00 760 0.05 0.00 0.00 0.23 0.15 0.15 0.00
31.13 763 0.10 0.00 0.00 0.27 0.16 0.18 0.00
31.25 766 0.09 0.00 0.00 0.20 0.12 0.15 0.00
31.38 769 0.08 0.00 0.00 0.15 0.07 0.11 0.00
31.50 772 0.03 0.00 0.00 0.09 0.02 0.09 0.00
31.63 775 0.04 0.00 0.00 0.12 0.01 0.12 0.05
31.75 778 0.08 0.00 0.00 0.06 0.09 0.06 0.04
31.88 781 0.00 0.00 0.00 0.02 0.00 0.00 0.00
32.00 784 0.00 0.00 0.00 0.03 0.00 0.04 0.00
32.13 787 0.07 0.00 0.00 0.06 0.00 0.09 0.08
32.25 790 0.09 0.00 0.00 0.03 0.00 0.09 0.07
32.38 793 0.03 0.00 0.00 0.00 0.00 0.03 0.02
32.50 796 0.00 0.00 0.00 0.00 0.00 0.00 0.00
32.63 799 0.06 0.00 0.00 0.00 0.00 0.06 0.04
32.75 802 0.06 0.00 0.00 0.00 0.00 0.02 0.05
32.88 805 0.00 0.00 0.00 0.00 0.00 0.00 0.00
33.00 808 0.01 0.00 0.00 0.00 0.00 0.00 0.00
33.13 811 0.03 0.00 0.00 0.00 0.00 0.00 0.00
33.25 814 0.06 0.00 0.00 0.00 0.00 0.00 0.00
33.38 817 0.08 0.00 0.00 0.00 0.00 0.00 0.00
33.50 820 0.03 0.00 0.00 0.00 0.00 0.00 0.00

82

 

Table 02 continued

 

 

 

 

 

 

 

 

 

 

 

 

33.63 823 0.06 0.00 0.00 0.00 0.00 0.00 0.00
33.75 826 0.03 0.00 0.00 0.00 0.00 0.00 0.00
33.88 829 0.04 0.00 0.00 0.00 0.00 0.00 0.00

 

83

 

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8:528 on 032

87

Table D.4 Respirometer Calculated Data: Case B-1 Gas Production Rate

 

Gas Production Rate (mUhr)

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

88

 

 

 

 

Time Time WS ‘la W3 W8

(days) (hrs) WSN N 8 (rep A) (rep BL WN DI ‘la (WSN)
0 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

4 1.94 2.06 1.57 2.06 2.14 1.63 1.18 1.57

8 0.21 0.44 0.07 0.35 0.21 0.11 0.03 0.01

0.00 12 0.16 0.30 0.00 0.27 0.16 0.00 0.00 0.00
0.17 16 0.17 0.34 0.01 0.33 0.28 0.00 0.00 0.00
0.33 20 0.17 0.34 0.11 0.33 0.25 0.00 0.00 0.00
0.50 24 0.22 0.38 0.16 0.35 0.31 0.00 0.00 0.00
0.67 28 0.31 0.44 0.24 0.41 0.37 0.00 0.02 0.03
0.83 32 0.30 0.46 0.26 0.42 0.38 0.00 0.07 0.16
1.00 36 0.29 0.42 0.24 0.38 0.33 0.00 0.03 0.09
1.17 40 0.31 0.45 0.27 0.39 0.36 0.00 0.04 0.13
1.33 44 0.31 0.42 0.24 0.33 0.27 0.00 0.01 0.07
1.50 48 0.27 0.39 0.21 0.32 0.28 0.00 0.00 0.04
1.67 52 0.31 0.44 0.26 0.36 0.34 0.00 0.00 0.11
1.83 56 0.32 0.44 0.26 0.35 0.31 0.00 0.01 0.09
2.00 60 0.26 0.37 0.19 0.27 0.26 0.00 0.00 0.03
2.17 64 0.30 0.41 0.24 0.32 0.29 0.00 0.00 0.06
2.33 68 0.32 0.41 0.22 0.31 0.24 0.00 0.00 0.04
2.50 72 0.32 0.44 0.27 0.33 0.30 0.00 0.00 0.04
2.67 76 0.44 0.52 0.35 0.41 0.41 0.00 0.00 0.16
2.83 80 0.44 0.50 0.36 0.40 0.39 0.00 0.00 0.14
3.00 84 0.37 0.45 0.30 0.35 0.32 0.00 0.00 0.08
3.17 88 0.42 0.49 0.32 0.36 0.34 0.00 0.00 0.09
3.33 92 0.41 0.48 0.32 0.36 0.31 0.00 0.00 0.08
3.50 96 0.49 0.50 0.35 0.39 0.40 0.00 0.00 0.13
3.67 100 0.69 0.59 0.46 0.45 0.50 0.00 0.00 0.24
3.83 104 0.66 0.57 0.43 0.44 0.48 0.00 0.02 0.19
4.00 108 0.57 0.48 0.36 0.35 0.37 0.00 0.02 0.12
4.17 112 0.59 0.49 0.38 0.38 0.40 0.00 0.00 0.14
4.33 116 0.54 0.52 0.41 0.40 0.39 0.00 0.02 0.14
4.50 120 0.50 0.55 0.44 0.19 0.47 0.00 0.06 0.19
4.67 124 0.55 0.62 0.49 0.60 0.50 0.00 0.09 0.24
4.83 128 0.55 0.60 0.50 0.50 0.51 0.00 0.08 0.23
5.00 132 0.45 0.54 0.42 0.33 0.41 0.00 0.02 0.14
5.17 136 0.51 0.58 0.47 0.25 0.45 0.00 0.00 0.18
5.33 140 0.50 0.61 0.48 0.54 0.43 0.00 0.00 0.17
5.50 144 0.56 0.65 0.50 0.43 0.53 0.00 0.03 0.25
5.67 148 0.58 0.70 0.53 0.41 0.56 0.00 0.07 0.26
5.83 152 0.62 0.74 0.56 0.62 0.58 0.00 0.10 0.29
6.00 156 0.53 0.65 0.48 0.49 0.50 0.00 0.02 0.19
6.17 160 0.57 0.68 0.52 0.53 0.53 0.00 0.00 0.24
6.33 164 0.61 0.74 0.56 0.57 0.56 0.00 0.03 0.26
6.50 168 0.58 0.72 0.54 0.56 0.56 0.00 0.01 0.24

 

Table D4 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

6.67 172 0.57 0.82 0.61 0.65 0.57 0.00 0.03 0.26
6.83 176 0.68 0.84 0.64 0.68 0.70 0.00 0.09 0.35
7.00 180 0.62 0.76 0.59 0.61 0.62 0.00 0.04 0.28
7.17 184 0.64 0.78 0.60 0.64 0.66 0.00 0.07 0.32
7.33 188 0.63 0.75 0.62 0.64 0.66 0.00 0.03 0.32
7.50 192 0.67 0.77 0.63 0.69 0.70 0.00 0.08 0.35
7.67 196 0.70 0.77 0.67 0.72 0.73 0.00 0.09 0.40
7.83 200 0.65 0.73 0.61 0.69 0.70 0.00 0.10 0.35
8.00 204 0.67 0.75 0.65 0.75 0.75 0.00 0.03 0.40
8.17 208 0.70 0.77 0.64 0.78 0.80 0.04 0.13 0.44
8.33 212 0.64 0.73 0.61 0.75 0.75 0.10 0.08 0.42
8.50 216 0.59 0.68 0.58 0.75 0.74 0.06 0.08 0.40
8.67 220 0.59 0.69 0.60 0.77 0.79 0.10 0.10 0.44
8.83 224 0.53 0.67 0.60 0.76 0.78 0.08 0.08 0.43
9.00 228 0.50 0.61 0.57 0.75 0.79 0.09 0.10 0.43
9.17 232 0.48 0.64 0.59 0.76 0.81 0.12 0.11 0.48
9.33 236 0.39 0.55 0.57 0.69 0.73 0.06 0.05 0.41
9.50 240 0.32 0.50 0.54 0.68 0.73 0.00 0.06 0.41
9.67 244 0.37 0.51 0.58 0.70 0.79 0.10 0.11 0.47
9.83 248 0.36 0.42 0.52 0.62 0.76 0.03 0.05 0.39
10.00 252 0.19 0.27 0.43 0.51 0.63 0.00 0.00 0.32
10.17 256 0.17 0.26 0.44 0.50 0.64 0.00 0.00 0.32
10.33 260 0.08 0.17 0.38 0.43 0.52 0.00 0.00 0.25
10.50 264 0.05 0.15 0.38 0.43 0.52 0.00 0.00 0.29
10.67 268 0.00 0.15 0.38 0.45 0.53 0.00 0.00 0.31
10.83 272 0.00 0.12 0.36 0.42 0.51 0.00 0.00 0.32
11.00 276 0.00 0.03 0.31 0.36 0.39 0.00 0.00 0.26
11.17 280 0.00 0.05 0.31 0.38 0.37 0.00 0.00 0.27
11.33 284 0.00 0.02 0.28 0.28 0.32 0.00 0.00 0.24
11.50 288 0.00 0.02 0.28 0.22 0.35 0.00 0.00 0.30
11.67 292 0.00 0.05 0.27 0.38 0.38 0.00 0.00 0.33
11.83 296 0.00 0.07 0.25 0.22 0.31 0.00 0.00 0.33
12.00 300 0.00 0.03 0.19 0.32 0.19 0.00 0.00 0.24
12.17 304 0.00 0.06 0.22 0.24 0.25 0.00 0.00 0.35
12.33 308 0.00 0.02 0.13 0.15 0.16 0.00 0.00 0.27
12.50 312 0.00 0.08 0.16 0.17 0.20 0.00 0.00 0.33
12.67 316 0.00 0.00 0.07 0.26 0.09 0.00 0.00 0.23
12.83 320 0.01 0.09 0.17 0.21 0.18 0.00 0.13 0.35
13.00 324 0.00 0.00 0.00 0.02 0.00 0.00 0.03 0.18
13.17 328 0.00 0.00 0.01 0.05 0.01 0.00 0.07 0.18
13.33 332 0.00 0.00 0.00 0.01 0.00 0.00 0.01 0.07
13.50 336 0.00 0.00 0.00 0.00 0.00 0.00 0.03 0.09
13.67 340 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
13.83 344 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
14.00 348 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
14.17 352 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
14.33 356 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

89

 

Table 04 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

14.50 360 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
14.67 364 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
14.83 368 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
15.00 372 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
15.17 376 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
15.33 380 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
15.50 384 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
15.67 388 0.00 0.00 0.00 0.06 0.00 0.00 0.00 0.00
15.83 392 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
16.00 396 0.00 0.00 0.00 0.05 0.00 0.00 0.00 0.00
16.17 400 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
16.33 404 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
16.50 407 0.00 0.05 0.00 0.00 0.00 0.00 0.00 0.00

 

 

 

 

 

90

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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396 .3 CC.0 N0.C0 60 .CN. .009 3N.Nn. C0.. 33.60. 06.30. 0N0 30. .N
396 .3 CC.0 .000 00.0.. 0. 6C. 6. .Nn. C0.. N360. 06.3n. 6N0 C0. .N
396.3 CC.0 03.06 0.0.. 00.NC. .6..0. C0.. C060. 0630. CNO nn..N
396 .3 CC.0 N006 .N.0.. 00. .C. 6000. C0.. C060. 06.30. 0.0 3.. .N
390 .3 CC.0 66.06 CN.3.. N0.CC. NO0N. C0. . C060 . 06.30. N .0 CC. .N
390 .3 CC.0 66.06 0. .0. . 60.00 0 . .0N. C0. . C060. 06.30. 0C0 00.CN
390 .3 CC.0 66.06 60.0.. C . .00 360N. C0.. C060 . 06.30. 600 30.CN
390 .3 CC.0 3.06 36.6.. 0N00 N0.3N. C0.. C0 .60. 06.30. CCO C0.CN
390 .3 CC.0 3.06 N0.n.. 60.30 0NON. C0.. C060. 0630. 006 00.CN
390 .3 CC.0 3.06 00 .N.. 03.00 00.6N. C0.. C060. 06.30. N06 3..CN
39N .3 CC.0 0C06 00.... 00.00 C0.nN. C0. . C060 . 06.30 . 006 CC.CN
39N .3 CC.0 60.06 .00.. 6.00 .0. .N. C0.. C060. 06.30. 606 00.0.
39N .3 CC.0 N306 N60C. 3 .60 0C.CN. C0.. C0 .60. 06.30. C06 30.0.

 

 

 

 

 

 

 

 

 

 

 

 

00:52.60 0 d 0.3.0...

95

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

39NN3 C0. .. .n.00 N.. .N. .0 .0N. 06.60. 00.0 66.00. .3.3n. 6N3 n0.0N
39NN3 C0... .n.00 N...N. .0.0N. 06.60. 00.0 66.00. .3.30. CN3 30.0N
39NN3 C0. .. .n.00 N...N. .0.0N. 06.60. 00.0 66.00. .3.30. 0.3 C0.0N
39NN3 C0. .. .n.00 N...N. .0.0N. 06.60. 00.0 66.00. .3.30. N .3 00.0N
39NN3 C0. .. .n.00 N...N. .0 .0N. 0660. 00.0 66.00. .3.30. 0C3 3..0N
39.N3 C0. .. .n.00 N...N. .0.0N. 06.60. 00.0 66.00. .3.30. 6C3 CC.0N
39.N3 C0. .. .n.00 N.. .N. .0.0N. 06.60. 00.0 66.00. .3.3n. CC3 n0.0N
39.N3 C0. .. .n.00 N...N. .0.0N. 06.60. 00.0 66.00. .3.30. 000 30.0N
39.N3 C0. .. .n.00 N. . .N. .0.0N. 06.60. 00.0 66.00. .330. N00 C0.0N
39.N3 C0. .. .0.00 N.. .N. .0.0N. 06.60. 00.0 66.00. .3.3n. 000 00.0N
39.N3 C0. .. .n.00 N.. .N. .0.0N. 06.60. 00.0 66.00. .3.3n. 600 3 .0N
39CN3 C0. .. .0.00 N.. .N. .0 .0N. 06.60. 00.0 66.00. .3.3n. C00 CC.0N
39CN3 C0. .. .n.00 N.. .N. .0.0N. 06.60. 00.0 66.00. .3.3n. 030 00.3N
39CN3 C0. .. 0N.00 N. . .N. .0.0N. 06.60. 00.0 66.00 . .330. N30 30.3N
39CN3 C0. .. 0N.00 N.. .N. .0.0N. 06.60. 00.0 66.00. .3.30. 000 C0.3N
39CN3 C0. .. 0N.00 N...N. .0.0N. 0660. 00.0 66.00. .3.30. 600 nn.3N
39CN3 C0... 0N.00 N.. .N. .0.0N. 06.60. 00.0 66.00. .330. C00 3..3N
390 .3 C0. .. 0N.00 N.. .N. .0.0N. 06.60. 00.0 66.00. .3.3n. 000 CC.3N
390 .3 C0. .. NN.00 N...N. .0.0N. 06.60. 00.0 66.00. .3.30. N00 n0.0N
390 .3 C0. .. n..00 N...N. .0.0N. 06.60. 00.0 66.00. .3.3n. 060 30.0N
390 .3 .0. .. n3.N0 N...N. .0.0N. 06.60. 03.0 66.00. .3.3n. 660 C0.0N
390 .3 06. .. 0N.N0 N.. .N. .0 .0N. 06.60. 03.0 V6.00. .3.3n. C60 nn.0N
390 .3 0N. .. 00. .0 N...N. 00.0N. 06.60. 00.0 66.00. .3.3n. 000 3..0N
390 .3 0.... CN. .0 N...N. 6NON. 06.60. 30.0 66.00. .3.3n. N00 CC.0N
390 .3 .C. .. 00.C0 N...N. NC.0N. 0660. 00.0 66.00. .3.3n. 0N0 00.0N
390 .3 03.0. C000 N.. .N. 30.0N. 06.60. 0C.n 66.00. .3.3n. 6N0 30.0N
390 .3 N00. 0 . .00 N...N. n . .0N. 06.6n. 33.N 66.00. .3.3n. CNO C0.0N
390 .3 0 ..C. 60.00 N...N. N0.3N. 06.6n. 00.N 66.00. .3.3n. 0.0 nn.0N
390.3 .C.C. 0.00 N...N. 0n.3N. 06.6n. 60N 66.00. .3.30. N.0 3..0N
3C3 .3 .00 C330 N...N. NC.3N. 06.6n. 06.N 66.00. .3.30. 0C0 CC.0N
393.3 N00 60.30 N...N. 06.0N. 06.6n. Nn.N 66.00. .3.3n. 6C0 00.6N

 

 

 

 

 

 

 

 

 

 

 

 

3333338 3.3 3.33.

