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ABSTRACT

Previous studies of thermophilic anaerobic digestion were

reviewed. Batch digestion (55°C) was used to develop a

thermophilic seed population from OWASA mesophilic digestion

sludge. Buffering was deemed to be beneficial. A sequence of 3 digestions produced a strong, viable thermophilic population. A ratio, intermediate alkalinity to partial alkalinity, was shown

to be a good measure of the important volatile acids to bicarbonate alkalinity ratio in anaerobic digestion. A

continuous thermophilic anaerobic digester was operated at

10 days hydraulic residence time, at 55°C, with daily draw and

feed. Operation was stable, with steady state achieved after

two residence times. Volatile solids destruction was 43 % and

gas generated was 900 ml/g volatile solids destroyed. Fecal

Coliforms and fecal streptococci were measured by the 5 tube Most Probable Number method. Fecal coliforms were reduced 5.8 logs,

down to logjDl.4. Fecal streptococci were reduced 2.75 logs down

to logju3.19. Proposed Class A pathogen reduction requires

logjQ2.00 for both indicator organisms. Therefore, the process

will not meet the proposed Class A requirement based on indicator organism levels in the effluent. Additional work is needed on

actual pathogen destruction using thermophilic anaerobic

digestion.

(2)

I'd like to thank my primary advisor, Mike Aitken, who

counseled me throughout this project, Mark Sobsey who contributed

valuable suggestions on MPN procedures, and Don Francisco who was

always a willing consultant at the Wastewater Research Center.

Of course, my fellow students and researchers at the Wastewater

Research Center always made it an enjoyable and cooperative place

to work. I appreciate OWASA funding this project, I trust it

answers some questions they had about thermophilic anaerobic

digestion. In particular I'd like to single out Walter

(3)

LIST OF TABLES AND FIGURES...v

1. INTRODUCTION...1

2 . LITERATURE REVIEW...3

2.1 Full-scale, Mixed, Thermophilic Digestion...4

2.2 Full-scale, Unmixed Thermophilic Digestion...9

2.3 Thermophilic Digestion in Moscow, U.S.S.R...11

2 . 4 Early Laboratory Experiments...11

2.5 Experimentation in the 1950's and 60's...13

2.6 Recent Laboratory Studies...15

2 . 7 Discussion...18

3. BATCH DIGESTION, DEVELOPMENT OF THERMOPHILES...24

3 .1 Method...24

3.2 Results...2 5 4. INTERMEDIATE/PARTIAL ALKALINITY RATIO (IA:PA)...35

5. CONTINUOUS THERMOPHILIC ANAEROBIC DIGESTION...40

5 .1 Method...40

5.2 Results...4 2 6 . DESTRUCTION OF INDICATOR ORGANISMS...59

6. 1 Method...59

6.2 Results...63

7 . CONCLUSIONS...70

REFERENCES...___...72 APPENDIX

MPN Raw Data

MPN Medium Formulas

(4)

1 .1 Proposed Criteria for Sludge Classification...2

3 . 1 Batch Digestions...26

5.1 Continuous Digestion - Steady State Operation...58

6 . 1 Summary of MPN Data...69

FIGURES 3 .1 Batch Digestion Run # 1...29

3 . 2 Batch Digestion Run # 2...30

3 . 3 Batch Digestion Run # 3...31

3 . 4 Batch Digestion Run # 4...32

3 . 5 Batch Digestion Run # 5...33

3 . 6 Batch Digestion Run # 6...34

4.1 Titrations, Addition of Acetate...37

4.2 Alkalinity, Addition of Acetate...38

4.3 IA:PA, Addition of Acetate...39

5 . 1 Continuous Digester Equipment...41

5.2 Feed Fixed Solids...43

5.3 Feed Volatile Solids...44

5.4 Feed Total Solids...45

5 . 5 Combined Feed Solids...46

5.6 Effluent Solids...47

5.7 pH...48

5.8 Alkalinity...49

5 . 9 Intermediate : Partial Alkalinity...50

5.10 Daily Gas Generated...51

5.11 Cumulative Gas Generated...52

5.12 Fraction Volatiles Destroyed...53

5.13 ml Gas / g Volatiles Destroyed...54

6.1 Effluent Fecal Coliform - MPN...64

(5)

1 1. INTRODUCTION

The Orange County (NC) Water and Sewer Authority (OWASA)

presently applies stabilized wastewater sludge to agricultural

land and desires to continue the practice. Recently proposed

federal regulations (7) will change how sludge is defined

regarding its usage for land application. OWASA sponsored this

project to investigate the applicability of thermophilic

anaerobic digestion to meet the proposed Class A sludge

requirements for pathogen destruction. As stated in the proposed

rule:

To achieve Class A reduction, the pathogenic

bacteria, viruses, protozoa and helminth ova

in the sewage sludge must be reduced to below detectable limits...An alternative

requirement is presented in the proposed rule

for Class A pathogen reduction because of the

difficulty in demonstrating that all four

types of pathogens are below detectable limits. EPA is proposing that when the

temperature of sewage sludge is raised (53

degrees Celsius for 5 days or 55 degrees

Celsius for 3 days) and the density of fecal

coliforms and fecal streptococci (enterocci)

per gram of volatile suspended solids are

each equal to or less than 100, the Class A

pathogenic reduction requirements are

achieved.

The proposed rule changes sludge classification from

technology based to performance based. Presently sludge is

classified as being treated by a "Process to Significantly Reduce

Pathogens" (PSRP), or the more effective "Process to Further

Reduce Pathogens" (PFRP) (37). The proposed federal regulations

(6)

pathogen content of the sludge. Performance requirements are

1isted in Table 1.1.

Table 1.1

Summary of Criteria Proposed by EPA for

Classification of Sludge Destined for Land Application (7)

(per gram of volatile suspended solids)

Organism Class A Class B Class C

Salmonel la spp. <.3 2 log reduction 1.5 log reduction

viruses <.1 pfu 2 log reduction 1.5 log reduction

protozoa <.1 no limit no limit

helminths 11 egg no limit no limit

Indicators^

fecal coliform 12 log,(j 16 log|Q 16.3 log,Q

fecal streptococcus 12 log,(j 16 log,Q 16.7 logjQ

This report contains an extensive literature review of

thermophilic anaerobic digestion, procedures developed to obtain

a viable thermophilic seed sludge using batch digestion, and data

on fecal coliform and fecal streptococci destruction using a

bench scale, continuous thermophilic anaerobic digester.