96

 

 

 

 

 

 

 

390N3 C0... .n.00 N...N. .0.0N. 06.60. 00.0 66.00. .3.3n. 063 3000
390N3 C0. .. .n.00 N...N. .0.0N. 06.60. 00.0 66.00. .3.3n. C63 C0.C0
390N3 C0... .n.00 N...N. .0.0N. 0660. 00.0 66.00. .3.3n. 003 00.C0
390N3 C0... .n.00 N...N. .0.0N. 06.60. 00.0 66.00. .3.3n. N03 3..Cn
39NN3 C0... .n.00 N...N. .0.0N. 06.60. 00.0 66.00. .3.30. 0N3 CC.Cn

 

 

 

 

 

 

 

 

 

 

 

0025.50 0.0 030.3

97

Table 0.6 Respirometer Calculated Data: Case B-2 Gas Production Rate

 

Gas Production Rate (mUhr)

 

Time

Time

WSN

WSN

WS

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Adan) (my (rep A) (rep 8) V: N “’s s 3" ”(“3” °'

0 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

4 1.44 1.28 1.34 1.26 1.21 1.28 1.06 1.15
0.00 8 0.01 0.01 0.04 0.04 0.02 0.01 0.00 0.05
0.17 12 0.01 0.00 0.01 0.02 0.00 0.00 0.00 0.04
0.33 16 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.50 20 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.67 24 0.00 0.00 0.04 0.10 0.00 0.00 0.00 0.01
0.83 28 0.10 0.03 0.11 0.10 0.06 0.00 0.00 0.07
1.00 32 0.03 0.04 0.04 0.03 0.01 0.00 0.00 0.00
1.17 36 0.03 0.01 0.02 0.02 0.00 0.00 0.00 0.00
1.33 40 0.04 0.03 0.02 0.02 0.00 0.00 0.00 0.00
1.50 44 0.04 0.04 0.01 0.05 0.00 0.00 0.00 0.00
1.67 48 0.07 0.07 0.00 0.07 0.01 0.00 0.00 0.00
1.83 52 0.08 0.08 0.00 0.08 0.07 0.00 0.00 0.02
2.00 56 0.01 0.00 0.00 0.01 0.01 0.00 0.00 0.00
2.17 60 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
2.33 64 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
2.50 68 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
2.67 72 0.00 0.00 0.00 0.02 0.00 0.00 0.00 0.00
2.83 76 0.04 0.05 0.00 0.06 0.02 0.07 0.00 0.00
3.00 80 0.02 0.02 0.00 0.02 0.02 0.03 0.00 0.00
3.17 84 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
3.33 88 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
3.50 92 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
3.67 96 0.04 0.03 0.00 0.07 0.02 0.07 0.00 0.00
3.83 100 0.14 0.10 0.00 0.11 0.12 0.12 0.00 0.01
4.00 104 0.03 0.04 0.00 0.02 0.03 0.04 0.00 0.03
4.17 108 0.01 0.01 0.00 0.02 0.00 0.00 0.00 0.00
4.33 112 0.06 0.04 0.00 0.06 0.04 0.08 0.00 0.00
4.50 116 0.04 0.05 0.00 0.05 0.02 0.05 0.00 0.01
4.67 120 0.07 0.07 0.00 0.04 0.03 0.00 0.02 0.02
4.83 124 0.10 0.09 0.00 0.10 0.09 0.13 0.08 0.07
5.00 128 0.01 0.01 0.00 0.01 0.01 0.02 0.00 0.00
5.17 132 0.02 0.00 0.00 0.00 0.00 0.01 0.00 0.00
5.33 136 0.00 0.00 0.00 0.00 0.00 0.04 0.00 0.00
5.50 140 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
5.67 144 0.05 0.03 0.00 0.02 0.00 0.06 0.00 0.00
5.83 148 0.08 0.07 0.00 0.06 0.01 0.07 0.00 0.00
6.00 152 0.01 0.01 0.00 0.01 0.00 0.02 0.00 0.00
6.17 156 0.03 0.02 0.00 0.02 0.00 0.04 0.00 0.00
6.33 160 0.07 0.05 0.00 0.04 0.00 0.07 0.00 0.00
6.50 164 0.03 0.02 0.00 0.02 0.00 0.01 0.00 0.00
6.67 168 0.13 0.12 0.00 0.03 0.07 0.09 0.00 0.00

 

98

 

Table 0.6 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

6.83 172 0.16 0.15 0.00 0.18 0.12 0.16 0.00 0.00
7.00 176 0.08 0.07 0.00 0.06 0.02 0.06 0.00 0.00
7.17 180 0.07 0.05 0.00 0.04 0.01 0.06 0.04 0.00
7.33 184 0.09 0.09 0.00 0.08 0.08 0.13 0.06 0.00
7.50 188 0.10 0.08 0.00 0.08 0.03 0.08 0.01 0.00
7.67 192 0.18 0.17 0.00 0.16 0.11 0.16 0.09 0.00
7.83 196 0.17 0.16 0.00 0.14 0.13 0.17 0.08 0.00
8.00 200 0.11 0.10 0.00 0.10 0.03 0.08 0.01 0.00
8.17 204 0.06 0.05 0.00 0.05 0.00 0.06 0.00 0.00
8.33 208 0.10 0.09 0.00 0.09 0.08 0.14 0.00 0.00
8.50 212 0.11 0.10 0.00 0.10 0.04 0.10 0.00 0.00
8.67 216 0.19 0.17 0.00 0.17 0.12 0.16 0.04 0.00
8.83 220 0.20 0.18 0.00 0.19 0.13 0.07 0.04 0.00
9.00 224 0.18 0.15 0.00 0.15 0.09 0.23 0.08 0.00
9.17 228 0.16 0.15 0.00 0.16 0.08 0.14 0.03 0.00
9.33 232 0.18 0.16 0.00 0.16 0.12 0.21 0.06 0.00
9.50 236 0.25 0.24 0.00 0.24 0.16 0.21 0.10 0.00
9.67 240 0.29 0.26 0.01 0.28 0.19 0.25 0.13 0.00
9.83 244 0.34 0.30 0.00 0.31 0.23 0.31 0.17 0.00
10.00 248 0.29 0.26 0.00 0.26 0.17 0.24 0.09 0.00
10.17 252 0.30 0.28 0.00 0.28 0.19 0.27 0.12 0.00
10.33 256 0.33 0.28 0.00 0.29 0.20 0.31 0.14 0.00
10.50 260 0.38 0.35 0.00 0.34 0.23 0.33 0.16 0.00
10.67 264 0.44 0.40 0.00 0.41 0.28 0.38 0.20 0.00
10.83 268 0.47 0.41 0.00 0.42 0.32 0.42 0.23 0.01
11.00 272 0.46 0.38 0.00 0.41 0.27 . 0.38 0.19 0.06
11.17 276 0.48 0.43 0.00 0.43 0.28 0.40 0.19 0.04
11.33 280 0.51 0.46 0.00 0.44 0.34 0.47 0.24 0.07
11.50 284 0.51 0.47 0.00 0.44 0.30 0.41 0.19 0.04
11.67 288 0.51 0.46 0.00 0.43 0.25 0.37 0.16 0.00
11.83 292 0.60 0.54 0.00 0.51 0.37 0.51 0.27 0.06
12.00 296 0.56 0.51 0.00 0.42 0.29 0.44 0.18 0.01
12.17 300 0.62 0.56 0.00 0.49 0.33 0.48 0.22 0.00
12.33 304 0.61 0.56 0.00 0.48 0.35 0.51 0.23 0.01
12.50 308 0.66 0.59 0.00 0.50 0.34 0.52 0.25 0.00
12.67 312 0.72 0.65 0.00 0.52 0.38 0.55 0.27 0.03
12.83 316 0.76 0.71 0.00 0.56 0.44 0.61 0.29 0.06
13.00 320 0.75 0.57 0.00 0.47 0.33 0.55 0.22 0.00
13.17 324 0.75 0.76 0.00 0.48 0.40 0.57 0.25 0.00
13.33 328 0.77 0.73 0.00 0.49 0.39 0.57 0.27 0.00
13.50 332 0.80 0.74 0.00 0.49 0.40 0.58 0.28 0.00
13.67 336 0.88 0.82 0.00 0.56 0.48 0.66 0.35 0.00
13.83 340 0.91 0.83 0.00 0.57 0.50 0.68 0.37 0.02
14.00 344 0.85 0.81 0.00 0.50 0.42 0.61 0.32 0.06
14.17 348 0.83 0.78 0.00 0.49 0.42 0.58 0.29 0.00
14.33 352 0.83 0.79 0.00 0.50 0.45 0.64 0.34 0.07
14.50 356 0.87 0.81 0.00 0.51 0.44 0.62 0.32 0.05

 

99

 

Table D.6 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

14.67 360 0.92 0.88 0.01 0.59 0.53 0.64 0.40 0.15
14.83 364 0.91 0.87 0.00 0.56 0.54 0.66 0.41 0.14
15.00 368 0.83 0.78 0.00 0.52 0.44 0.58 0.33 0.07
15.17 372 0.76 0.75 0.00 0.48 0.42 0.50 0.28 0.04
15.33 376 0.77 0.74 0.00 0.49 0.48 0.55 0.32 0.08
15.50 380 0.72 0.68 0.00 0.46 0.42 0.47 0.27 0.05
15.67 384 0.77 0.75 0.00 0.53 0.52 0.51 0.33 0.13
15.83 388 0.77 0.65 0.00 0.53 0.51 0.48 0.32 0.13
16.00 392 0.61 0.57 0.00 0.38 0.38 0.32 0.18 0.03
16.17 396 0.61 0.56 0.00 0.40 0.40 0.30 0.17 0.00
16.33 400 0.59 0.53 0.00 0.37 0.38 0.26 0.15 0.00
16.50 404 0.56 0.50 0.00 0.36 0.37 0.22 0.10 0.00
16.67 408 0.64 0.58 0.00 0.45 0.47 0.32 0.19 0.04
16.83 412 0.64 0.58 0.00 0.43 0.45 0.29 0.17 0.10
17.00 416 0.49 0.47 0.00 0.34 0.33 0.16 0.04 0.02
17.17 420 0.48 0.50 0.00 0.38 0.36 0.18 0.02 0.00
17.33 424 0.41 0.49 0.00 0.37 0.38 0.23 0.11 0.00
17.50 428 0.31 0.51 0.00 0.40 0.38 0.23 0.09 0.00
17.67 432 0.34 0.63 0.00 0.50 0.49 0.34 0.19 0.15
17.83 436 0.27 0.59 0.00 0.49 0.46 0.33 0.16 0.16
18.00 440 0.09 0.43 0.00 0.39 0.34 0.20 0.06 0.04
18.17 444 0.03 0.33 0.00 0.36 0.26 0.16 0.00 0.00
18.33 448 0.00 0.18 0.00 0.34 0.26 0.21 0.01 0.00
18.50 452 0.00 0.07 0.00 0.29 0.19 0.13 0.00 0.00
18.67 456 0.00 0.12 0.00 0.40 0.29 0.22 0.00 0.00
18.83 460 0.00 0.05 0.00 0.40 0.27 0.22 0.02 0.00
19.00 464 0.00 0.04 0.00 0.36 0.21 0.20 0.00 0.00
19.17 468 0.00 0.02 0.00 0.42 0.26 0.25 0.04 0.00
19.33 472 0.00 0.02 0.00 0.43 0.30 0.31 0.08 0.00
19.50 476 0.00 0.00 0.00 0.42 0.26 0.26 0.05 0.00
19.67 480 0.00 0.00 0.00 0.44 0.27 0.28 0.06 0.00
19.83 484 0.00 0.00 0.00 0.43 0.24 0.30 0.05 0.00
20.00 488 0.00 0.00 0.00 0.37 0.21 0.24 0.04 0.00
20.17 492 0.00 0.00 0.00 0.39 0.20 0.25 0.02 0.00
20.33 496 0.00 0.00 0.00 0.35 0.19 0.24 0.00 0.00
20.50 500 0.00 0.00 0.00 0.32 0.18 0.24 0.00 0.00
20.67 504 0.00 0.00 0.00 0.24 0.21 0.22 0.07 0.00
20.83 508 0.00 0.00 0.00 0.17 0.11 0.21 0.00 0.00
21.00 512 0.00 0.00 0.00 0.19 0.24 0.26 0.00 0.00
21.17 516 0.00 0.00 0.00 0.18 0.27 0.25 0.05 0.00
21.33 520 0.00 0.00 0.00 0.19 0.31 0.24 0.04 0.00
21 .50 524 0.00 0.05 0.00 0.18 0.33 0.19 0.18 0.00
21.67 528 0.00 0.01 0.00 0.03 0.29 0.10 0.10 0.00
21.83 532 0.00 0.00 0.03 0.20 0.32 0.10 0.11 0.00
22.00 536 0.00 0.00 0.04 0.00 0.22 0.02 0.04 0.00
22.17 540 0.00 0.00 0.00 0.10 0.16 0.00 0.00 0.00
22.33 544 0.00 0.00 0.00 0.01 0.25 0.00 0.00 0.00