Criteria for indicators can be met in place of criteria for

individual pathogens. For Class A sludge, indicators can only be

used to meet criteria if a high temperature treatment process is

(7)

2. LITERATURE REVIEW

A review of the literature concerning thermophilic anaerobic

digestion of municipal sludge was conducted, and the main body of

the review attempts to present a synopsis of the advantages and

disadvantages of the process. For concise, authoritative works

on the broader subjects of sludge digestion and land application

the reader is directed:

For anaerobic digestion of municipal sludge, the review

of Parkin and Owen in 1986 with 151 references. (28)

For thermophilic anaerobic digestion - the review of

Buhr and Andrews in 1976 with 51 references. (3)

For land application of municipal sludge - A report of

the Task Committee of the American Society of Civil

Engineers in 1987 with 292 references. (39)

Operating anaerobic digesters in the thermophilic range, 45°

to 65°C, has been known to be feasible for many years. The

question is whether or not the claimed advantages - increased

rates of digestion, greater destruction of volatile solids, and

greater destruction of pathogens - outweigh the claimed

disadvantages of reduced process stability, increased heat

requirements, higher concentrations of dissolved constituents

(8)

increased odor intensity of the digested sludge (2). EPA has expressed substantial doubt that anaerobic digesters can be

operated reliably at temperatures above 49°C (37). As a result,

EPA does not include thermophilic anaerobic digestion in the list

of Processes to Further Reduce Pathogens (37). This list is

currently used as a guideline for classifying wastewater sludges destined for land application.

Few, if any, full scale plants in Europe use thermophilic anaerobic digestion for sludge stabilization (2). Review of

publications generated as part of the Commission of the European Communities activity "Treatment and Use of Organic Sludges and Liquid Agricultural Wastes" confirm that Europeans are pursuing other processes for sludge stabilization and pathogen reduction. Such processes include prepastuerization or thermophilic aerobic digestion followed by mesophilic anaerobic digestion (1,4).

2.1 FULL-SCALE, MIXED, THERMOPHILIC DIGESTION

Three, full-scale studies of mixed thermophilic digesters have been reported in the literature. The first was conducted at Los Angeles' Hyperion Plant (10,11,13); the second was done at the West-Southwest Sewage Treatment Works in Chicago (32), and the third in Elmira, Ontario (34).

In general, although each study examined many parameters,

Los Angeles was most interested in improving the dewatering

characteristics of digested sludge using thermophi1ic digestion.

(9)

existing digesters by taking advantage of the increased rate of digestion in the thermophilic temperature range.

It is interesting that in all three locations, start-up and/or operational difficulties occurred which resulted in

increased volatile acid concentrations, pH reduction and

"souring" of the digesters. However in all cases the digesters were brought back under control. Garber, at Los Angeles in 1953, increased the temperature of a mesophilic digester over a 3 month

period to 49°C while continuing to load volatile solids at a rate

of 1.65 kg m"^ d"^ (10). No operational problems occurred and he

was able to drop the temperature 5°C and return to 49° with no

upset. Loading was doubled and no problems occurred, however on

a mass basis, volatile solids destruction and gas generation may have been reduced slightly. Volatile acids increased six-fold over mesophilic digestion and were about 800 mg/1.

In 1972 Garber again reported operation of a thermophilic digester at Los Angeles (11). A mesophilic digester loaded at 1.3

kg VSS m"^ d"^ was increased in temperature at a rate of 0.56^C per

day to a final temperature of 52.2°C. At this point volatile

acids were above 4000 mg/1, the volatile acids to alkalinity

ratio was high at 1.0, pH was below 7, and gas production had

stopped. The digester was "sour". Loading was stopped and temperature maintained for 4 months, but the digester showed no

change. Temperature was reduced to 49°C and over a 3 week period

gas production and methane levels increased, volatile acids

(10)

satisfactory operation for the next 6 months at a loading rate of

1.3 kg m'^ d"^. Temperature was then increased 0.56°C per day to

53°C and souring occurred again. After returning to stable

operation again at 49°C Garber was able to operate the digester

successfully between 46 and 51°C at loading rates of 2.0 kg VSS

m"^ d"^. In 1982 Garber reported (13) that thermophilic anaerobic

digestion had been operating in Los Angeles since 1953. He

concluded that at a temperature of 49°C, a temperature

differential of less than 0.8°C must be maintained; and at 52°C

the temperature differential must be less than 0.28°C. It is this

report that probably led EPA to conclude (37) that a thermophilic

anaerobic digester cannot be successfully controlled at

temperatures above 50°C.

In 1982, Rimkus, Ryan, and Cook (32) reported on results of full scale thermophilic digestion at the West-Southwest treatment works in Chicago. They raised the temperature of a mesophilic

digester in 3°C increments by increasing the temperature O.e'^C

per day for 5 days and then allowing the digester to stabilize for an additional 2 to 3 weeks. The digester was operating at 14

days detention time. At 46°C the volatile acids increased

twelve-fold to 600 mg/1, but digestion continued to proceed

normally. With the temperature at 53°C, at the 39th week,

volatile acids increased to 2300 mg/1 and the volatile acids to

alkalinity ratio had increased to 0.3. Gas production per unit

volatile solids added decreased. During the next 7 weeks

(11)

7

acids to alkalinity ratio was 0.3. Gas production was reduced by

^5 %. The digester then stabilized and volatile acids remained

below 500 mg/1 for the duration of the 130 week study. Loading

was increased to achieve a 7 day detention time and it was

concluded that the digester could be successfully operated at

this rate between the temperatures of 51 and 54°C.

In 1977, Smart and Boyko (34) reported on extensive studies

of full scale thermophilic anaerobic digestion done in Ontario,

Canada. Although this was the most detailed report reviewed,

little information was given on startup. It is apparent though

that some problems occurred as evidenced by a high level of

volatile acids, a high volatile acid to alkalinity ratio, and

erratic gas production during startup. Loading during the

startup phase was 1.3 kg m'^ d'' volatile solids and temperature

54°C. The digester was brought under control after 20 weeks,

possibly by recirculating digested sludge from a secondary

digester, although that is not clear. Successful loading up to

3.2 kg m'^ d"' at 53°C was achieved during the study, with volatile

acids at 2400 mg/1.

All three locations were able to operate successfully at

detention times as low as 7 days. In general good mixing and

tight temperature control were required to do this. All three

locations reported slight increases in volatile solids

destruction over mesophilic digestion. On the question of

process stability, results vary somewhat. However, all locations

(12)

maintenance problems once the process had stabilized. All

locations reported somewhat different operational requirements,

mostly focusing on temperature and mixing. It should be

recognized that each location had different concentrations and

proportions of sludge feed, reactor configurations, heating

methods, mixing methods, and startup methods which would affect

operational performance. Even in Los Angeles, during the

extended use of thermophilic anaerobic digestion, feed type,

reactor configurations, heating and mixing all changed, which may

account for variations in operational control requirements as

reported by Garber (11,12,13).

All plants were able to achieve a stable process once the microbial population had been established. If desired, the detention time could be about 1/2 that of mesophilic digestion with no loss of volatile solids destruction or gas generation and quality. Pathogen destruction was greatly enhanced over

mesophilic digestion. Garber (13) reported that operating at

49°C, fecal coliform concentration was reduced to log,q3.73/1 GO

ml, a more than 3 log reduction over mesophilic digestion. Fecal

streptococcus was reported as log|Q4.15/100 ml, a more than 2 log

reduction over mesophilic digestion. Although an improvement

over mesophilic digestion, neither fecal coliform or fecal

streptococcus concentrations would meet the proposed Class A

requirement.