100

 

Table 0.6 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

22.50 548 0.00 0.00 0.00 0.00 0.23 0.00 0.00 0.00
22.67 552 0.00 0.00 0.00 0.02 0.30 0.00 0.12 0.00
22.83 556 0.00 0.00 0.00 0.02 0.33 0.00 0.12 0.00
23.00 560 0.00 0.00 0.00 0.00 0.23 0.00 0.02 0.00
23.17 564 0.00 0.00 0.00 0.00 0.22 0.00 0.01 0.00
23.33 568 0.00 0.00 0.00 0.00 0.28 0.00 0.04 0.00
23.50 572 0.00 0.00 0.00 0.00 0.30 0.00 0.07 0.00
23.67 576 0.00 0.00 0.00 0.00 0.31 0.00 0.12 0.00
23.83 580 0.00 0.00 0.00 0.03 0.31 0.00 0.09 0.00
24.00 584 0.00 0.00 0.00 0.00 0.25 0.00 0.05 0.00
24.17 588 0.00 0.00 0.00 0.00 0.27 0.00 0.06 0.00
24.33 592 0.00 0.01 0.00 0.00 0.33 0.00 0.14 0.00
24.50 596 0.00 0.00 0.00 0.00 0.25 0.00 0.08 0.00
24.67 600 0.06 0.12 0.07 0.16 0.45 0.07 0.35 0.09
24.83 604 0.00 0.03 0.11 0.00 0.27 0.00 0.17 0.11
25.00 608 0.00 0.00 0.03 0.00 0.13 0.00 0.09 0.02
25.17 612 0.00 0.00 0.02 0.00 0.09 0.00 0.11 0.02
25.33 616 0.00 0.00 0.03 0.00 0.11 0.00 0.12 0.04
25.50 620 0.00 0.00 0.02 0.00 0.08 0.00 0.12 0.03
25.67 624 0.00 0.00 0.08 0.00 0.13 0.00 0.19 0.10
25.83 628 0.00 0.00 0.08 0.00 0.09 0.00 0.19 0.07
26.00 632 0.00 0.00 0.04 0.00 0.05 0.00 0.14 0.04
26.17 636 0.00 0.00 0.02 0.00 0.02 0.00 0.12 0.02
26.33 640 0.00 0.00 0.03 0.00 0.05 0.00 0.15 0.04
26.50 644 0.00 0.00 0.00 0.00 0.00 0.00 0.11 0.01
26.67 648 0.00 0.00 0.02 0.00 0.00 0.00 0.10 0.02
26.83 652 0.00 0.00 0.00 0.00 0.00 0.00 0.02 0.00
27.00 656 0.00 0.00 0.00 0.00 0.00 0.00 0.01 0.00
27.17 660 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
27.33 664 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
27.50 668 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
27.67 672 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
27.83 676 0.00 0.00 0.00 0.00 0.00 0.00 0.01 0.00
28.00 680 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
28.17 684 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
28.33 688 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
28.50 692 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
28.67 696 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
28.83 700 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
29.00 704 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
29.17 708 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
29.33 712 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
29.50 716 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
29.67 720 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
29.83 724 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
30.00 728 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
30.17 732 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

 

101

 

Table 0.6 continued

 

 

 

 

30.33 736 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
30.50 740 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
30.67 743 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

 

 

 

 

 

 

 

 

 

 

102

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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333 s. 2.3 3.: 2.3.: 3.2. 3.5.; 2.3.5.... 2.3.; “MM.” 3.33

 

 

 

 

 

 

 

 

 

 

3.5 330 02.33.50

 

 

 

 

330 303.3830 0 330 "San. 33m 33232331 30 203...

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003—5:00 5.0 050...

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0035.000 5.0 030.3

105

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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00:35:00 5.0 0.00...

106

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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3333338 ..3 2333

107

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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3333338 .3 333.

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50.0 3.0 00003 3 00.5V0 00.003 3 050003 00.00 05.000 00.3003 00. 3V0 V00 00.V0
50.0 3.0 03.3033 0V.5V0 50.0V33 300003 00.00 05.500 00.3303 00.000 000 00.00
50.0 3.0 50.000 3 50.5V0 35.0033 V0000 3 0V.00 0V.000 55.0003 05 .500 030 50.00
50.0 3.0 000003 00 .0V0 00.03 33 00.5003 03.00 0 3 .000 00.0003 00.000 030 00.00
50.0 3.0 00.5003 00.0V0 00.003 3 050003 00.00 00.000 00.3003 00.000 000 00.00
50.0 3.0 V3 .0003 00.0V0 00.0003 5 3.0003 00.00 00.000 50.0503 03. 300 V00 5300
50.0 3.0 0 3 .000 3 0V.VVO 00.050 3 00 .000 3 00.00 00.500 50.0003 30.000 000 00.00
50.0 3.0 0 3 .V003 00.0V0 00.0003 00.V003 50.00 0 3 .000 05.V003 30.000 005 00.00
50.0 3.0 00.000 3 00.000 0V.0V0 3 V0.V00 3 00.00 00.000 50.0V03 00 .000 005 50.00
50.0 3.0 V0. 3003 30.000 00.0003 00.0003 00.00 05.000 5V.5003 00.000 005 00.00
50.0 3.0 00.0003 00. 300 050003 VV.0003 00.00 0 3 .0V0 00.0003 00.030 V05 00.00
50.0 3.0 000003 0 3 .000 03.3303 00.3003 00.00 V0.5V0 05.0003 0V0 30 005 53.00
50.5 3.0 050003 00.000 00.000 00 .0003 00.00 00.0V0 00.0 303 30.030 055 00.00
50.5 3.0 30.5003 03 .30 03.500 50.0503 00.00 30.0V0 000003 00030 055 00. 30
50.5 3.0 50.000 3 00.500 30.050 00.550 3 00 .00 V0 .0V0 00.0003 00 .500 005 50. 30
50.5 3.0 000003 V3. 300 50.000 V3 .0503 00.00 30.0V0 3V.003 3 V0000 V05 00. 30
50.5 3.0 00.V00 3 00.V00 00.000 50.V50 3 00.00 V5000 00.00 3 3 00 .000 005 00. 30
50.5 3.0 53.V003 00.000 00. 3V0 V0.0503 00.00 30.500 30.V03 3 00. 300 005 53. 30
50.0 3.0 00.0003 00.000 V5000 00.3503 00.00 V0000 00.053 3 00.005 005 00. 30
50.0 3.0 00.000 3 00 .050 50 .000 00.050 3 00.00 3V.V00 3V.05 3 3 00.505 0V5 00.00
50.030 0V. 3003 00.050 00.000 03.0003 00.00 00 .000 000033 05.V05 VV5 50.00
50.0 3.0 50.000 3 00.000 00.000 30.500 3 00.00 00. 300 00.003 3 00.005 0V5 00.00
50.020 V0.0503 55.500 30.000 0V.000 3 00.00 00.000 00.00 3 3 00. 305 005 00.00
50.0 3.0 00.0503 05. 300 00. 300 V0.0003 00.00 V0000 00.003 3 05.005 005 53.00
50.0 3.0 00.050 3 V0.0V0 00.050 00.000 3 00.00 30.500 3V.00 3 3 00.005 005 00.00

 

 

 

 

 

 

 

 

 

 

 

 

33:03.00 5.0 030...

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50. 30.0 00.0V33 5V.000 30.3003 30.VOV3 00.00 VV.0533 V0.0003 00. 3V03 050 53.0V
50. 30.0 00.0V3 3 5V.000 33.0003 00.VOV3 00.00 05003 3 35.V003 00.0003 000 00.0V
50. 30.0 30.0V33 0V.000 00.0V03 03.VOV3 00.00 0V.0033 00.V003 00.0003 V00 00.00
50.30.0 00.03 3 3 3.000 0 3 .5V03 00.00V3 00.00 V0.0V3 3 0 3 .0003 00.V003 000 50.00
50.30.0 00.5V33 00.V00 00.0V03 03.00V3 00.00 35.V033 00.0003 V0.0303 000 00.00
50.30.0 V0.5V33 V0.V00 V0.VV03 00.00V3 00.00 03.0033 05.3003 00.0303 000 00.00
50.30.0 V3.5V33 50.V00 05.0V03 00.00V3 00.00 00.5333 00.0003 V0.0003 0V0 53.00
50. 30.0 05.03 3 50.V00 50. 3V03 00.00V3 00.00 00.003 3 00.0003 0V.0003 VVO 00.00
50.30.0 03.0V3 3 0V.V00 05.0003 VV. 30V3 00.00 00.3033 00.0003 0 3 .V00 0V0 00.00
50. 30.0 00.0V33 V0000 30.5003 50.00V3 00.00 V3.0003 V3.0003 05.500 000 50.00
50. 30.0 00.333 3 00.000 00.0003 00.000 3 00.00 00.0003 05.000 3 33.300 000 00.00
50. 30.0 00.0V33 00.000 0V.V003 50.0003 00.00 00.0503 00.0003 00.050 000 00.00
50.30.0 30.0V33 00.000 55.0003 V3.0003 00.00 00.3503 03.V003 00.000 V00 5300
50. 30.0 00.0V33 55.000 00.3003 000003 00.00 00.V003 000003 33.000 000 00.00
50. 30.0 00. 3V33 00.000 00.0003 0V.000 3 00.00 00.0003 53.3003 03.500 030 00.50
50. 30.0 00.0V3 3 V3000 00.0003 05.5003 00.00 V0.0003 00.0503 05.000 030 50.50
50. 30.0 00.5033 V3000 30.0003 00.5003 00.00 03.0Vo3 00.0503 5V.VVO 000 00.50
50. 30.0 0V.00 33 V3 .000 00.0003 00.500 3 00.00 00. 3V03 00.0503 00.000 V00 00.50
50.30.0 03.0033 V3000 30.0003 00.0003 00.00 03.0003 00.0003 50.000 000 53.50
50.30.0 V0.0033 V3000 00.0003 000003 00.00 00.3003 050003 30000 000 00.50
50. 30.0 000033 V3000 00.3003 030003 00.00 05.0003 00.0V03 00.000 000 00.00
50. 30.0 00.003 3 V3 .000 0 3 .0003 00.000 3 00.00 00.000 3 0V.000 3 00.0 30 000 50.00
50.30.0 00.V033 V3000 30.0303 000003 00.00 30.0303 33.5303 V5.500 V00 00.00
50. 30.0 VV.0033 V3000 00.0303 000003 00.00 05.32 0V.0003 00.300 000 00.00
50.30.0 00.0033 00.000 00.5303 500003 00.00 00.3303 00.00V3 05.000 050 53.00
50. 30.0 500033 00. 300 00.0303 000003 00.00 00.5003 00.V5V3 00.000 050 00.00
50. 30.0 0003 33 00. 300 000303 00.V003 3V.00 0V.0003 00.00V3 00.000 000 00.00
50.30.0 03.0333 00.000 00.V303 000003 50.00 00.000 30.0VV3 05.050 V00 50.00
50.30.0 00.V333 03.000 30.0303 000003 03.00 30.000 50.00V3 33.350 000 00.00
50.30.0 00.0333 55.0V0 030303 500003 00.00 V0300 00.03V3 53.000 000 00.00
50.30.0 00.3333 00.0V0 00.0303 030003 00.30 V0000 50.00V3 55.300 000 53.00

 

 

 

 

 

 

 

 

 

 

 

 

00:35:00 5.0 030...

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50.30.0 00.0033 00.500 3V.0003 V3.03V3 00.00 00. 3V03 00.0303 0V.5003 0003 00.0V
50.30.0 0V.0033 V0.500 00. 3003 00.03V3 00.00 00.0003 30.0303 50.3003 0003 53.0V
50.30.0 00.0033 55.000 00.3003 00.03V3 00.00 V0.0003 5V.3303 500033 0003 00.0V
50.30.0 00.0033 0V.000 V0.0003 00.V3V3 00.00 00.0303 00.0303 V0.0033 V003 00.VV
50.30.0 050033 30.000 00.0503 03.V3V3 00.00 00.00V3 00.0303 V0.V033 0003 50.V
50.30.0 3 3.003 3 30.000 00.0503 0V0 3V3 00.00 00.00V3 V0.0003 V0053 3 0503 00.VV
50.30.0 05.5033 30.000 00.0503 00.03V3 00.00 00.05V3 00.0003 000533 0503 00.VV
50.30.0 00.5033 30.000 0V.0503 00.03V3 00.00 50.VOV3 0V.0003 000033 0003 53.VV
50.30.0 50.0033 30.000 00.0503 00.03V3 00.00 50.30V3 V0.5003 00.0033 V003 00.VV
50.30.0 30.0033 30.000 00.5503 V5.33V3 00.00 00.50V3 3V.5003 05.5033 0003 00.0V
50.30.0 00.0033 30.000 30.0503 00.33V3 00.00 00.00V3 00.0003 500033 0003 50.0V
50.30.0 00.00 33 30.000 05.0503 3V.0 3V3 00.00 00.00V3 000003 00.03 3 0003 00.0V
50.30.0 50.V033 30.000 V0.0503 3V.03V3 00.00 03.0003 0V.0003 00. 3V33 0V03 00.0V
50.30.0 05.V033 30.000 00.0503 V0.03V3 00.00 0V.0003 00.0003 3V.5033 VVo3 53.0V
50.30.0 00.V033 30.000 00.0503 00.03V3 00.00 00.0003 00.V003 0V.0033 0V03 00.0V
50.30.0 00.V03 3 30.000 V0.0503 00.00V3 00.00 00.V003 00.V003 3.503 3 0003 00.0V
50. 30.0 00.V033 30.000 55.V503 00.00V3 00.00 00.0V03 30.V003 000033 0003 50.0V
50. 30.0 5V.V03 3 30.000 55.0503 00.00V3 00.00 00.5003 00.0003 00.53 33 0003 00.0V
50.30.0 5V.V033 30.000 30.0503 53.00V3 00.00 V5.0303 000003 300333 V003 00.0V
50.30.0 03.V033 30.000 0V. 3503 55.00V3 00.00 00.0003 00.0003 00.5033 0003 53.0V
50.30.0 00.0033 30.000 00.0003 V0.00V3 00.00 00. 3003 0V.0003 030033 0303 00.0V
50.30.0 00.0033 00.000 00.0003 3V.00V3 00.00 00.0503 30.3003 000003 0303 00. 3V
50.30.0 03.0033 V5000 0V.0003 00.50V3 00.00 35.5003 03.3003 00. 3003 0003 50. 3V
50.30.0 00.003 3 30000 00.V003 00.50V3 00.00 3 3.0003 0V.0003 00.0003 V003 00. 3V
50.30.0 V0.0033 30.000 V0.0003 00.00V3 00.00 50.VV03 05.0003 V0.0003 0003 00. 3V
50.30.0 50.3033 5V.000 03.3003 00.00V3 00.00 00.0003 50.0003 00.0503 000 53. 3V
50. 30.0 0V. 303 3 5V.000 VV.0003 00.00V3 00.00 3 3.0003 00.0003 05.0003 000 00. 3V
50.30.0 03.3033 5V.000 V0.5003 00.00V3 00.00 00.0303 00.5003 03.V003 000 00.0V
50. 30.0 00.00 3 3 5V.000 00.0003 VV.00V3 00.00 30.0003 53.5003 0V.0003 V00 50.0V
50. 30.0 V0003 3 5V.000 0V.V003 00.00V 3 00.00 05.303 3 3V.0003 00.0003 000 00.0V
50.30.0 V3.0033 5V.000 03.0003 03.00V3 00.00 50.0033 30.0003 00.5V03 050 00.0V

 

 

 

 

 

 

 

 

 

 

 

 

3333338 ..3 233.

111

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

50. 30.0 00.0533 00.000 00.0003 00.00V3 00.00 V0.0353 00.0003 5V.03V3 0003 00.00
50.30.0 30.053 3 00.000 00.0003 00.00V3 00.00 00.5353 00.0003 05.03V3 0303 00.00
50.30.0 00.003 3 V5000 00.0003 V3.50V3 00.00 00.5353 05.5003 00.00V3 0303 53.00
50. 30.0 00.003 3 00.000 00.0003 00.00V3 00.00 V5.0353 00.5003 500003 0003 00.00
50. 30.0 00.0033 00.300 03.0003 05.VOV3 00.00 50.0353 00.5003 50.0003 V003 00.0V
50. 30.0 03.0033 00. 300 05.0003 00 .00V3 00.00 00.0353 0V.0003 3V.0003 0003 50.0V
50. 30.0 50.003 3 55.000 00 .0003 00. 30V3 00.00 00.0 353 500003 5V.0503 0033 00.0V
50. 30.0 0V.003 3 00.000 00.0003 30. 30V3 00.00 00.0 353 0V.0003 0 3 .000 3 003 3 00.0V
50.30.0 00.0033 00.000 03.0003 03.00V3 00.00 00.3353 00.V003 00.0003 0033 53.0V
50. 30.0 30.003 3 V3 .000 0 3.0003 50.00V3 00.00 00.0053 VV.V003 30.000 3 V033 00.0V
50. 30.0 50.003 3 V3 .000 0 3 .0003 3500V3 00.00 0V.5053 30.0003 00.0V03 003 3 00.0V
50. 30.0 0V.503 3 00.000 00.0003 00.50V3 00.00 00.0053 000003 30000 3 0533 50.0V
50. 30.0 00.0033 00.000 V0.0003 VV.00V3 00.00 05.0003 00. 3003 V0.0003 0533 00.0V
50. 30.0 00.0033 00.000 V0.0003 00.00V3 00.00 30.0003 03.3003 V5.0003 0033 00.0V
50.30.0 35.003 3 00.000 03.0003 V0.00V3 00.00 V5.0003 00.0003 00.0303 V03 3 530V
50. 30.0 00.003 3 00.000 03.0003 50.VOV3 00.00 030003 00.0 303 00.0003 003 3 00.0V
50. 30.0 00.003 3 00.000 0 3 .0003 VV.VOV3 00.00 00.0503 0V0 303 00.000 3 00 3 3 00.5V
50. 30.0 0V.003 3 00.000 03.0003 30.00V3 00.00 000503 00.0 303 000003 003 3 50.5V
50.30.0 00.003 3 00.000 0 3 .0003 30.00V3 00.00 00.0003 00.0303 30.0003 0V3 3 00.5V
50.30.0 00.003 3 00.000 00.0003 00.00V3 00.00 03.0003 03.0303 50.0003 VV3 3 00.5V
50.30.0 00.0033 0V.000 00.5003 50.00V3 00.00 00. 3003 00.5303 03.0503 0V33 53.5V
50.30.0 3 3.003 3 00.000 00.0003 00. 30V3 00.V0 30.0V03 50.0303 00.0003 003 3 00.5V
50.30.0 30.V03 3 50.000 0V.0003 50. 30V3 V0.V0 03.0003 00.0303 000003 0033 00.0V
50.30.0 00.003 3 V0.500 00.0003 00.00V3 00.00 00.0003 05.0303 030003 0033 50.0V
50.30.0 03.0033 00.500 03.0003 00.03V3 00.00 00.V303 03.0303 00.0V03 V033 00.0V
50.30.0 V0.0033 00.500 00.V003 V0.03V3 00.00 00.V003 05.V303 00.0V03 0033 00.0V
50.30.0 03 003 3 50.500 0V.V003 0V0 3V3 00.00 00.V003 5V.V303 05.0003 03 33 5 3 .0V
50.30.0 030033 00.500 30.V003 00.53V3 00.00 00.0003 33.V303 00.0003 0333 00.0V
50.30.0 50.303 3 00.500 000003 00.5 3V3 00.00 30.0503 05.0303 00.V003 003 3 00.0V
50.30.0 00.303 3 0V.500 00.0003 00.53V3 00.00 00.0003 0V.0303 V0.0303 V033 50.0V
50.30.0 00.3033 30.500 00.0003 05.03V3 00.00 00.3003 00.0303 330303 0033 00.0V

 

 

 

 

 

 

 

 

 

 

 

 

33333333 ..3 333.

112

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

50. 30.0 000533 00.000 00.0003 00.50V3 0V.033 50.0053 00.0003 00. 3VV3 0003 50.00
50. 30.0 00.0533 0V.000 00.0003 00.50V3 00.003 00.0053 33.0003 00.0VV3 0003 00.00
50. 30.0 000533 0V.000 00.0003 00.50V3 0V.003 50.0053 00.0003 00.0VV3 0003 00.00
50.30.0 00 .0533 0V.000 00. 000 3 00.50V3 05.503 50.0053 00.0003 00.0VV3 V003 5 3 .00
50. 30.0 000533 00.000 00.0003 00.50V3 00.503 00.0053 00.0003 00.0VV3 0003 00.00
50.30.0 00.0533 00.000 00.0003 00.00V3 00.003 00.0053 05.0003 05.0VV3 0503 00.00
50. 30.0 000533 00. 300 000003 0V.00V3 50.V03 00.0053 00.0003 00.0VV3 0503 50.00
50. 30.0 000533 00.050 00. 3003 00.00V3 00.003 00.V053 30.3003 V0.00V3 0003 00.00
50. 30.0 0V.0533 00.050 00. 3003 00.VOV3 00003 00.V053 00. 3003 00.00V3 V003 00.00
50.30.0 00.0533 05.050 00. 3003 V5. 30V3 00.303 00.0053 00. 3003 05.00V3 0003 53.00
50.30.0 00.0533 00.050 00. 3003 V0.00V3 V0.303 00.0053 30.3003 00.00V3 0003 00.00
50.30.0 030533 00.050 05. 3003 03.00V3 50.003 00.0053 05.0003 V0.00V3 0003 00.30
50.30.0 00. 3533 00. 350 00. 3003 0V.00V3 35.00 30.0053 V0.0003 00.00V3 0V03 50.30
50.30.0 0V. 3533 V0050 30.3003 V0. 30V3 V0.00 00. 3053 00.0003 05.00V3 VV03 00. 30
50.30.0 0V. 3533 00.000 30.3003 00.0VV3 00.00 00.3053 00.0003 03.00V3 0V03 00. 30
50.30.0 00.3533 55.500 5V. 3003 03.5VV3 00.00 V0.0053 00.0003 00.00V3 0003 53.30
50.30.0 00.3533 00.000 0V. 3003 00.0VV3 VV.50 00.0053 00.0003 00.VOV3 0003 00. 30
50.30.0 50.3533 00.000 00. 3003 0V.0VV3 V0.00 55.0353 00.0003 00.00V3 0003 00.00
50.30.0 05.0533 05.V00 30.3003 00. 3VV3 00.00 03.0353 00.0003 00.00V3 V003 50.00

 

 

 

 

 

 

 

 

 

 

 

 

3333338 .3 333.

113

Table D.8 Respirometer Calculated Data: Case C Gas Production Rate

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Gas Production Rate (mL/hr‘b
Days {I121 w,s,N W,M,S,N W,M,S w,s M,S,N w,s 3,8: M

o 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

4 5.00 4.84 4.45 3.83 2.45 2.06 2.19 2.29
0.00 8 0.23 0.25 0.17 0.13 0.00 0.04 0.01 0.13
0.17 12 0.78 0.47 0.28 0.11 0.00 0.00 0.00 0.10
0.33 18 4.29 1.02 1.15 0.31 0.00 0.03 0.00 0.18
0.50 20 2.46 1.43 4.42 1.38 0.01 0.03 0.00 0.16
0.67 24 0.00 0.51 1.13 5.38 0.00 0.06 0.00 0.19
0.83 28 0.00 0.30 0.00 2.98 0.19 0.04 0.00 0.16
1.00 32 0.00 0.31 0.00 0.01 0.08 0.00 0.00 0.10
1.17 36 0.00 0.35 0.00 0.00 0.00 0.00 0.00 0.09
1.33 40 0.00 0.47 0.00 0.00 0.00 0.00 0.00 0.18
1.50 44 0.00 0.54 0.00 0.00 0.00 0.00 0.00 0.20
1.67 48 0.00 0.84 0.00 0.00 0.00 0.00 0.00 0.25
1.83 52 0.00 0.66 0.00 0.00 0.00 0.00 0.00 0.30
2.00 58 0.00 0.58 0.01 0.00 0.00 0.04 0.00 0.28
2.17 80 0.00 0.62 0.00 0.00 0.00 0.03 0.00 0.28
2.33 84 0.00 0.70 0.00 0.00 0.00 0.10 0.00 0.35
2.50 88 0.02 0.64 0.00 0.00 0.00 0.05 0.00 0.30
2.87 72 0.16 0.65 0.00 0.00 0.00 0.02 0.00 0.31
2.83 78 0.15 0.62 0.00 0.00 0.25 0.07 0.00 0.34
3.00 80 0.03 0.55 0.00 0.00 0.17 0.04 0.02 0.32
3.17 84 0.17 0.61 0.10 0.00 0.26 0.11 0.14 0.38
3.33 88 0.17 0.66 0.19 0.00 0.32 0.21 0.12 0.44
3.50 92 0.09 0.58 0.16 0.01 0.30 0.15 0.07 0.39
3.67 98 0.12 0.53 0.21 0.02 0.35 0.15 0.04 0.39
3.83 100 0.10 0.50 0.22 0.00 0.37 0.20 0.11 0.48
4.00 104 0.09 0.45 0.22 0.00 0.31 0.20 0.08 0.46
4.17 108 0.15 0.49 0.28 0.00 0.36 0.26 0.13 0.51
4.33 112 0.15 0.49 0.31 0.00 0.37 0.31 0.14 0.56
4.50 118 0.14 0.47 0.30 0.00 0.34 0.30 0.13 0.56
4.87 120 0.24 0.52 0.44 0.00 0.49 0.37 0.22 0.68
4.83 124 0.19 0.50 0.48 0.00 0.47 0.34 0.19 0.71
5.00 128 0.23 0.52 0.42 0.00 0.51 0.37 0.19 0.75
5.17 132 0.32 0.53 0.49 0.00 0.59 0.42 0.23 0.87
5.33 136 0.34 0.51 0.49 0.00 0.62 0.43 0.27 0.93
5.50 140 0.41 ' 0.59 0.57 0.00 0.73 0.51 0.32 1.06
5.67 144 0.44 0.59 0.58 0.00 0.81 0.55 0.34 1.17
5.83 148 0.45 0.71 0.67 0.00 0.98 0.88 0.36 1.36
6.00 152 0.39 0.67 0.85 0.22 1.02 0.65 0.31 1.49
8.17 156 0.45 0.74 0.66 0.30 1.12 0.73 0.84 1.84
6.33 160 0.49 0.84 0.72 0.43 1.21 0.84 0.36 1.83
6.50 184 0.57 0.95 0.79 0.61 1.32 0.91 0.38 2.04
8.87 188 0.71 1.19 0.95 0.80 1.52 1.05 0.48 2.37
8.83 172 0.80 1.30 1.07 0.81 1.82 1.14 0.53 2.87

114

Table D.8 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

7.00 176 0.68 1.31 1.00 0.45 1.63 1.08 0.45 2.80
7.17 180 0.85 1.53 1.26 0.19 1.93 1.30 0.58 3.19
7.33 184 0.93 1.69 1.37 0.02 2.10 1.41 0.62 3.50
7.50 188 1.06 1.83 1.54 0.04 2.25 1.50 0.66 3.82
7.67 192 1.24 2.14 1.90 0.00 2.57 1.73 0.84 4.25
7.83 196 1.40 2.40 2.14 0.00 2.75 1.87 0.93 4.63
8.00 200 1.39 2.50 2.25 0.01 2.83 1.87 0.89 4.84
8.17 204 1.64 2.80 2.60 0.00 3.14 2.05 1.01 5.21
8.33 208 1.84 3.11 2.96 0.00 3.41 2.24 1.11 5.56
8.50 212 1.92 3.32 3.22 0.00 3.52 2.25 1.12 5.71
8.67 216 2.03 3.45 3.50 0.00 3.65 2.29 1.16 5.81
8.83 220 2.31 3.80 3.98 0.00 3.89 2.49 1.30 5.97
9.00 224 2.43 3.96 4.23 0.00 3.94 2.46 1.33 5.93
9.17 228 2.65 4.20 4.55 0.00 4.06 2.49 1.42 5.83
9.33 232 2.88 4.43 4.90 0.00 4.19 2.53 1.50 5.65
9.50 236 3.07 4.59 5.11 0.00 4.23 2.50 1.56 5.35
9.67 240 3.42 4.83 5.46 0.00 4.42 2.54 1.74 5.01
9.83 244 3.67 5.09 5.51 0.00 4.51 2.53 1.82 4.61
10.00 248 3.80 5.08 5.35 0.00 4.45 2.43 1.80 3.94
10.17 252 3.87 5.10 5.12 0.00 4.47 2.27 1.87 3.45
10.33 256 3.97 5.06 4.73 0.00 4.58 2.17 1.90 2.95
10.50 260 3.94 4.91 4.18 0.00 4.55 1.97 1.90 2.55
10.67 264 4.02 4.87 3.58 0.01 4.66 1.90 2.01 2.42
10.83 268 3.95 4.61 2.75 0.00 4.58 1.83 2.04 2.35
11.00 272 3.67 4.16 1.64 0.00 4.33 1.54 1.91 2.10
11.17 276 3.49 3.68 0.66 0.00 4.13 1.40 1.89 2.00
11.33 280 3.19 3.25 0.27 0.00 4.04 1.36 1.89 2.01
11.50 284 2.88 2.72 0.19 0.00 3.85 1.29 1.81 1.95
11.67 288 2.64 2.37 0.20 0.13 3.90 1.34 1.76 1.96
11.83 292 2.13 1.85 0.23 0.25 3.84 1.46 1.83 2.01
12.00 296 1.52 1.40 0.21 0.15 3.62 1.44 1.71 1.87
12.17 300 0.94 1.26 0.28 0.10 3.50 1.58 1.72 1.89
12.33 304 0.29 1.23 0.30 0.09 3.32 1.74 1.76 1.86
12.50 308 0.15 1.27 0.37 0.09 3.08 1.83 1.84 1.89
12.67 312 0.19 1.35 0.50 0.10 2.94 2.08 2.05 2.01
12.83 316 0.16 1.42 0.56 0.22 2.81 2.20 2.14 1.96
13.00 320 0.00 1.33 0.48 0.05 2.46 2.11 2.09 1.89
13.17 324 0.00 1.50 0.60 0.06 2.39 2.18 2.25 1.95
13.33 328 0.00 1.66 0.70 0.05 2.33 2.25 2.30 2.00
13.50 332 0.00 1.90 0.87 0.06 2.29 2.28 2.37 2.12
13.67 336 0.01 2.19 1.05 0.08 2.27 2.33 2.44 2.25
13.83 340 0.09 2.46 1.19 0.18 2.18 2.36 2.48 2.30
14.00 344 0.07 2.67 1.26 0.11 1.92 2.29 2.45 2.14
14.17 348 0.06 2.85 1.37 0.10 1.86 2.29 2.48 1.91
14.33 352 0.08 3.07 1.51 0.10 1.77 2.31 2.48 1.77
14.50 356 0.08 3.19 1.61 0.09 1.64 2.25 2.46 1.63
14.67 360 0.09 3.25 1.73 0.03 1.55 2.16 2.45 1.53
14.83 364 0.20 3.44 2.02 0.00 1.69 2.35 2.53 1.61