(13)

9

However if shorter digestion times are used, and a sludge to

sludge heat exchanger is employed to heat the incoming sludge

with the outgoing effluent, energy requirements might become

quite similar. Regarding energy usage, a great deal depends on

operating conditions, geographical location, and digester design.

Sludge liquids were reported by Garber (11) to have a 50 to 100 %

increase in ether solubles, COD, nitrogen, phosphorous and heavy

metals. The Chicago study (32) indicated a 75 % increase in

total solids in the supernatant. All three studies reported an

increase in odor intensity of the thermophilic sludge. In fact it

was reported that the primary reason the West-Southwest Plant in

Chicago did not switch to thermophilic anaerobic digestion was

concern about the odor of the sludge (8).

2.2 FULL SCALE, UNMIXED, THERMOPHILIC DIGESTION

In 1931, full-scale plant tests were run in Aurora, Illinois

comparing mesophilic to thermophilic digestion of raw sludge in

unmixed, single-stage digesters at 12 days detention time (9).

Conclusions were that slightly greater volatile matter

destruction was obtained than with mesophilic digestion, but the

supernatant was of much poorer quality. Also it was stated that

although the digested thermophilic sludge was somewhat thicker,

it was more difficult to dewater.

From 1942 to 1944 full-scale plant studies were done at

Jackson, MI (9). Mesophilic digestion was compared to

(14)

unmixed tanks in series each. Feed sludge was three parts waste

activated sludge to one part primary sludge. The first tank in

each train was heated to 29°C (mesophilic) and to 52°C

(thermophilic). The secondary and tertiary tanks were not

heated, but maintained temperature above ambient for the

mesophilic train and well above ambient for the thermophilic

train. Residence time in the primary digesters was 24 days and

the secondary and tertiary digesters had 16 days residence time

each. Results showed that thermophilic digestion produced more

gas and more volatile solids reduction than mesophilic digestion.

Also the supernatant drawn from the tertiary tank was of better

quality with thermophilic digestion. The mesophilic train was

then shut down, and the loading on the thermophilic train

effectively doubled. Temperature of the thermophilic primary

digester was set at 56°C. Gas generation and volatile solids

reduction, at the higher rate, were equivalent to what the

mesophilic train had produced at the lower rate. Supernatant

quality was significantly poorer than with mesophilic digestion.

The Jackson study also experimented with different heating

methods. Conventional hot water coils became encrusted with

sludge and corroded at thermophilic temperatures. Aspiration of

hot gases directly into the sludge was tried, but rejected

because of odors escaping with venting gas. Steam injection

directly into the sludge was selected as a satisfactory method of

heating. The amount of water vapor in the gas at thermophilic

(15)

2.3 THERMOPHILIC DIGESTION IN MOSCOW, U.S.S.R. (31)

Since 1934 laboratory investigations of thermophilic

digestion have been carried out in the U.S.S.R. Since 1958, eight

full-scale digesters of 5200 M^ each have operated at 51°C with a

residence time of 9 days. The digesters operate in two stages in

the thermophilic range with continuous loading of sludge. It was

reported that no viable eggs of helminths were found in the

digested sludge. Heating was by steam injection. Mixing was

deemed to be very important. As of 1977 (3), Moscow continued to

operate sludge digestion thermophi1ically.

2.4 EARLY LABORATORY EXPERIMENTS

Much of the early work in thermophilic digestion focused on

developing a thermophi1ically digesting sludge starting from

either ambient or higher mesophilic temperatures. In 1930

Heukelekein showed that when primary sludge was incubated with

ambient digested sludge in a batch reactor at 45 to 60°C, there

was a prolonged period with no gasification. However once

gasification commenced, it proceeded at a rapid rate. The total

time of digestion was 25 to 30 days. By then using the sludge

produced under these thermophilic conditions for the seed, total

time of digestion was reduced to 18 to 20 days (17). Later in the

same year, Heukelekian varied the ratio of thermophilic seed to

primary solids in a batch reactor (18). Results showed that

increasing the ratio of sludge to seed increased digestion time.

(16)

volatile solids basis, and 44 days for an 11.4:1 ratio. The

effect of added buffers (lime, ammonium carbonate, ammonium

bicarbonate, and dipotassium phosphate) on sludge digestion time

was also evaluated. With the buffers, digestion time was not

dependant on sludge to seed ratio, up to a ratio of 8:1. In

fact, in all cases digestion time was less than the 12 days

achieved in the 2:1 ratio which had no buffers. This study also

looked at the effect of temperature on gas generation rate. It

was determined that 55°C appeared optimum, with a sharp reduction

in rate at temperatures over 60°C.

In 1932 Heukelekian studied the effects of environmental

conditions on the seeding properties of thermophilic seed sludge

(20). He determined that the degree of digestion of seed sludge

affected the digestion time of mixtures made from it. Sludge as

seed from batch reactors performed best when 90 to 95% of the

total gas had been produced. Storage of thermophilic sludge up

to three months did not cause deterioration in its seeding value,

regardless of whether the sludge was stored at SO^C. or 20°C.

Storing sludge digested at 20°C for 40 days at 50°C decreased the

time required to complete the digestion of a mixture of seed

sludge and primary sludge from 37 to 20 days.

Heukelekian also studied adaptation and acclimation

requirements for a sludge to give efficient digestion in a range

between 28 and 42°C (21). In batch studies he found that when

sludge was digested using a seed from a 20°C digester, the time

(17)

increased. However when that digested sludge was used as the

seed for another digestion at the same temperature, the time

required for digestion was shortened. It appears, therefore,

that the larger the difference between the temperature at which a

sludge was produced and the temperature at which it will be used

for digestion, the greater will be the initial retardation and

the greater will be the benefit of re-use of the sludge.

Heukelekian's work showed that it is imperative not to draw any

conclusions from digestion at different temperatures without

preliminary acclimation of the sludge.

In 1937 Fair and Moore (6) concluded that the optimum

temperature for sludge digestion in the mesophilic range was

37°C, and 53°C in the thermophilic range. At the thermophilic

temperature, time of digestion was less than half that at the

mesophilic temperature.

2.5 EXPERIMENTATION IN THE 50'S AND 60'S

Golueke, in laboratory experiments, studied the effect of

temperature on digesters fed once per day (14). Sludge was

acclimated at temperatures from 30 to 65°C. after which digesters

were operated at a detention time of 30 days and solids loading

of 0.13 kg VSS M"^ d" . Mixing was done once per day. Digesters

operating from 30 to 40°C began producing gas immediately. Seven

day acclimation was required for a 45°C digester, and 21 days for

50 to 65°C digesters. Volatile matter destruction was 40% at

(18)

65°C. Gas production tracked volatile solids destruction.

Volatile acids increased with temperature and a dramatic increase

was observed from 500 mg/1 at 50°C to 2000 mg/1 at 55°C.