 

 

 

 

 

 

 

 

 

115

 

Table 0.8 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

15.00 368 0.10 3.35 2.04 0.02 1.54 2.17 2.22 1.46
15.17 372 0.08 3.29 2.18 0.07 1.52 2.17 2.04 1.47
15.33 376 0.13 3.33 2.33 0.07 1.56 2.17 1.85 1.50
15.50 380 0.10 3.32 2.44 0.06 1.55 2.10 1.54 1.49
15.67 384 0.21 3.35 2.60 0.26 1.62 2.13 1.46 1.60
15.83 388 0.26 3.47 2.70 0.15 1.63 2.13 1.29 1.65
16.00 392 0.23 3.33 2.74 0.11 1.61 2.09 1.08 1.65
16.17 396 0.26 3.25 2.76 0.09 1.61 2.04 0.92 1.66
16.33 400 0.29 3.17 2.78 0.10 1.69 2.05 0.83 1.60
16.50 404 0.34 3.14 2.86 0.10 1.71 1.98 0.76 1.33
16.67 408 0.44 3.08 2.92 0.09 1.95 2.04 0.76 1.19
16.83 412 0.51 3.01 2.97 0.08 2.20 2.01 0.78 1.11
17.00 416 0.48 2.82 2.96 0.13 2.41 1.89 0.72 1.06
17.17 420 0.49 2.67 2.86 0.16 2.68 1.75 0.66 1.06
17.33 424 0.54 2.54 2.87 0.12 2.96 1.60 0.65 1.11
17.50 428 0.56 2.36 2.80 0.09 3.00 1.49 0.63 1.15
17.67 432 0.66 2.29 2.85 0.16 2.53 1.49 0.69 1.29
17.83 436 0.73 2.13 2.81 0.16 1.64 1.38 0.69 1.37
18.00 440 0.69 1.86 2.62 0.05 0.91 1.21 0.58 1.09
18.17 444 0.76 1.75 2.57 0.11 0.66 1.15 0.57 0.81
18.33 448 0.78 1.56 2.44 0.07 0.57 1.09 0.57 0.66
18.50 452 0.80 1.42 2.36 0.09 0.58 1.04 0.55 0.58
18.67 456 0.93 1.38 2.33 0.10 0.63 1.04 0.60 0.61
18.83 460 0.95 1.32 2.25 0.09 0.63 1.01 0.62 0.68
19.00 464 0.91 1.21 2.16 0.10 0.61 0.88 0.55 0.59
19.17 468 0.90 1.12 2.32 0.15 0.59 0.74 0.52 0.57
19.33 472 0.95 1.08 2.14 0.08 0.61 0.76 0.56 0.60
19.50 476 1.00 1.03 1.82 0.05 0.61 0.64 0.52 0.58
19.67 480 1.17 1.14 1.77 0.15 0.80 0.66 0.64 0.70
19.83 484 1.18 1.10 1.59 0.13 0.83 0.63 0.62 0.72
20.00 488 1.18 1.04 1.39 0.06 0.80 0.52 0.55 0.66
20.17 492 1.24 1.00 1.24 0.06 0.84 0.49 0.57 0.70
20.33 496 1.34 1.10 1.10 0.08 1.00 0.56 0.61 0.73
20.50 500 1.34 1.06 0.91 0.05 1.04 0.51 0.59 0.73
20.67 504 1.48 1.17 0.80 0.08 1.22 0.59 0.65 0.88
20.83 508 1.61 1.29 0.72 0.14 1.39 0.66 0.73 0.96
21.00 512 1.57 1.25 0.55 0.08 1.39 0.68 0.69 0.90
21.17 516 1.67 1.34 0.48 0.09 1.55 0.75 0.72 0.98
21.33 520 1.82 1.49 0.47 0.13 1.75 0.89 0.80 1.06
21.50 524 1.89 1.69 0.46 0.13 1.85 1.00 0.82 1.13
21.67 528 1.99 1.87 0.46 0.14 2.02 1.09 0.85 1.17
21.83 532 2.00 2.00 0.40 0.10 2.10 1.32 0.74 1.21
22.00 536 2.02 2.10 0.28 0.01 2.11 1.34 0.76 1.16
22.17 540 2.07 2.19 0.25 0.00 2.27 1.47 0.80 1.18
22.33 544 2.16 2.14 0.30 0.00 2.50 1.75 0.89 1.33
22.50 548 2.27 1.76 0.32 0.00 2.62 1.73 0.92 1.35
22.67 552 2.40 1.27 0.43 0.00 2.83 1.69 1.00 1.50
22.83 556 2.49 0.78 0.44 0.00 3.02 1.42 1.09 1.59

 

 

 

 

 

 

 

 

 

116

 

Table D8 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

23.00 560 2.51 0.48 0.42 0.00 3.12 1.05 1.15 1.61
23.17 564 2.66 0.47 0.46 0.00 3.29 0.79 1.40 1.71
23.33 568 2.66 0.44 0.48 0.00 3.34 0.55 1.44 1.78
23.50 572 2.63 0.38 0.46 0.00 3.38 0.36 1.48 1.82
23.67 576 2.71 0.43 0.53 0.09 3.56 0.40 1.62 1.97
23.83 580 2.68 0.42 0.53 0.14 3.63 0.42 1.69 2.03
24.00 584 2.60 0.34 0.44 0.07 3.62 0.36 1.67 1.97
24.17 588 2.51 0.27 0.43 0.02 3.73 0.39 1.73 2.01
24.33 592 2.52 0.39 0.47 0.08 3.91 0.51 1.88 2.13
24.50 596 2.35 0.38 0.48 0.06 3.94 0.49 1.96 2.16
24.67 600 2.34 0.47 0.56 0.07 4.08 0.59 2.13 2.22
24.83 604 2.25 ' 0.51 0.63 0.07 4.23 0.70 2.32 2.24
25.00 608 1.99 0.46 0.56 0.06 4.16 0.69 2.36 2.10
25.17 612 1.93 0.47 0.66 0.23 4.35 0.83 2.58 2.07
25.33 616 1.71 0.62 0.61 0.13 4.33 0.89 2.72 1.66
25.50 620 1.58 0.56 0.62 0.09 4.34 0.80 2.78 0.98
25.67 624 1.52 0.68 0.69 0.11 4.40 0.97 2.77 0.64
25.83 628 1.30 0.66 0.63 0.05 4.05 1.00 2.65 0.39
26.00 632 0.84 0.55 0.51 0.04 3.09 0.89 2.38 0.25
26.17 636 0.69 0.63 0.60 0.04 3.20 0.91 2.30 0.27
26.33 640 0.52 0.43 0.61 0.00 3.22 0.99 2.18 0.30
26.50 644 0.44 0.53 0.62 0.00 3.14 0.90 2.03 0.26
26.67 648 0.49 0.64 0.76 0.00 3.08 0.95 2.00 0.33
26.83 652 0.41 0.57 0.79 0.00 2.66 0.97 1.94 0.38
27.00 656 0.47 0.54 0.85 0.00 1.32 0.94 1.86 0.37
27.17 660 0.44 0.69 0.89 0.00 0.74 0.96 1.83 0.38
27.33 664 0.43 0.60 0.95 0.00 0.49 0.99 1.88 0.41
27.50 668 0.44 0.69 1.01 0.00 0.32 1.02 1.89 0.38
27.67 672 0.50 0.67 1.09 0.00 0.33 1.13 1.99 0.42
27.83 676 0.49 0.70 0.88 0.00 0.36 1.25 2.05 0.44
28.00 680 0.43 0.57 0.72 0.00 0.24 1.23 1.99 0.30
28.17 684 0.41 0.49 0.64 0.00 0.25 1.33 2.02 0.27
28.33 688 0.45 0.57 0.63 0.15 0.32 1.50 2.09 0.30
28.50 692 0.31 0.49 0.49 0.05 0.24 1.49 1.94 0.16
28.67 696 0.33 0.48 0.46 0.02 0.21 1.53 1.83 0.11
28.83 700 0.28 0.55 0.41 0.01 0.22 1.63 1.74 0.11
29.00 704 0.25 0.51 0.34 0.00 0.20 1.68 1.65 0.07
29.17 708 0.25 0.56 0.34 0.00 0.22 1.84 1.58 0.09
29.33 712 0.24 0.57 0.29 0.00 0.20 1.94 1.44 0.09
29.50 716 0.27 0.62 0.26 0.00 0.22 2.01 1.48 0.00
29.67 720 0.36 0.76 0.36 0.00 0.29 2.23 1.56 . 0.22
29.83 724 0.34 0.84 0.39 0.00 0.30 2.29 1.58 0.23
30.00 728 0.45 0.85 0.35 0.00 0.36 2.29 1.54 0.18
30.17 732 0.40 0.91 0.33 0.00 0.28 2.29 1.53 0.16
30.33 736 0.38 0.95 0.34 0.00 0.36 2.31 1.51 0.16
30.50 740 0.41 1.01 0.34 0.00 0.29 2.35 1.45 0.16
30.67 744 0.46 1.15 0.39 0.00 0.38 2.48 1.61 0.23
30.83 748 0.57 1.23 0.46 0.00 0.37 2.62 1.63 0.27

 

 

 

 

 

 

 

 

 

117

 

Table 0.8 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

31.00 752 0.48 1.29 0.36 0.00 0.34 2.59 1.54 0.19
31.17 756 0.52 1.36 0.37 0.00 0.35 2.66 1.55 0.20
31.33 760 0.51 1.39 0.36 0.00 0.33 2.71 1.53 0.17
31.50 764 0.54 1.46 0.37 0.00 0.37 2.79 1.54 0.19
31.67 768 0.64 1.65 0.46 0.00 0.39 2.91 1.62 0.26
31.83 772 0.64 1.70 0.47 0.00 0.35 3.03 1.64 0.29
32.00 776 0.64 1.68 0.42 0.00 0.32 2.99 1.52 0.23
32.17 780 0.63 1.81 0.44 0.00 0.25 3.03 1.49 0.23
32.33 784 0.66 1.81 0.45 0.00 0.28 3.14 1.41 0.26
32.50 788 0.62 1.87 0.41 0.00 0.14 3.13 1.09 0.22
32.67 792 0.75 2.10 0.53 0.00 0.25 3.30 0.92 0.33
32.83 796 0.66 2.21 0.56 0.11 0.22 3.36 0.74 0.33
33.00 800 0.65 2.21 0.47 0.10 0.17 3.28 0.39 0.24
33.17 804 0.59 2.32 0.50 0.05 0.14 3.31 0.24 0.25
33.33 808 0.53 2.25 0.48 0.06 0.14 3.34 0.13 0.27
33.50 812 0.58 2.27 0.56 0.08 0.13 3.37 0.17 0.33
33.67 816 0.54 2.46 0.57 0.07 0.19 3.41 0.12 0.33
33.83 820 0.52 2.58 0.57 0.07 0.14 3.40 0.10 0.33
34.00 824 0.42 2.57 0.51 0.04 0.04 3.23 0.01 0.22
34.17 828 0.49 2.71 0.47 0.03 0.07 3.19 0.01 0.25
34.33 832 0.54 2.75 0.55 0.04 0.10 3.07 0.03 0.27
34.50 836 0.54 2.82 0.61 0.04 0.09 2.79 0.02 0.28
34.67 840 0.73 2.98 0.79 0.05 0.21 2.22 0.12 0.38
34.83 844 0.86 3.15 0.79 0.06 0.22 1.31 0.15 0.42
35.00 848 0.90 3.24 0.75 0.03 0.15 0.73 0.02 0.35
35.17 852 1.00 3.33 0.76 0.03 0.01 0.38 0.10 0.30
35.33 856 1.10 3.35 0.82 0.03 0.18 0.32 0.10 0.40
35.50 860 1.24 3.40 0.89 0.04 0.11 0.26 0.09 0.39
35.67 864 1.41 3.51 0.96 0.17 0.13 0.33 0.13 0.49
35.83 868 1.56 3.55 1.03 0.13 0.20 0.34 0.17 0.53
36.00 872 1.55 3.54 0.97 0.05 0.11 0.27 0.09 0.44
36.17 876 1.64 3.71 0.99 0.06 0.14 0.14 0.10 0.49
36.33 880 1.51 3.47 0.87 0.01 0.06 0.27 0.02 0.35
36.50 884 1.48 3.42 0.86 0.00 0.00 0.15 0.00 0.34
36.67 888 1.56 3.33 1.03 0.00 0.00 0.23 0.00 0.45
36.83 892 1.58 3.34 1.10 0.00 0.06 0.31 0.00 0.55
37.00 896 1.55 3.00 1.15 0.00 0.11 0.30 0.00 0.53
37.17 900 1.51 2.54 1.19 0.00 0.00 0.32 0.00 0.55
37.33 904 1.50 1.53 1.24 0.00 0.11 0.32 0.00 0.57
37.50 908 1.48 1.00 1.28 0.00 0.00 0.31 0.00 0.56
37.67 912 1.57 0.74 1.51 0.00 0.19 0.44 0.00 0.59
37.83 916 1.59 0.55 1.59 0.00 0.17 0.47 0.11 0.40
38.00 920 1.50 0.41 1.57 0.00 0.06 0.35 0.04 0.19
38.17 924 1.48 0.32 1.61 0.00 0.12 0.35 0.02 0.14
38.33 928 1.51 0.37 1.73 0.00 0.13 0.42 0.09 0.19
38.50 932 1.52 0.29 1.76 0.00 . 0.06 0.38 0.03 0.14
38.67 936 1.66 0.35 1.97 0.00 0.24 0.48 0.15 0.25
38.83 940 1.59 0.28 2.06 0.00 0.14 0.47 0.12 0.24