Chromatographic analysis of the acids indicated the same

concentration ratios of acid type regardless of digestion

temperature. All the sludges had the same blackish color, gritty

texture and tarry odor. Some equipment problems resulted in

short term temperature reductions of 5 to 10 degrees lasting

several hours; in all cases this resulted in sharp reductions in

volatile solids destruction. Apparently once temperature was

re-established, digestion proceeded as before.

Digestion failure, brought on by a gradual increase in

organic loading, was studied by Pohland and Bloodworth in

1963 (30). Experiments ranging in length up to nearly one year

were carried out at 36, 52 and 60°C. Extensive data were

collected and reported, particularly relating to digestion

"souring" (which the authors referred to as retardation and

severe retardation). Unfortunately, it is apparent that the

tests in the thermophilic ranges were hampered by not starting

with an acclimated seed. Therefore even at the beginning of the

experiment, at the lowest organic loading, digestion was

retarded. As expected, upon retardation volatile acid

concentration increased. However the study also demonstrated

that the relative quantities of individual volatile acids changed

considerably, depending primarily on the degree of inhibition of

(19)

digestion, butyric increased somewhat, and propionic

concentration increased the most. Therefore the mechanism of

degradation of propionic acid to either gas or lower molecular

weight acids was affected to the greatest degree by adverse

environmental conditions.

2.6 RECENT LABORATORY STUDIES

Ghosh extensively studied single and two-phase anaerobic

digestion at both mesophilic and thermophilic temperatures (15).

The two-phase experiments examined the effect of separating the

acid and methanogenic phases of digestion by using two reactors

in series. Residence times were 1 to 2 days for the acid phase

and 2 to 13 days for the methane phase. Experiments were

performed with the reactors operating in several temperature

combinations, with a mesophilic temperature of 35°C and a

thermophilic temperature of 55°C. Comparison was made to single

stage digesters operating at the same loading rates, residence

times and temperatures. Conclusions were that two-phase anaerobic

digestion stabilized municipal sludge at higher efficiencies than

single stage digestion.

Unfortunately, the study was flawed in several ways, some of

which were pointed out by Pfeffer (29). It was noted by Ghosh

that thermophilic digestion was inhibited for reasons he

attributed to inhibition of acetogenic bacteria and acetate

(20)

7.5, was likely to be inhibitory at 55°C. After review of the

experimental details, it is possible that the thermophilic

inoculum was not well acclimated. Therefore the only true

comparisons that can be made among Ghosh's results are between

two-phase and single stage mesophilic digestion. One interesting

result of the study was the much higher concentrations of

isovaleric and caproic acids found in the thermophilic digesters

compared to the mesophilic reactors. These acids are known to

have more unpleasant odors then the lower aliphatic acids

(formic, acetic) (27).

Lee et al repeated much of the work of Ghosh with greater

success, and in addition examined pathogen destruction (24).

Feed was a 2:1 mixture of waste activated and primary sludge.

Reactors were operated on a draw and fill mode every eight hours.

Digester temperatures of 35° and 53°C. were investigated. Single

stage digesters were operated at detention times of 10 and 20

days. Two-phase digesters were operated at 1 day in the acid

phase and 9 or 19 days in the methanogenic phase. Low volatile

acids to alkalinity ratios indicated that all digestions ran

well. Contrary to Ghosh's results, it was found that volatile

solids reduction in the single stage digesters were essentially

the same as in the two-phase digesters for both mesophilic and

thermophilic conditions. Gas generation was not reported. At 20

day detention times, slightly more volatile solids destruction

occurred than at 10 days.

2

(21)

Three indicator bacteria and one virus were chosen for

determination of pathogen destruction. They were fecal coliform,

Escherichia coli, fecal streptococcus and enterovirus. Ascaris

ova die-off was determined in batch tests for helminth

destruction rates. For mesophilic operation, two-phase digestion

increased the log bacterial reduction by 0.5 for fecal

streptococcus and by 0.91 for fecal coliform compared to single

stage at 20 days residence time. However, no additional

reduction in viruses were observed with two-phase mesophilic

digestion vs. single stage. Under mesophilic conditions, virus

destruction was 60% greater with 20 day than with 10 day

residence time. Thermophilic operation frequently resulted in

reduction of bacteria and viruses below detection limits

(discussed further below). Acid phase digestion alone resulted

in more than 4 log reduction in fecal coliform and Escherichia

coli, slightly less for fecal streptococcus. Except for one

sample, all virus determinations for thermophilic effluents were

below detectable limits, resulting in a reduction of at least 2

logs. Tests on Ascaris eggs showed that no eggs were viable

after 4 hours at 53°C.

Therefore it was determined that thermophilic anaerobic

digestion at 53°C reduces to essentially undetectable levels

indicator bacteria, enterovirus, and viable Ascaris eggs for

detention times as low as 10 days. Unfortunately, the detection

limits were set at log,QCFU/100 ml = 3.00. This is an order of

(22)

the values were above the detection limit, indications are that

the thermophilic process studied would not meet the Class A

requirement based on indicator organism destruction.

2.7 DISCUSSION

The most important requirement for a stable and efficient

anaerobic digestion process is a large and viable population of

methane producing bacteria. In order to achieve this it is

necessary to provide adequate solids detention time, good mixing,

and a proper environment. For thermophilic digestion, good

mixing and control of environment are more critical than with

mesophilic digestion, particularly for short detention times in a

thermophilic digester.

It is apparent from the literature that several researchers

were able to operate well controlled and stable thermophilic

digesters. Others, however, had problems. The reasons why some

processes were successful and others were not are not always

clear. It is also not always clear why some operations required

a particular controlled environment while others had more

options. For instance in 1954 Garber reported he was able to

operate a digester at 49°C successfully while allowing the

temperature to vary by as much as 5°C within 48 hrs. In 1982,

however, he required temperature control within +,-0.8° at 49°C.

Some parameters had changed such as methods of mixing and

heating, and undoubtedly there were other differences not noted

(23)

The initial requirement for a stable and efficient

population of thermophilic bacteria is the development of that

population. Two methods have been employed. The first, favored

by operators of plant size digesters, is to increase the

temperature of the digester gradually until the desired

temperature is reached. Careful monitoring of control parameters

is required to insure the methane producers are not inhibited and

washed out. The second method is to mix a portion of digesting

sludge with fresh sludge in a batch reactor and increase the

temperature immediately to the desired point. Digestion begins

after a period of acclimation, reaches a peak, and then falls off

as the biodegradable solids are consumed. It has been shown that

when this sludge is then used as seed for the next digestion, the

acclimation period is greatly reduced, and is optimum by the

third batch.

It is fairly well agreed that thermophilic sludge digestion

is carried out by anaerobes that have optimal growth temperatures

in the thermophilic range. It has been shown in batch studies

that if a reactor operating well in the thermophilic range is

suddenly dropped in temperature down to the mesophilic range and

maintained there, digestion will essentially cease for at least 3

months. This would indicate that digestion was being carried out

by facultative thermophiles that grow extremely slowly in the

mesophilic range, and that microorganisms with optimal growth

(24)

As noted above, there are two approaches to thermophilic

reactor startup. One school of thought believes that by

increasing the temperature quickly, some thermophiles might be

killed off that would otherwise be nurtured along with gradual

temperature increases. Another belief is that the long and slow

process of increasing the temperature in small steps is fraught

with peril. Changes in loading, temperature or other

environmental parameters might sour the digester and require

essentially starting over. It is likely that different microbial

populations would predominate in the two approaches.

Raising the temperature quickly under batch conditions has a

different effect on the microbial population than slowly raising

the temperature of a continuous digester. Under batch conditions

the mesophiles would quickly die off. The facultative

thermophiles would go through a period of acclimation and would

not be washed out since there is no digester discharge. After

several days a growth phase occurs with no competition from

mesophiles. As the stationary phase is reached, gas generation

levels off. Gas generation then decreases during the endogenous

phase. It has been shown that left alone, at thermophilic

(25)

from a secondary tank can be recycled to the primary tank to

restore the thermophilic microbial population.

Another important factor is to have efficient mixing of

sludge in anaerobic digesters. If mixing is not adequate, the

process is less efficient and less stable. Amazingly, supposedly

fully mixed digesters have been shown to exhibit from 10 to 89%

dead space and from 18 to 72% short-circuiting (26). Mixing

problems reduce the effective digester size, increase temperature

differentials within the digester, reduce the contact between the

microorganisms, food and enzymes, and reduce the rate at which

products are taken away. Two of the most successful thermophilic

trials employed mechanical mixing. The Ontario full scale

digester used two turbine mixers with draft tubes (34) and the

most successful bench scale trials used a single immersed high

speed turbine in a narrow vertical cylinder (24). These trials

ran at 54° and SS^C respectively. The prevalent method of full

scale digester mixing today is by gas recirculation, in use

primarily because of the low maintenance required relative to

mechanical mixing. The evidence is circumstantial, but it should

be noted that Garber seemed to have better stability in the

1950's with his mechanically mixed digester than in the I970's

with his digester that was gas mixed (10,12). The full scale

thermophilic digester in Chicago was mixed by sludge

recirculation pumping and was claimed to be stable at 52°C and

able to handle changes in temperature of up to 3°C in 24 hours

(26)

efficient mixing should be well understood and carefully planned

for.

There have been claims and counter-claims regarding

increased volatile solids destruction and enhanced gas generation

using thermophilic digestion. It appears that any enhancement is

dependent on feed makeup and operating conditions. It can be

said with some confidence, however, that with thermophilic

digestion volatile solids reduction and gas generation should be

at least as good as with mesophilic digestion, and residence

times can be decreased substantially, perhaps by 1/2. One

problem with thermophilic digestion gas is that the vapor

pressure of water is 42 mm at 35°C and 118 mm at 55°C. Therefore

considerably more water is contained in gas from a thermophilic

digester than from a mesophilic digester. This presents

particular problems in warm climates where the water is less

likely to condense and reflux back into the digester on its own.

The definitive study to date on pathogen destruction was

done by Lee et al, at the behest of EPA (24). It should be noted

that two of the coauthors work for EPA in their Cincinnati, Ohio

laboratories and are involved in developing sludge regulations.

Lee et al concluded that "thermophilic anaerobic digestion at

53°C reduces to essentially undetectable levels indicator

bacteria, enterovirus, and viable Ascaris eggs for an SRT as low

as 10 days". Unfortunately the detection limits they set were

(27)

fecal coll form and fecal streptococcus concentrations above the

detectable limit of 1000 CFU/100 ml.

EPA did not designate thermophilic anaerobic digestion as a

PFRP because they believe the operation cannot be well controlled

above 49°C (37). This belief is based on the experiences of

Garber (11,13), but two other full scale trials have been

successfully run at above 53°C (32,34); and as discussed above,

the EPA has shown that bench scale thermophilic digestion can be

very well controlled at 53°C.

Odors are a concern with thermophi1ically digested sludge.

Malodorous sludge is perceived as poorly stabilized and possibly

harmful. If thermophilic sludge can meet Class A requirements, it

may still have an odor some people might find offensive. The

odor is probably the result of increased volatile acids

(particularly the higher aliphatic acids butyric, valeric, and

caproic) and ammonia in the sludge. Two-phase digestion greatly

reduces the volatile acids in the methane phase, which will

(28)

3. BATCH DIGESTION, DEVELOPMENT OF THERMOPHILIC POPULATION

As discussed in chapter 2, two basic methods for development

of a viable thermophilic seed sludge are found in the literature.

The method that has been used to start up full scale digesters is

to very slowly increase the digester temperature from the

mesophilie range to thermophilic, while continuing to feed

sludge. This method takes from 6 months to 1 year and is subject

to souring as documented in the literature. The second method,

as documented by Heukelekien in the 1930's, is to mix a two to

one ratio of primary sludge to mesophi1ically digested sludge on

a volatile solids basis, and immediately subject the mixture to

thermophilic temperatures under batch conditions. The second

method was employed for this project.

3.1 METHOD FOR BATCH DIGESTIONS

Mesophilie digested sludge and raw primary sludge were

obtained from the OWASA Mason Farm treatment plant. Two parts

primary sludge and one part mesophilic sludge, on a volatile

solids basis were mixed together and placed in a two liter glass

bottle which served as a batch reactor. Two grams of sodium

bicarbonate were added as a buffer. The bottle was placed in a

constant temperature water bath maintained at 55°C (+,- 0.2°).

The top of the bottle had a rubber stopper with a glass tube

inserted to allow gas to escape. Gas obtained as the digestion

proceeded was trapped and measured by displacement of an

(29)

first run was then used as seed for Run # 2, using the same 2 to

1 primary sludge to digested sludge proportions. Run # 3 used

the digested sludge from Run # 2 in the same manner. This

sequential batch digestion was used to obtain a viable

thermophilic seed sludge.

The experiment, Run # 1, to develop a thermophilic sludge

from mesophilic seed was repeated in Run # 4, except this time no

buffer was added. After the digestion was complete, the

resulting sludge was split into two aliquots. One portion of the

sludge was held at 55°C for 3 months and the other held at

ambient temperature for three months to determine if they

remained viable. These two sludges were then used as seed for

batch thermophilic digestions, once again using the 2 to 1

primary volatile solids to seed sludge volatile solids. Run # 5

used seed held at ambient temperature, and Run # 6 used seed held

at 55°C. Experimental details for each batch run are summarized

in Table 3.1.

3.2 RESULTS OF BATCH DIGESTIONS

Thermophilic digestion occurred in all runs. Results are

tabulated in Table 3.1. In the initial experiment using

mesophi1ically digested sludge as seed with a buffer added

(Run # 1), digestion began immediately. Gas production is

plotted in Figure 3.1. After digestion was complete, primary

sludge was added to a portion of the resulting thermophi1ically

(30)

Batch Digestions

RUN # I 1 I 2 3 1 4 I 5 ! 6

1

Seed 1

1

OWASA

meso

w/buffer

! from ! run # 1

1 1

from

run # 2

! OWASA 1 j meso I I no buffer!