 

 

 

 

 

 

 

 

 

118

 

Table D.8 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

39.00 944 1.57 0.26 2.04 0.00 0.14 0.40 0.03 0.15
39.17 948 1.48 0.17 2.02 0.00 0.05 0.35 0.00 0.09
39.33 952 1.51 0.19 2.12 0.00 0.16 0.37 0.07 0.13
39.50 956 1.47 0.17 2.15 0.00 0.09 0.34 0.02 0.08
39.67 960 1.53 0.20 2.31 0.00 0.09 0.39 0.04 0.15
39.83 964 1.55 0.23 2.39 0.00 0.16 0.43 0.08 0.12
40.00 968 1.41 0.15 2.32 0.00 0.05 0.31 0.01 0.08
40.17 972 1.44 0.16 2.42 0.00 0.04 0.38 0.00 0.13
40.33 976 1.39 0.17 2.41 0.00 0.16 0.39 0.00 0.08
40.50 980 1.33 0.10 2.42 0.00 0.02 0.33 0.00 0.03
40.67 984 1.39 0.19 2.57 0.00 0.06 0.38 0.00 0.09
40.83 988 1.44 0.19 2.65 0.00 0.14 0.45 0.00 0.15
41.00 992 1.38 0.16 2.62 0.00 0.08 0.40 0.00 0.07
41.17 996 1.38 0.18 2.72 0.00 0.09 0.43 0.00 0.10
41.33 1000 1.28 0.12 2.72 0.00 0.07 0.44 0.01 0.09
41.50 1004 1.34 0.17 2.81 0.00 0.08 0.42 0.00 0.09
41.67 1008 1.39 0.18 2.90 0.00 0.17 0.47 0.06 0.14
41.83 1012 1.39 0.19 2.99 0.00 0.12 0.46 0.06 0.13
42.00 1016 1.32 0.14 2.96 0.00 0.06 0.39 0.01 0.06
42.17 1020 1.29 0.09 3.01 0.00 0.03 0.39 0.00 0.07
42.33 1024 1.26 0.11 3.05 0.00 0.10 0.34 0.00 0.07
42.50 1028 1.22 0.07 3.04 0.00 0.02 0.24 0.00 0.00
42.67 1032 1.27 0.11 3.24 0.00 0.00 0.25 0.00 0.05
42.83 1036 1.29 0.12 3.43 0.00 0.17 0.19 0.00 0.01
43.00 1040 1.25 0.12 3.48 0.00 0.03 0.08 0.00 0.00
43.17 1044 1.25 0.09 3.48 0.00 0.05 0.09 0.00 0.03
43.33 1048 1.11 0.01 3.43 0.00 0.04 0.08 0.00 0.04
43.50 1052 1.27 0.13 3.37 0.00 0.00 0.05 0.00 0.09
43.67 1056 1.33 0.17 3.40 0.00 0.17 0.05 0.00 0.15
43.83 1060 1.38 0.20 3.57 0.00 0.16 0.11 0.00 0.15
44.00 1064 1.36 0.13 3.47 0.00 0.13 0.16 0.00 0.11
44.17 1068 1.27 0.13 3.40 0.00 0.10 0.11 0.00 0.09
44.33 1072 1.31 0.14 3.28 0.00 0.09 0.09 0.00 0.09
44.50 1076 1.35 0.15 2.88 0.00 0.11 0.13 0.00 0.10
44.67 1080 1.42 0.18 2.57 0.00 0.16 0.16 0.00 0.15
44.83 1084 1.43 0.15 2.60 0.00 0.19 0.17 0.11 0.17
45.00 1088 1.38 0.12 2.56 0.00 0.13 0.15 0.08 0.14
45.17 1092 1.43 0.13 2.60 0.00 0.13 0.15 0.07 0.13
45.33 1096 1.47 0.15 2.60 0.00 0.06 0.15 0.06 0.13
45.50 1100 1.41 0.07 2.57 0.00 0.14 0.10 0.01 0.07
45.67 1104 1.48 0.13 2.66 0.00 0.13 0.12 0.04 0.12
45.83 1108 1.45 0.09 2.63 0.00 0.10 0.10 0.03 0.08
46.00 1112 1.46 0.09 2.62 0.00 0.08 0.08 0.00 0.05
46.17 1116 1.52 0.09 2.68 0.00 0.13 0.11 0.01 0.00
46.33 1120 1.48 0.08 2.60 0.00 0.11 0.09 0.03 0.17
46.50 1124 1.49 0.10 2.57 0.00 0.11 0.07 0.00 0.08
46.67 1128 1.64 0.13 2.60 0.00 0.17 0.13 0.04 0.13
46.83 1132 1.70 0.17 2.51 0.04 0.26 0.21 0.16 0.24

 

 

 

 

119

 

 

 

 

 

 

Table D.8 continued

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

47.00 1136 1.73 0.14 2.20 0.16 0.12 0.13 0.09 0.13
47.17 1140 1.81 0.18 1.99 0.17 0.28 0.18 0.14 0.20
47.33 1144 1.70 0.12 1.82 0.07 0.18 0.10 0.06 0.12
47.50 1148 1.56 0.05 1.68 0.00 0.03 0.01 0.00 0.00
47.67 1152 1.69 0.13 1.69 0.00 0.10 0.00 0.00 0.01
47.83 1156 1.75 0.13 1.65 0.00 0.13 0.00 0.00 0.05
48.00 1160 1.72 0.11 1.47 0.00 0.06 0.00 0.00 0.00
48.17 1164 1.75 0.17 1.40 0.00 0.14 0.00 0.00 0.02
48.33 1168 1.73 0.14 1.19 0.00 0.16 0.04 0.00 0.05
48.50 1172 1.77 0.20 1.07 0.00 0.14 0.00 0.00 0.00
48.67 1176 1.92 0.25 1.02 0.00 0.28 0.10 0.00 0.15
48.83 1180 1.95 0.22 0.89 0.00 0.29 0.11 0.11 0.15
49.00 1184 1.80 0.16 0.63 0.00 0.17 0.01 0.00 0.03
49.17 1188 1.83 0.12 0.49 0.00 0.19 0.00 0.05 0.02
49.33 1192 1.82 0.12 0.29 0.00 0.22 0.03 0.07 0.05
49.50 1196 1.84 0.11 0.21 0.00 0.22 0.01 0.04 0.02
49.67 1200 1.99 0.14 0.29 0.00 0.36 0.11 0.16 0.15
49.83 1204 1.86 0.15 0.24 0.00 0.34 0.09 0.14 0.12
50.00 1208 1.88 0.09 0.17 0.00 0.30 0.03 0.09 0.05
50.17 1212 1.81 0.09 0.16 0.00 0.31 0.01 0.11 0.05
50.33 1216 1.80 0.08 0.13 0.00 0.34 0.00 0.13 0.06
50.50 1220 1.67 0.06 0.11 0.00 0.34 0.08 0.14 0.04
50.67 1224 1.58 0.10 0.19 0.15 0.44 0.09 0.22 0.10
50.83 1228 1.19 0.10 0.17 0.18 0.45 0.07 0.23 0.08
51.00 1232 0.87 0.06 0.15 0.13 0.44 0.03 0.25 0.05
51.17 1236 0.63 0.07 0.12 0.15 0.48 0.01 0.28 0.03
51.33 1240 0.41 0.06 0.12 0.13 0.49 0.01 0.30 0.02
51.50 1244 0.16 0.05 0.09 0.10 0.49 0.00 0.31 0.00
51.67 1248 0.14 0.08 0.15 0.19 0.61 0.02 0.41 0.08
51.83 1252 0.05 0.09 0.15 0.22 0.68 0.05 0.44 0.08
52.00 1256 0.01 0.08 0.10 0.19 0.69 0.01 0.39 0.04
52.17 1260 0.04 0.07 0.09 0.15 0.70 0.00 0.38 0.02
52.33 1264 0.03 0.08 0.10 0.23 0.56 0.02 0.38 0.03
52.50 1268 0.02 0.06 0.07 0.20 0.35 0.00 0.34 0.01
52.67 1272 0.10 0.12 0.18 0.31 0.27 0.09 0.36 0.14
52.83 1276 0.10 0.11 0.16 0.31 0.13 0.09 0.36 0.11
53.00 1280 0.03 0.06 0.06 0.23 0.01 0.00 0.18 0.01
53.17 1284 0.01 0.02 0.02 0.18 0.00 0.00 0.07 0.00
53.33 1288 0.00 0.00 0.00 0.17 0.00 0.00 0.00 0.00
53.50 1292 0.00 0.01 0.01 0.24 0.00 0.00 0.00 0.00
53.67 1296 0.02 0.06 0.09 0.28 0.00 0.00 0.03 0.01

 

 

 

 

 

120

 

APPENDIX E

GAS CHROMATOGRAPH CALIBRATION CURVES

121

% CH4

Table E.1 Gas Chromatograph Calibration Data - Methane

 

 

 

 

 

 

 

Samgll'eflze P733223” Area Height
100 5.622 290,824 19,131

75 5.792 231,558 14,555

50 5.943 154,392 10,120

50 (LD) 5.920 166,176 10,668
25 5.410 68,240 5,514

 

 

 

 

 

L0 = lab duplicate

100 ¢

 

90 -ll-- ___,Ai________ _____ _m _i" 7 /

so 2“ .. /
y = 3.3032E-04x
R2 = 0.93503
70 _. _______, A“ ,

 

 

 

50 ""— 4—‘_— / V —
4° 47 f /
30 —’

/

 

 

 

 

20 -fi—

10

 

 

 

 

 

0 50.000 100.000 150.000 200.000 250.000 300.000
GC Peak Area

Figure E.1 Methane Calibration Curve

The trend line was set to a zero-intercept.

122

 

350.000

% C02

Table E.2 Gas Chromatograph Calibration Data - Carbon Dioxide

 

 

 

 

 

 

 

Sample Size Peak time .

(PL) ( min.) Area Height

100 8.170 391,603 20,814

100 (LD) 8.188 394,110 20,909
75 8.123 296,020 16,444

50 8.285 202,706 12,209

25 8.168 108,070 7,143

25 (LB) 8.517 121,700 6,926

 

 

 

 

 

 

LD = lab duplicate

100 /
90 " if /
80 7 7 7 /
7° y = 2.5147E-04x
R2 = 0.99310
60 ~- ~

50+-

 

 

 

 

 

 

40

 

 

 

 

30 *9

 

 

20

1o - A

 

 

 

 

 

0 50.000 100.000 150.000 200.000 250.000 300.000 350.000 400.000 450.000
GC PeakArea

Figure E.2 Carbon Dioxide Calibration Curve

The trend line was set to a zero-intercept.

123

APPENDIX F

GAs CHROMATOGRAPHY DATA

124

Tables F.1, F .2, F.3 and FA present the gas chromatography data for
Cases A, B-1, B-2 and C, respectively. The samples are listed in the order in
which they were collected and analyzed, to maintain any evidence of situational
effects. For example, it can be deduced that the methane present in the de-
ionized water sample (Tables F.1, F .2 and F.3) is residual from the preceding
sample.

“lsothermic” refers to a malfunction in the temperature ramp. These
analyses were carried out at an oven temperature of 40°C rather than the regular
40°C to 120°C ramp. The only significant affect was a delayed peak time; the
peak areas are comparable and therefore the results were judged valid.
Readings were marked as ‘below the detection limit’ for those resulting in a
negative value on a calibration curve.

The gas chromatograph was first operational at the very last days of Case
A, for which calibration samples were also analyzed on 5/9/07. Equipment
malfunctioned before the wastewaterlseed/nutrients flask could be analyzed; the
trial was over before the problems were remedied. For Case B-1, equipment
malfunctioned following the fifth sample analysis (which also had an unidentified
peak at 7.737 minutes). Testing was resumed several days later once the
equipment was replaced. All flasks analyzed on the first day were re—sampled
during this second day of testing. For Case C, gas samples from each flask were
tested three days apart to test for methane fluctuations, which were considerable

for some flasks (see also Table 4.5).

125

Table F.1 Gas Chromatography Data: Case A

 

 

 

 

 

 

 

 

 

 

 

 

Sample Peak

Date Sample ID Slze (pli Time Area % (gas)
5/9/07 Wastewater, Seed 100 5.421 188,866 62.4 CH4
“6”) 8.028 37,212 9.4 002
Wastewater, Seed 100 5.718 220,889 73.0 CH4

(rep B) 8.511 43,752 11.0 002
5/10/07 CH4 75 5.408 194,676 84.3 CH4
C02 75 5.571 1,276 0.4 CH4

7.915 286,545 72.1 C02

CH4 50 5.464 130,148 43.0 CH4

8.086 11,584 2.9 002

002 50 7.949 193,482 48.7 002

Seed 100 5.425 195,331 64.5 CH4

8.065 33,827 8.5 002

112 (Wastewater, 100 5.783 142,342 47.0 CH4

seed' Numents) 8.555 35,201 8.9 002
Wastewater, Nutrients 100 5.788 113,680 37.6 CH4

8.548 19,387 4.9 002

De'i°"ized Water 100 5.849 78,102 25.8 CH4

 

 

 

 

 

 

126

 

Table F.2 Gas Chromatography Data: Case B-1

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Sample Peak

Date Sample Size (uL) Time Area % (gas)
6/1/07 CH4(isothermic) 50 6.868 156,819 51.8 CH4
002 50 8.743 229,834 57.8 002
Wastewater, Seed, 100 5.851 164,196 54.2 CH4
Numems 8.665 30,678 7.7 coz
Wastewater, Seed 100 5.803 144,777 47.8 CH4

(rep 8’ 8.602 21,276 5.4 002
H

13290333233; 1°° 3:33.? 33:33: ”Suki;

8.560 27,369 6.9 C02

6/7/07 CH4 (isothermic) 50 6.983 136,269 45.0 CH4
002 50 7.977 203,189 51.1 002
Wastewater, Seed, 100 5.724 214,741 70.9 CH4
V’Numems 8.511 26,599 6.7 002
Wastewater, 100 5.722 14,538 4.8 CH4
Numents 8.397 15,953 4.0 002

Seed 100 5.695 207,282 68.5 CH4

8.492 14,105 3.5 002

Wastewater, Seed, 100 5.700 197,445 65.2 CH4
Numems 8.477 30,746 7.7 002

1/2 (Wastewater, 100 5.689 134,902 44.6 CH4

seed’ Numems) 8.431 15,592 3.9 002
De-ionized Water 100 5.817 17,254 5.7 CH4
Wastewater, Seed 100 5.667 206,199 68.1 CH4