Run 3 held @ ambient

! Run 3 1 held @ !55 deg. C Batch 1

Size (ml) 1 1600

1

! 1060

1600 ! 1200 1 596

1

! 1421 Seed vol I

(ml) ! 519 1 260 559

1 1

i 400 i

280

1

i 550

Seed % 1

solids I fixed 1 volatile | 2.12 0.83 1.29

I 2.88 1 1.38 1 1.51

2.42 1.11 1.31

1 1

i 2.38 !

! 0.91 1 ! 1.47 1

2.92 1.40 1.52

1

1 2.13 1 1.08 ! 1.05 Primary !

vol (ml) 1 1081

1

800 1041

t 1

! 800 1 316

1

871 Primary % I

solids ! fixed ! volatile j 1.75 0.54 1.21 1

i 1.86

1 0.39 1 1.47

1.62 0.40 1.22

1 1

! 1.86 ! 1 0.39 !

! 1.47 1

3.25 0.56 2.69

1

i 3.25

1 0.56 j 2.69

Total * I

Gas (ml) ! 8000

1

j 8250 8850

1 1

I 8370 i

4600

1

! 17900 Gas @ I

3 days I

(ml) !

2050

1

j 3800

1 r

5000

1 1

! 625 !

1 1 1 1

1735

1

! 1570

1 1

% of Tot 1 Gas in I

3 days j

1 1

26 %

1

j 46 %

1 1 1

56 %

1 1

! 7 % i

1 1 II

38 %

1

! 9 %

1 1 1

Days to j 90 % Gas 1 Production,' 11.6 1 1 1 8.9

1 t

! 20.0 !

1 1 1 1

9.1

1

I 19.4

I 1

Gas per | volatiles |

fed (ml/g)!

612

1

I 701

1 1

697 ! 711 1

1 1

541

1

I 764

1 1

(31)

quickly. Gas production for Run # 2 is plotted in Figure 3.2.

The sludge resulting from this digestion was then used as seed

for Run # 3. Digestion rate was slightly improved over Run # 2

and gas production is plotted in Figure 3.3. This sequence of

three digestions developed a strong, viable population of

thermophilic anaerobes which was used to seed the continuous

digester during that portion of the project.

Three other batch experiments were conducted. In Run # 4

mesophi l.ical ly digested sludge which was stored for one month at

ambient temperature, in the absence of oxygen, was used as the

seed. No buffer was added. Although several days of lag

occurred, and total time of digestion was nearly twice as long as

in Run # 1, successful thermophilic anaerobic digestion did

occur. Gas production rate for Run # 4 is shown in Figure 3.4.

Digested sludge from Run # 4 was split and one portion

stored at ambient temperature in an oxygen free atmosphere. The

other portion was stored at 55°C in an oxygen free atmosphere.

After three months storage the ambient temperature sludge was

used as seed for Run # 5, and the thermophi1ically stored sludge

was used as seed for Run # 6. Both seeds had remained viable and

digestion proceeded. Digestion proceeded more quickly with the

sludge stored at ambient temperature, but more volatiles were

destroyed with the sludge stored at thermophilic temperature.

Figures 3.5 & 3.6 show gas generation of Runs 5 & 6.

(32)

exception that a thermophilic seed sludge can be developed

readily by batch digestion, and does not appear to be killed off

by storage at ambient or thermophilic temperatures in the absence

(33)

Batch Digestion Run # 1

Mesophilic Seed

10

8

ml gas (Thousands)

Figure 3.1

Mesophilic seed Sludge from OWASA

Two to One primary sludge to seed mix

on a voiatiles basis

Batch size « 1600 ml. Temp - 55 deg. Celcius

Primary voiatiles fed = 13.08 grams

Buffered with 2 grams sodium bicarbonate

10 15

DAYS

20 25 30

(34)

Thermophilic Seed from Run # 1

10

8

6

ml gas (Thousands)

Figure 3.2

Seed taken from digested sludge of Run # 1

Two to one primary solids to seed mix

on a volatiles basis

Batch size ' 1060 ml. Temp => 55 deg Celcius

Primary volatiles fed = 11.8 grams

0 10 15

DAYS

20 25 30

CO

(35)

Thermophilic Seed from Run # 2

10

8

ml gas (Thousands)

Figure 3.3

0

Seed from digested sluge from Run #2

Two to one primary to seed sludge

on a volatiles basis

Batch size « 1600 ml. Temp > 55 deg Celcius

Primary volatiles fed

ͣ

12.7 grams

10 15

DAYS

20 25 30

(36)

Stored Mesophilic Seed, No Buffer

10

8

ml gas (Thousands)

Figure 3.4

0

Mesophilic seed from OVVASA

Stored at ambient one month

Two to one primary to seed sludge

on a volatiles basis

Batch size = 1200 ml. Temp = 55 deg Celcius

No buffer added

Primary volatiles fed » 11.8 grams

10 15

DAYS

20 25 30

00

(37)

Thermophilic Seed held at Ambient temp

ml gas (Thousands)

Figure 3.5

0

Thermophilic seed from Run # 4 held at

ambient temp, for 3 months

Two to one primary to seed sludge

on a volatiles basis

Batch size » 596 ml. Temp > 55 deg Celcius

Primary volatiles fed

ͣ

8.5 grams

0 6 8

DAYS

10 12 14

(38)

Thermophilic Seed held at 55 deg. C.

20

ml gas (Thousands)

Figure 3.6

15

10

0

Thermophilic seed sludge form Run # 4

held at 55 deg. Celcius for 3 months

Two to one primary to seed sludge

on a volatiles basis

BAtch size - 1421 ml. Temp > 55 deg. Celcius

Primary volatiles fed "> 31.9 grams

10 15

DAYS

20 25 30

(39)

4. INTERMEDIATE ALKALINITY / PARTIAL ALKALINITY RATIO (IA:PA)

Determination of alkalinity by titration to pH 4.3 is a

common measure used to monitor buffering capacity during

anaerobic digestion. However since the carbonic acid

-bicarbonate equilibrium has a pKg of 6.3 (35), it has been

suggested that a better measure of bicarbonate buffering is

titration to pH 5.75 (23). This effectively removes the impact

of volatile acids from the titration since most of them have a

pKg near 4.8 (27). It is also of great interest to monitor the

concentration of volatile acids during anaerobic digestion, since

it is well known that increases in volatile acids indicate a

relative reduction in methanogen activity, and foreshadows

digester "souring" (28). However, methods to measure volatile

acid concentrations directly in sludge are laborious and not

always performed by wastewater treatment plants.

A simple titration method has been proposed to measure the

relative concentrations of bicarbonate buffering and volatile

acid concentration (33). Titration to 5.75 is performed and

recorded as partial alkalinity (PA), then titration is continued

to 4.3 and recorded as intermediate alkalinity (lA). The ratio

of intermediate to partial alkalinity is analogous to the ratio

of volatile acids to bicarbonate alkalinity. As IA:PA increases,

the ratio of volatile acids to bicarbonate alkalinity would

increase. An experiment was conducted to show this is true.

OWASA mesophilic sludge was titrated to pH 4.3 and the IA:PA

(40)

added to match initial sludge pH) were made to sludge from the

same batch and titrated (Figure 4.1). This simulates increases in

concentration of volatile acids in the sludge. It can be seen in

Figure 4.2 that partial alkalinity, a reflection of bicarbonate

buffering, remained nearly constant. Intermediate alkalinity,

analogous to organic acid concentration, increased. It is also

important to note that total alkalinity also increased with

increasing acetic acid concentration, which is usually considered

good. However in this case the increase in total alkalinity was

was due entirely to increases in volatile acids, which are

normally associated with digester problems.

Examination of the calculated IA:PA in Figure 4.3 shows a

smooth increase as the concentration of volatile acids increased.

Since volatile acid concentrations for thermophilic digestion

have been reported in the literature from a few hundred mg/1 up

to several thousand mg/1, the IA:PA ratio was chosen as a simple

method to monitor changes in bicarbonate buffering and volatile

(41)

Titrations - Mesophilic Sludge

Additions of Acetate

Figure 4.1

Titration of 50 ml OWASA mesophilic

digeted sludge

Acetate ion added as Sodium Acetate solution

adjusted to pH 7.2 with acetic acid

Volume increase less than 1 ml

Acetate ion addition simulates

an increase in volatile acids

15 20 25

ml 0.1N HCI

— standard

'^ * 1000 mg/l Ac

+ 500 mg/l Ac

+ 2000 mg/l Ac

(42)

Alkalinity - Mesophilic Sludge

Additions of Acetate

Alkalinity (mg/l as CaC03) (Thousands)

Figure 4.2

2.5

2

Total alkalinity - titrated to pH 4.3

Partial alkalinity - titrated to pH 5.75

Intermediate alkalinity - titrated from pH 5.75 to 4.3

1

None

+500 mg/l +1000 mg/l

Additions of Acetate

+2000 mg

— Total Alk

Partial Alk

Intermediate Alk

CO

(43)

IA:PA - IVIesophilic sludge

Additions of Acetate

•1 -4

A:PA Ratio

Figure 4.3

1.1

y"

1

-y^

0.9

-"

ͣ

ͣ

y^

0.8

-. ^^^^-.-.^-^

0.7

-^^.^--^'^^'^^

0.6

r\

r-^^^

1 1 ͣ

0.5

None

+500 +1000

Additions of Acetate (mg/l)

(44)

5. OPERATION OF THE CONTINUOUS THERMOPHILIC ANAEROBIC DIGESTER

A continuous digester was placed in a temperature controlled

water bath and operated at 55°C for 41 days. Hydraulic residence

time was 10 days, and the digester was drawn then fed daily. The

digester was a three liter Pyrex bottle with a # 10 rubber

stopper in the top. Four holes were drilled in the stopper to

accommodate the feed tube, draw tube, gas discharge tube, and a

thermometer to monitor temperature. Masterflex peristaltic pumps

were used for both draw and feed. Gas was collected in a

calibrated tube with three liter capacity, displacing an

acidified (pH < 4.3) saturated NaCl solution. The water bath was

set for 57°C since this temperature was determined to achieve an

average 55.5°C in the digester. The water level in the bath was

maintained approximately one inch higher than the level within

the digester at all times. Figure 5.1 is a schematic of the

equipment.

5.1 METHOD

Each day, at about the same time, the following procedure

was performed. Temperature of the bath was measured.

Temperature within the digester was recorded. The digester was

well mixed, swirling it by hand, and the temperature within the

digester recorded again. Two hundred ml of sludge were drawn

from the digester. Fifty ml of this drawn sludge was titrated

with 0.1 N HCl to pH 4.3 and the full titration curve recorded.

(45)

#^

#k

•^

Figure 5.1 Continuous Digester

^

1. 2. 3. 4. 5. 6. 7. 8. 9. 10, 11

205 ml graduated cylinder - feed Pump tubing. Masterflex 64 04-18

Masterflex pumps, Model # 7520-35, head # 7018-00

3 liter borosilicate bottle w/#10 rubber stofiper

3/8" OD X 1/4" ID rigid polethylene tubing, feed and draw

5 mm glass tubing, 18" long

0-100 C thermometer w/0.1^ divisions

Gas tubing, Tygon S-50-HL Class VI

Calibrated gas trap bottle, Bellco 7730-38440, 3 liter 3 liter aspirator bottle, acidified salt solution storage Temperature controlled water bath, GCA Precision Model 66850

(46)

Methods 209A and 209D (36). One hundred m1 of sludge from the

OWASA fermentation digester were mixed with 150 ml of waste

activated sludge. This matches the approximate proportions

normally fed to OWASA mesophilic digestion. The mixture was

warmed to about 45°C. Two hundred ml of this mixture were fed to

the thermophilic digester, after purging the feed line of

residual sludge. The digester was mixed, swirling by hand.

Feed sludge from OWASA was obtained every three days,

measured for solids by methods identified above, and stored at

4°C for the next two days feed. Feed was changed every 3 days,

except during the indicator organism destruction runs where feed

was constant over 5 days. Gas volume generated each day was

measured by lifting the calibrated gas trap tube to equilibrate

pressure with the digester, and recording the amount of liquid

that had been displaced. Gas was then discharged to zero the

calibrated tube. Some of the discharged gas was burned over a

bunsen burner to make sure it burned as expected for a gas with a

large proportion of methane.

5.2 RESULTS

Figures 5.2 through 5.13 show continuous digestion operating

conditions. Initially the continuous digester contained 1.8

liters of thermophi1ically digested sludge obtained from the

batch digestions. Total and volatile solids were rather low at

1.45 and 0.8% respectively. Feeding began on day 1, and the draw

(47)

2

1.5

continuous digestion - 10 day HRT

Weight % '^'Qure 6.2

0.5

-^

-^^-^M^

«^«*********V« /***>*

*---•---

ͣ

---''^^^ ^---'---'---""^ ^'---'---^- TJf-Nf-*

^1f-»^A—"• • • ^^ ~^\.

ͣ

.***^ ***t

/-+-+-^^^^^^^V,y^^'~^^^

J_______ I____________I_____________1____________L 0 6 10 15 20 25 30 35 40

DAT

-^ WAS -^FERMENTED ~*-TOTAL

(48)

continuous digestion - 10 day HRT

Weight %

Figure 5.3

^e^^^

ttY

*^le

\

f^ t ͣ» t

/ V^Mk ./H^y «

*-^

ͣ

^ ͣ*-*

V*^

^^....v^

y,-^ -*—\

N_*.