(rep B) 8.444 21,691 5.5 002

CH4 75 5.673 223,581 73.9 CH4

8.477 4,586 1.2 002

 

 

 

 

 

 

127

 

Table F.3 Gas Chromatography Data: Case B-2

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Sample Peak

Date Sample Size (uL) Time Area % (gas)
7/13/07 602 50 9.199 210,200 52.9 002
002 50 9.027 193,959 48.8 002

CH4 50 5.798 121,183 40.0 CH4
CH4(isothermic) 75 7.337 237,352 78.4 CH4
Wastewater, Seed, 100 5.816 179,418 59.3 CH4
Numents(rep A) 8.619 26,214 6.6 002
Wastewater, Seed 100 6.162 85,328 28.2 CH4

9.086 9,157 2.3 002

1/2 (Wastewater, 100 6.213 117,078 38.7 CH4
seed'Numents) 9.161 15,120 3.8 002

Seed, Nutrients 100 6.207 207,459 68.5 CH4

9.199 24,659 6.2 602

Seed 100 6.135 171,570 56.7 CH4

9.088 14,026 3.5 002

Wastewater, Seed, 100 6.113 226,356 74.8 CH4
Nutrientsuep 8’ 9.079 31,383 7.9 002
De-ionized Water 100 6.257 16,982 5.6 CH4

 

 

128

 

Table F.4 Gas Chromatography Data: Case C

 

 

 

 

 

 

 

 

 

 

 

 

 

Sample Peak
Date Sample Size (EL) Time Area % Ages)
808/07 CH4 50 6.66 170,266 56.2 CH4
coz 50 8.679 193,748 48.7 002
Manure, Seed 100 5.954 214,560 70.9 CH4
8.827 50,627 12.7 002
Manure. Seed. 5.897 191,580 63.3 CH4
. 100
Nutnents
8.734 55,393 13.9 002
Wastewater, Manure, 100 5.935 175,228 57.9 CH4
Seed, Nutrients
8.756 84,255 21.2 C02__
Wastewater, Seed, 5.963 82,791 27.3 CH4
. 100
Nutnents
8.754 45,745 11.5 C02
Manure 100 5.899 192,828 63.7 CH4
8.737 55,904 14.1 C02
Wastewater, Manure, 5.862 188,31 1 62.2 CH4
100
Seed
8.673 92,910 23.4 C02
Seed, Nutrients 100 5.968 184,817 61.0 CH4
8.873 92,910 23.4 COL
Wastewater, Seed 1 00 6.1 1 9 15,806 5.2 CH4
8.909 39,333 9.9 002
8mm CH4 75 6.467 238,939 78.9 CH4
002 50 9.305 184,557 46.4 002
Wastewater. Seed. 6.060 190,201 62.8 CH4
Nutrients 100
9.105 114,662 28.8 002
Wastewater, Manure, 100 6.393 120,978 40.0 CH4
seGd' Numems 9.405 57,958 14.6 COL
Manure. Seed. 6.372 234,058 77.3 CH4
Nutrients 100
9.428 73,680 18.5 C02
Manure. Seed 100 6.321 235,355 77.7 CH4
9.372 60,933 15.3 C02
Manure 100 6.355 213,580 70.5 CH4
9.398 77,922 19.6 002

 

 

 

 

 

 

 

 

 

 

 

 

129

 

 

Table F.4 continued

 

 

 

 

 

8/31/07

continued Seed. Nutrients 100 6.417 247,295 81.7 CH4
9.502 60,663 15.3 002
Wastewater, Seed 100 65:” 52'916 17'5 CH4
9.513 106,658 26.8 coz
Wastewater. Manure. 5.917 177,918 58.8 CH4

Seed 100
8.72 85,738 21.6 002
LD Manure, Seed 100 5.837 199,465 65.9 CH4
8.665 52,157 13.1 coz

 

 

 

 

 

LD = Lab Duplicate

130

 

APPENDIX G

QUALITY ASSURANCE AND QUALITY CONTROL

131

Quality assurance and quality control measures for the parameters
analyzed in-house included lab duplicates and standards, when applicable. Lab
duplicates were utilized in all testing. Table 6.1 gives the average percent
relative range of the lab duplicates for the various parameters. Standards were

available for COD, total phosphorus and gas chromatography testing. Table 6.2

gives the average percent recovery for these tests.

Table 0.1 Percent Relative Range for Duplicates

 

Average

 

 

 

 

 

 

 

 

 

 

Standard No. of
0
Parameter A 2:52“ Deviation Analyses
Total Solids 6.57% 9.68% 4
Volatile Solids 2.50% 2.91% 3
COD 5.29% 3.39% 7
Total Phosphorus 8.64% 2.1 1% 3
Respirometer o o
(cumulative gas) 2'74 /° 1'45 /° 3
Gas Chromatography 17.91% 1.79% 2

 

Table 6.2 Percent Recovery for Standards

 

 

 

 

 

 

 

 

Avera e Standard No. of
Parameter % Recogery Deviation Analyses
COD 104.1% 2.7% 10
Total Phosphorus 94.8% 12.8% 3
Gas 94.2% (0H4) 9.47% (CH4) 9
Chromatography 101.0% (002) 8.52% (002) 8

 

132

 

 

APPENDIX H

ANAEROBIC DIGESTION FEASIBILITY PROTOCOL

133

H.1 Processor’s Goals and Objectives
Obtain the following information from the food processor and compare

these goals and expectations with reasonable deliverables. See Appendix J for

assessment worksheets.
1. Determine the processor’s interest in anaerobic digestion.
a. If a regional digester or co-digestion is being pursued, the

protocol must be carried out for all contributors, and a
representative substrate must be tested. Check all
governing regulations, as some locales prohibit the mixing Of
certain waste streams.

b. There should be no difference in assessment for individual
treatment vs. energy Objectives.

i. An energy study may conclude ‘only adequate for
treatrnent’.

ii. A treatment study may also conclude ‘adequate for
energy recovery.’

0. Methane potential can only be an estimate; there are several
determining factors in full-scale operation such as mixing
effects which cannot be accounted for in lab-scale testing.

2. Determine the desired biogas applications. There are many
indirect considerations for electric generation which should be
addressed upfront. (This is outside the scope of this protocol.

Consult an appropriate professional.) For example, if the electric

134

power will be sold back to a common grid, the utility company may

assess significant hook-up fees.

3. Identify the discharge requirements: the COD (mg/L) and/or BOD
(mg/L) as per regulations for applicable effluent discharge. BOD is
the conventional measurement of wastewater quality, however
COD is easier to measure and more representative of anaerobic
treatment potential than BOD.

a. It is assumed that fruit and vegetable processing waste
streams contain below the regulated limits for nitrogen and
phosphorus (and other nutrients and metals). If this is not
the case, these nutrients must also be factored in at this
step.

b. The required COD or BOD discharge concentrations will be
compared with waste stream concentrations to determine
the degree of treatment required. If adequate treatment
cannot be achieved by anaerobic digestion alone, an
alternate treatment or additional aerobic unit must be

considered. See Section H.3.2 to estimate treatment

potential.
4. Assess the relative economic status of the project.
a. Some operating costs and methane cost savings are

discussed throughout the protocol. Digestion of any given

waste may require regular addition of an alkalinity source,

135

nitrogen, phosphorus or metals and thus, an added
operating cost. This may be a significant or negligible cost
depending on the nutrient and level Of deficiency.

b. These considerations may be used to supplement a full cost-
benefit analysis (which is beyond the scope of this protocol).

5. Determine the processor’s timeline for operational treatment or

compliance.

a. This protocol may require several months for sampling and
testing. Further pilot-scale testing may be recommended,

which would require several months additional.

b. Full-scale system design and permit applications may take
over a year.

c. Construction, start-up and stabilization may require over a
year additional.

H.2 Plant Profile
Obtain the following information from the food processor. See Appendix J
for plant assessment worksheets.
1. Determine the plant’s average monthly energy usage (natural gas
in thm/month, and/or electricity in kWh/month). This can be

calculated from billing costs.

136

Identify the plant’s wastewater streams (by commodity or location in

the plant). Characterize the fluctuation in flow and COD loading

throughout the year and average temperature of each stream.

a.

If necessary, convert the units of COD (or BOD) to kg/day

and wastewater flow to malday.

Identify waste streams that are most appropriate for

anaerobic digestion, with high soluble organic loading.

i. Determine if streams currently may be combined to
equilibrate COD and volume loadings or may be
readily combined by installing piping. Alternately,
consider if streams with low organic loading could be
readily separated and diverted, such as storm water.

ii. A high peak in volume or COD may require a large

equalization tank, adding to construction costs.

Identify the commodities processed and the fluctuation in volume

processed throughout the year. See Appendix I for assessment

worksheets.

b.

Correlate this with the data from section H.1.2 above.

If data for section H.1.2 iS not available, the plant’s
commodity data and water use may be used to approximate
ranges for BOD loading and waste stream flow using

published data for each commodity (ex: gal/day per ton

137

processed). Weight these accordingly for each commodity

processing rate per year (tons/month * # of months/year).

List any known cleaners, sanitizers or chemical additives used in

processing that may be present in the different waste streams. lf

certain compounds are only used in Specific areas (waste streams)

specify which.

a.

Compounds may include (but are not limited to):

Oxidizing sanitizers

o Hyperchlorites, chlorine, chloramines

- Organic bromine

- Iodine, alcohol-iodine, iodophors

0 Hydrogen peroxide, peroxy acids

Biocides and non-oxidizing sanitizers

0 Organic acids (e.g. acetic acid, propionic acid, formic
acid, carboxylic acids)

0 Acid anionic sanitizers

o Acid-quat sanitizers

o Quaternary ammonium compounds

Any compounds present may serve as potential sources of

toxicity that may interfere with anaerobic digestion. It may

be possible for a full scale digester may acclimate and adapt

to such toxicity.

138

c. If specific concentrations can be determined, compare the

present levels to a known l050 (inhibitive concentration) if

available. See Blum and Speece (1991).

d. For concentrations near the l05o level, anaerobic treatment

and methane production may be severely retarded. An
alternate wastewater treatment Should be pursued if the
chemical(s) of concern cannot be replaced with one(s) less

toxic.

H.3 COD Conversion to Heat and Electric Potential

1.

If historical plant data is unavailable (section H.2.3), analyze the
processing plant’s average daily wastewater COD concentration
and daily water volume usage. Characterize COD levels for as
many commodities as possible. If time does not permit testing of all
commodities, consult published COD estimates to identify ‘high’
and ‘low’ COD level commodities in order to ensure that
representative commodities are tested at the very least. Take
samples during a transition period to include at least two
commodities. Using results from only the ‘worst’ commodity (i.e.
that with the highest COD) may provide overestimated results in
methane potential.

a. Test COD using Hach Method 8000.

i. Collect field duplicates.

139

ii. Verify testing methods using lab duplicates. The
percent difference should be less than 20%.
b. Compare test results against published commodity ranges.

(See _Commogitv Report and Categorization of Michigan

crogs.)

2. Consider the average and peak COD loading (kg/m3/d) and

assume an appropriate reactor type based on Table H.1 below,
with a given COD removal treatment efficiency (e.g. 80 to 90%):

Table H.1 Types of Anaerobic Digesters

 

 

 

 

 

 

 

 

 

 

 

Reactor Type COD loading* COD removal rates*
COHtaCt (ANCP)** 1_5 kg/mgld 70-95%
Filters 5_20 kg/m3/d 70-90%
EFB" 10-40 kglmsld 60'35%
*Totzke (2006)

** ANCP = Anaerobic Contact Process
UASB = Up-flow Anaerobic Sludge Blanket
EFB = Expandedl fluidized bed

3. Calculate a COD removal rate (kg/d) based on reactor treatment

efficiency using equation H.1.

COD removal rate (kg/d) = minimum %COD removal (%I 100) * average COD

influent (kg/m3) * flow rate (ma/d) [H.1]
4. Based on COD removal, calculate the heating and electric
potentials.

140

a. For estimated heating potential see equation H.2 (Speece,

1996x

Btu/d = 12x106 Btu l 1000 kg COD removed * COD removal rate (kg/d) [H.2]

b. For estimated electric wattage potential see equation H.3

(Speece, 1996):

MWhr = (1 MWI107 Btu) * (12x106/ 1000 kg COD removed) * COD removal rate

(mm*umw mm

5. Compare these results to the processor’s energy needs (section
H.1). If the results are appropriate for the processor’s intended

anaerobic applications, continue on to section H4.

H4 Substrate Characterization Tests

The COD conversions to Btu and MW estimates do not account for
variability in substrate biodegradability. To properly assess the anaerobic
digestibility of a given waste stream, several other parameters must be analyzed.
Historical data should be available (Often collected monthly and annually per
regulations).

1. Retrieve historical wastewater effluent data for the past 1 to 2

years.

141

2. Collect wastewater effluent samples, throughout the season if

possible. Samples must be representative of both the dominant

commodity(s) and those with the highest COD loading (which may

be more seasonal, e.g. pumpkins).

3. Test the samples for the parameters listed in Table H.2.

Table H.2 Substrate Characterization Analyses

 

 

 

 

 

 

 

 

 

Analysis Method Suggested Range Source
pH pH meter 6.5 to 8.2 Speece, 1996
Alkalinity Hach 8203 2000 to 3000 Speece, 1996
mglL CaCO3
COD Hach 8000 > 1000 mglL COD Speece, 1996
(EPA approved)
Total Nitrogen EPA-350.1, 353.2, 3 to 5 mg/L N per Bouallagui et al.,
series 351.3, 3502/3513 100 mg/L COD 2004b
Ammonia EPA-350.1 Speece, 1996
> 4° ‘° 7° "‘Q’L ”“4 Calli, et al. 2005
< 1500 mg/L NH4
Total Phosphorus Hach 8190 0.5 to 1 mg/L P per Bouallagui et al.,
100 mg/L COD 2004b
Total Solids (TS) Hach 8271 < 10% for batch tests Carucci et al., 2005
(EPA approved)

 

Volatile Suspended
Solids (VSS)

Hach 8158, 8164

Calculate VSS:TS.
The higher, the better.

 

Sulfide

EPA-376.2

>2mgLS
<200 rqu S

Isa et al., 1986

 

 

Sulfate

 

EPA-375.4

< 5000 mglL $04
for treatment

< 300 mg/L $04
for biogas applications

 

 

Isa et al., 1986

 

4. If processed commodities include foods high in polyphenols or long

chain fatty acids (> 100 mglL), then pretreatment may be required

(see Chapter 2: Literature Review), which would raise capital

and/or Operating costs depending on the chosen treatment method.

142

 

a.

High-phenol foods include (www.kirkmanlabs.com):

Apricots
Berries
Cherries
Dill

Licorice (Anise)
Mint

Olives
Oranges
Pineapple
Peppers
Red grapes

Tomatoes

5. Analyze the test results and assess the implications for the

processor’s goals as described below.

a.