.^^-^^

-|_-(-H^H-+

V-M-^-+

Vh-/ \-f-/

-M-S

\

4-f-10 15 20 25

DAY

30 35 40

WAS

FERMENTED —<^ TOTAL

(49)

5

continuous digestion - 10 day HRT

Weight % ^*9"^^ ^-^

-*-M-r"^^

f-*-*-,^

^-^^Z"*"*^"*"^' V-^_____^—X,

2 h

0 5 10 15 20 25 30 36 40

DAY

(50)

continuous digestion - 10 day HRT

Weight %

Figure 5.5

0

.*.-_.^-"-*--^.-.-.^-^

^ 3f-^

/

-^M^

-*-*-ͣ

*- t t ')(:

-k

N I I I I l-t-l I'

I I I I I t^-H-K^ . .>H-4-

ͣ^

ͣ

N-I,. ... I J_________________L

5 10 15 20

DAY

25 30 35 40

(51)

continuous digestion - 10 day HRT

Weight %

Figure 5.6

1.5

1

0.5

0

_ͣ—•—»_

^^I^^^-^Nm^-*

xj^-4HSj^-^iHS|f-^

+^H^^^

0 10 16 20

DAY

25 30 35 40

(52)

continuous digestion - 10 day HRT

Figure 5.7

(53)

continuous digestion - 10 day HRT

mg/l as CaC03 (Thousands)

Figure 5.8

„a---B_—•-\

v^

^

/

-M-M-^-^-^

Total alkalinity - titrate to pH 4.3

L/+^.

Partial alkalinity - titrate to Ph 5.75

^ HHH^^ir*--*-*-^!^,^,^^^.

Intermediate alkalinity - titrate between pH 5.75 and 4.3

0

10 15

20

DAY

25 30 35 40

^~ Total alk -+- Partial alk -*— Intermediate alk

(54)

Intermediate : Partial Alkalinity

continuous digestion - 10 day HRT

0.65

Ratio

0.56

0.45

0.35

0 10 15 20

DAY

Figure 5.9

25 30 35 40

(55)

continuous digestion - 10 day HRT

ml gas per day (Thousands)

Figure 5.10

(56)

continuous digestion - 10 day HRT

100

ml gas (Thousands)

Figure 6.11

(57)

Fraction volatiles destroyed

continuous digestion - 10 day HRT

fraction volatiles destroyed

Figure 5.12

(58)

ml gas / gram volatiles destroyed

continuous digestion - 10 day HRT

(59)

generation was 1800 ml/day which was in the lower range of gas production achieved throughout the study. Examination of the

IA:PA ratio indicated a slight increase in volatile acid concentration during the first 3 days of operation. This

corresponds to a slight drop in pH over the same period. Volatile

solids destruction reached a stable value of approximately 43%

within 3 days. Day 3 is the point where the digester began

performing in an obviously well controlled manner. Steady-state

was not achieved until much later simply because the

concentration of solids in the feed was much higher than the initial seed concentration of the digester. Two to three residence times were required to bring the digester solids concentrations up to steady-state conditions.

Throughout the 41 day study, pH was remarkably consistent

and after 2 residence times was 7.52 (+,-0.03). The IA:PA ratio stayed below 0.45 and no major changes were noted in the

titration curves. Gas production ranged between 1800 and 2500 ml/day with no obvious reason for the variation. Gas production

is better illustrated as cumulative production, and is shown to be consistent in Figure 5.11. Gas produced per gram volatiles destroyed was approximately 900 ml/g. Total alkalinity (titrate to pH = 4.3) was consistent throughout the run at slightly over

3500 mg/1 as CaCOj. Partial alkalinity (titrate to pH = 5.75), a

reflection of bicarbonate ion buffering, was consistent at about

(60)

also consistent at about 1100 mg/1 as CaC03. Temperature of the

water bath remained constantly at 57°C (+,-0.2°). Since the

digester was not being continuously mixed, some temperature variation occurred within the digester. Each day, prior to

mixing, temperature in the center of the digester was 54.5°C

(+,-0.3°). After mixing the temperature was 55.6°C (+,-0.4°). At the

wall of the digester, prior to mixing, it can be assumed that the

temperature was close to the water bath temperature of 57°C.

Therefore on a daily basis there were temperature variations

within the digester totaling about 2.5°C, which did not impede

successful operation of the continuous digester. No correlation

was noted between temperature variation and gas production.

It appears that volatile solids were being destroyed at high rates during the first two days of operation, but little gas was

generated. This accounts for the more than 10 days it took for calculated cumulative gas generated/volatiles destroyed to get over the 800 ml/g mark. It is possible that in the initial two days volatiles were being destroyed to make volatile acids, but also questionable was the method used to remove effluent during these first two days. The method may have artificially lowered the volatile solids concentration in the sample (i.e. the

digester may not have been well mixed, and the effluent contained

(61)

To summarize, a continuous thermophilic anaerobic digester was operated, in a well controlled manner, at 10 days residence

time and 55°C, for 40 days, using OWASA sludge as feed. Volatile

solids destruction and gas production per volatile solids

destroyed were well within the rule-of-thumb limits taken from Metcalf & Eddy (25). Volatile solids destruction was somewhat

(62)

: After Three HRT's of

Continuous Digestion

MEAN

STANDARD

DEVIATION

RANGE

MIN MAX

PH 7.53 0.02 7.49 7.57

Alkalinities (mg/l as CaC03)

TA (4.3)= 3525 44 3480 3630

PA (5.75)= 2413 38 2370 2520

IA= 1113 40 1060 1200

IA:PA= 0.46 0.02 0.42 0.49

EFFLUENT DRAWN %

Total solids 2.45 0.05 2.37 2.56

Fixed solids 0.97 0.02 0.93 1.01

Volatile solids 1.49 0.03 1.42 1.55

FEED (g)

WASTE ACTIVATED SLUDGE

Total solids 4.09 0.18 3.91 4.33

Fixed solids 1.18 0.03 1.14 1.22

Volatile solids 2.91 0.15 2.77 3.11

FERMENTED SLUDGE

Total solids 2.90 0.59 2.17 3.55

Fixed solids 0.55 0.17 0.34 0.74

Volatile solids 2.35 0.42 1.84 2.82

TOTAL FEED %

WASTE ACTIVATED SLUDGE Total solids

Fixed solids

Volatile solids

FERMENTED SLUDGE

Total solids Fixed solids Volatile solids

COMBINED FEED %

Total solids Fixed solids Volatile solids

2.46 0.11 2.35 2.60

0.71 0.02 0.68 0.73

1.75 0.09 1.66 1.87

1.16 0.24 0.87 1.42

0.22 0.07 0.14 0.30

0.94 0.17 0.74 1.13

3.61 0.34 3.21 4.02

0.93 0.09 0.82 1.03

2.69 0.25 2.40 2.99

Gas/day (ml) 2209 287 1850 2750

Fraction Volatile solids (vs)

Destroyed 0.44 0.00 0.43 0.44

gas/vs destroyed (ml/g)

gas/vs fed (ml/g)

902 393

7 2

894 390

Figure

Figure 5.1 Continuous Digester

References

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