If pH is too low, then acetate production does not occur and

methane will not be produced. If pH iS too high, then less

ammonia (NH3) ionizeS to ammonium (NH4+) and becomes

toxic.

Estimate the alkalinity amendment required using equation

H.4. This is only a rough estimate, and alkalinity production

will not be accurately represented at a lab scale.

143

Added alkalinity mglL [day = 10%(influent COD mglL) - influent alkalinity mg/L
[H.4]

i. Low-protein waste will generate little to no alkalinity
during digestion.

ii. Consider the cost of alkalinity treatment per year and
include as an operating cost. Cost can vary widely
with alkalinity source and potentially be significant.
See Speece (1996) for treatment options and cost
calculations.

iii. Alkalinity Should be tested and determined later
during full-scale reactor operation in proportion VFA
levels, and residual alkalinity calculated.

c. COD/NIP Should be approximately 100/4/1 by weight
(Bouallagui et al., 2004b). Low N or P levels will ultimately
limit digestion, but may take more than 20 to 40 days to
manifest in a large scale system.

i. Co-digestion with a nutrient-rich substrate may help.
Otherwise, nutrients must be added. E.g. manure
and yogurt are high in phosphorus; manure and
beans are high in nitrogen.

ii. Estimate the cost of nutrient addition per year. The
cost will depend on which compound(s) are chosen

as a nutrient source. These costs account for

144

operating costs and are calculated by equations H5

and H6.

Cost of N addition ($lyr) = [Required N (kg N/1000 kg COD) *COD loading
(kg/day) - Available N (mg/L) *1 kgl1000 mg*wastewater loading (Uday)]

*cost of N ($lkg as N) * days Of operation/yr [H.5]

00st of P addition ($lyr) = [1/4 *Required N (kg Nl1000 kg COD) * COD loading
(kg/day) - Available P (mg/L) * 1kg/1000 mg * wastewater loading (Uday)]

* cost of P ($Ikg as P) * days of operation/yr [H.6]

d. Total solids >10% can inhibit digestion, particularly in batch
tests.
e. The % Volatile solids is the organic fraction, which is

available for biodegradation.

f. High sulfide concentrations will produce H28 gas, and
sulfate concentrations will promote sulfate reducing bacteria
which produce H28 gas. The biOgas may need to be

pretreated.

i. For example, Tennessee air permits required less

than 1800 ppm H2S so an industrial digester installed

a biogas scrubber (Rosdil, 2006).

145

ii. Some internal combustion engines can utilize biogas
if the hydrogen sulfide is less than 60 ppm.

iii. Hydrogen sulfide at 800 to 1000 ppm can be fatal to
humans.

9. High salt concentrations may inhibit digestion. Over time, a
digester may be able to acclimate to a higher degree.

h. High phenol or LCFA concentrations may require
pretreatments (see Chapter 2: Literature Review), which
would raise capital and/or operating costs, depending on the
chosen treatment method.

6. If initial test concentrations are within the acceptable ranges,
continue to Section H.5. If some of the concentrations are outside
the appropriate ranges, estimate the costs to rectify these issues.
a. If the required nutrient addition or toxicity treatment is

economically prohibitive, the waste-stream is inappropriate

for anaerobic treatment.

H.5 Anaerobic Respirometry

The respirometer is used to conduct the biodegradability tests (similar to
' serum bottles). Microbial seed, nutrient media and wastewater substrate are
measured out in multiple reaction flasks. Flasks are stirred and incubated at a
constant temperature in a water-bath. The respirometer measures individual

real-time biogas production for each flask. Computer software calculates

146

progressive gas production rates and cumulative gas production. Gas samples

of the headspace are collected by syringe and analyzed by gas chromatograph

to determine the percent methane production. The specific procedure is

presented below.

1.

Collect an appropriate feed stock sample from the processing plant.
Synthesized feed solution CANNOT be used. The full array of
processing waste constituents cannot be replicated and may
include disinfectants or toxic compounds that could disrupt
anaerobic digestion, the affects of which must be properly
analyzed. Any solid waste in the sample Should be removed or
processed to a liquid consistency and diluted to a total solids
content of 1 to 5%. To test the biodegradability of intact solid
constituents consider implementing a bench—scale reactor instead,
as high solids content can inhibit batch systems.

Identify an anaerobic seed source. Possible resources include a

local anaerobic digester, a lagoon at the food processing plant

showing evidence of anaerobic activity, manure (rumen) slurry or a

lab culture.

a. TO maximize biological activity, collect fresh seed just before
setting up the respirometer. Color can serve as an indicator
of anaerobe quality. Active seed will exhibit a dark black
color; inactive or unviable seed may be grey or light Olive

green.

147

Refrigerate the seed sample if time necessitates.
Anaerobes will remain dormant yet viable at low
temperatures. A longer refrigeration period will result in a
longer start-up time; in this case such a delay is not the
result of toxicity or acclimation but from the anaerobes Slow

reactivation.

Set up the respirometer. See Appendix I for the respirometer set-

up procedure and the Challenge System respirometer manual.

Collect gas samples from the head space of each reaction flask.

Analyze the samples via gas chromatography and record the CH4

and 002 fractions throughout normal reactor operation.

At a minimum, sample the flasks during peak gas production
and at the end of the run.

Designate one gas-collection syringe for all sampling to
ensure the same operation and sample volume for each
flask.

Between samplings flush the syringe with ambient air
several times (rather than headspace gas), to minimize the
volume drawn from the flasks and reduce negative pressure

in the respirometers bubble counters.

148

d. Use gas cylinders of standardized composition (CH4 and

002) to establish a calibration curve. Verify calibration with

each sampling event.
If methane production remains low or unstable 15 days after

startup, consider the following amendments.

a. Add a greater volume of seed to each flask.
b. Add more micronutrients (S, Fe, Ni, 00)
c. If solid waste is being tested, be sure to dilute to < 5% TS.

End the respirometer test once all flasks cease gas production.

Test the pH and COD of each flask.

Analyze the respirometer results.

a. Graph the cumulative biogas production (mL) vs. time
(days).

b. Graph the biogas production rate (mUhr) vs. time (days).

c. Calculate the approximate percent theoretical methane
production.
i. Subtract out methane production from the seed

control.

ii. The theoretical (maximum possible) methane

production is 395 mL CH4 per 1000 mg COD at 35°C.

d. Compare methane potential to current energy usage. Use

the results from sections H.2.2 or H.3.1 (COD) and section

149

H.5.7 (respirometer) to reassess the economic benefit of an

anaerobic system (first evaluated in section H35). 1 thm
can be provided by 96.7 ft3 natural gas.
If the overall respirometer results are poor (after allowing 30 for
seed acclimation), then conduct a toxicity test (section H.6) to

determine if substrate components are a source of methanogen

inhibition. Poor results are constituted by:
a. < 60% CH4 fraction in biogas
b. < 60% theoretical biogas produced.

lf respirometer methane production is good, then proceed to

Section H.7 to interpret the overall results.

H.6 Toxicity Test

lf overall respirometer tests are poor, conduct a toxicity test.

1.

See Speece (1996) and/or Owen et al. (1979) for toxicity test
methods. The basis of the test is to monitor gas production rate
while adding increasing levels of substrate. If the methane
production rate decreases as the substrate level added increases,
this is an indication of toxicity.

lf toxicity is confirmed, conclude ‘no further study’ is necessary and
report anaerobic digestion to be an inappropriate treatment

technique for this substrate.

150

lf toxicity is not an issue, essential nutrients may be lacking or the
seed-to-substrate ratio in the reaction flasks may be too large to
distinguish gas production from the substrate. Consider a different

respirometer set-up and run the test again with fresh seed.

H.7 Interpretation

1.

Compare the predicted COD destruction and methane production

to the intended treatment goals and biogas applications. Compare

methane results to theoretical methane production and energy

potential.

Consider implications of various results, including economic and

environmental consequences.

a. If nutrients are lacking and respirometer results are poor, co-
digestion may be worth considering.

b. Re-evaluate the protocol for the blended substrate
conditions.

If conclusions support anaerobic digestion, the processor should

then conduct a pilot scale reactor study. Small batch tests such as

the respirometer provide are not representative of large-scale

mixing effects or sustained alkalinity needs. Pilot scale reactors

must be tested before full-scale projects are pursued.

151

APPENDIX |

RESPIROMETER SET-UP PROCEDURE

152

I.1 Flask Allocation

Determine the desired flask assignments including which will serve as
controls and which as duplicates. Then determine the appropriate volume
allocation of substrate, seed (if used) and nutrient solution (if used) for each
flask, using the following guidelines. When any constituent is not used for a
particular flask, that volume should be replaced with de-ionized water.

First, allocate the substrate. Include between 150 and 250 mg COD.
More than 150 mg Should insure a significant net biogas volume; less than 250
mg should insure that the trial finishes in less than 45 days, though this will also
depend on the seed activity. This COD amount will correspond to a given
volume of substrate based on its COD concentration (mg/L). Subtract this
substrate volume from the working flask volume, where the working volume is
equal to the total volume less 10% for the headspace. This remaining volume

consists of the seed and nutrient solution:

VSeed + Nutrients = 0-9 VTotal - VSubstrate [31]

where VSubstrate = 200 mg COD / X mglL CODSubstrate

The seed and nutrient volume is subdivided at a ratio of 1 part seed to 4
parts nutrient solution. Resazurin, an oxygen indicating dye, should be added to
each flask for a final concentration of 1 mglL. For 600 mL flask volumes, add
approximately 0.5 mg. As resazurin iS a fine powder, it is easiest to first mix a
concentrated solution (1000 mglL) dissolving 10 mg in 10 mL of water and then

pipetting 0.5 mL into each flask.

153

Most flasks will not include all three components. For these cases,
replace any component (or partial volume, e.g. 1/2 nutrients or 1/2 [wastewater,
seed, nutrientsj) with de-ionized water. This insures the different flasks have

comparable dilutions.

l.2 Nutrient and Metal Solutions

The nutrient solution is composed of mineral and metal solutions. This is
such because the trace metals are at such a low concentration in the nutrient
solution that it is necessary to mix a more concentrated metal solution first. The
nutrient solution is taken from Shelton and Tiedje (1984).

Measure out one liter of de-ionized water into an Erlenmeyer flask with a

stir bar on a stir plate. Add to the flask the following measured amounts.

0 0.500 g MnCIz - 4H20

. 0.050 g H3B03

o 0.050 g ZnCl2

. 0.030 g CuCl2

. 0.010 g NazMoO4 . 2Hzo1
o 0.500 g COCI2 ° 6H20

o 0.050 g NiCIz ° 6H20

0.050 g NaZSe03

1
In the original text, this is denoted ‘Na2M04- 2H20’, and is assumed to be an error.

154

This constitutes the metal solution. Only a small fraction will be used for the
nutrient solution; the remaining can be stored for later testing.

New mineral solution should be made for each respirometer trial. For the
mineral solution, measure out enough de-ionized water to satisfy the flask
allocation requirements of nutrient solution, and pour into an Erlenmeyer flask
with a stir bar on a stir plate. Add to the flask the following amounts per liter of

water.
. 0.270 g KH2PO4
o 0.350 g K2HPO4
. 0.530 g NH4CI
o 0.075 g CaCI2 ° 2H20
. 0.100 g MgClz - 6H20 2
o 0.020 g FeClz ° 4H20

In the original text, this is denoted ‘MgCI - 6H20’, and is assumed to be an error.

Once all is dissolved, pipette 1 mL of metal solution into the mineral
solution. Transfer this mixed solution into glass jars with autoclavable caps.
Measure out the volume of de—ionized water required for the flask allocations into
similar glass containers. Sparge the headspace of each container with nitrogen
gas for at least ten seconds and cap tightly. Autoclave the containers for ten
minutes to drive off any dissolved oxygen. Once the containers have cooled to

room temperature (can be the following day). carefully transfer the solution to a

155

large Erlenmeyer flask taking care not to aerate it. Continuously sparge the flask

headspace with nitrogen gas while stirring gently with a stir bar and stir plate.

Add 1.20 g NaHCO3 per liter of solution, and cover the flask with parafilm.

I.3 Flask Set-up

Remove the wastewater sample(s) from storage to warm up. Collect the
seed sample at this time (if possible) and leave it at ambient temperature (or
remove from storage and warm to ambient temperature. Add a stir bar to each
clean reaction flask and then measure out the flask constituents, doing one at a
time for all flasks. Cap the flasks tightly, with a new septum in each cap. Take
care not to over tighten the caps and break them.

The color of the resazurin in the flasks should turn from blue to pink as the
seed (and sometimes the wastewater) is added, and again from pink to
‘colorless’ as the flasks are placed in the water bath and stirred. This color
change is indicative of reducing conditions and microbial activity.

As soon as possible, fill the water bath and place in the flasks, and then
start the water bath heater. It is best to bring up the flask temperatures gradually
with the water bath, rather than place the flasks in a pre-heated bath and
potentially shock the system. Vent the flasks at this time and hook them up to
the respective gas counters. Set up the software program and start data
collection immediately. The first eight to twelve hours, the gas pressure will
equilibrate as the temperature rises. Thus, the reported gas rates will not be

representative of true seed activity or actual gas production during this

156

equilibration period. After this initial start up period, check that the seeded flasks
have returned to septic conditions and are no longer tinted pink; any pink flasks

at this point may indicate a loose cap.

157

APPENDIX J

PROCESSING PLANT ASSESSMENT WORKSHEETS

158

Worksheet 1 of 3

 

 

 

 

Plant Name: Contact Info:

Assessment Date: Completed By:

1. Have you taken any measures to reduce water use or waste production?
Yes No

 

Please explain:

 

 

2. Have you considered anaerobic digestion?
Yes No

 

Please explain:

 

 

3. Anaerobic digestion can potentially produce methane (natural gas).
Does the plant use natural gas?

 

 

No
Yes, approximately thms per month
4. a. What is the current wastewater treatment method?

 

b. Are there discharge requirements?
BOD (mg/L)
Other

 

 

5. Please provide the plant’s current process-flow diagram(s).

Please note: All identifying information will be kept in strict confidence.
(Page 1 of 2)

159

6. Please list in the table below any cleaners, sanitizers or chemical additives
used in processing. lf certain compounds are only used in specific processing
lines (and waste streams) please specify which.

Such compounds may include (but are not limited to):
Oxidizing sanitizers
. Hyperchlorites, Chlorine, chloramines
0 Organic bromine
o Iodine, alcohol-iodine, iodophors
0 Hydrogen peroxide, peroxy acids
Biocides agd non-oxidizing sanitizers
0 Organic acids (e.g. acetic acid, propionic acid, formic acid, carboxylic
acids)
Acid anionic sanitizers
Acid-quat sanitizers
Quaternary ammonium compounds

Chemical Used Processing Line! Application Frequency
Waste stream ID ex: metered in or

 

Please note: All identifying information will be kept in strict confidence.
(Page 2 of 2) '

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162

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163

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