Gas Characterization, Microbiological
Analysis, and Disposal of Refuse in GRI
(Gas Research Institute) Landfill Simulators
Cincinnati Univ., OH
PB86-179504
Prepared for
Environmental Protection Agency, Cincinnati, OH
Apr 86
, •>
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PC 86- V7950<4
EPA/600/2-86/041
April 1986
GAS CHARACTERIZATION, MICROBIOLOGICAL ANALYSIS,
AND DISPOSAL OF REFUSE IN GRI LANDFILL SIMULATORS
by
Riley N. Kinman, Janet Rickabaugh,
David Nutini, and Martha Lambert
Department of Civil and Environmental Engineering
University of Cincinnati
Cincinnati, Ohio 45221
Contract No. 68-03-3210-12
Project Officer
Joseph K. Burkart
Land Pollution Control Division
Hazardous Waste Engineering Research Laboratory
Cincinnati, Ohio 45268
HAZARDOUS WASTE ENGINEERING RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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TECHNICAL REPORT DATA
(f'ltasc read Instructions on Ihc ic\cnc before cot"f!ctinFl
. REPORT NO.
b'PA/600/2-86/041
4. TITLE AND SUBTITLE
Gas Characterization, Microbiological Analysis, and
Disposal of Refuse in GRI Landfill Simulators
5 REPORT DATE
April 1986
6. PERFORMING ORGANIZATION CODE
. AUTHORISI ~~
Riley N. Kin.nan, Janet Rickabaugh, David Nutini,
and Martha Lambert
6. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
University of Cincinnati
Department of Civil and Environmental Engineering
Cincinnati, Ohio 45221
10. PROGRAM ELEMENT NO.
BRDIA
11. CONTRACT/GRANT NO
68-03-3210 WA £12
12. SPONSORING AGENCY NAME AND ADDRESS
Hazardous Waste Engineering Research Laboratory
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
13. TYPE OF RE PORT AND PERIOD COVERED
Final
14. SPONSOF..NG AGENCY CODE
EPA/600/14
15. SUPPLEMENTARY NOTES
Project Officer: Joseph K. Burkart
16. ABSTRACT
This report describes the termination of a five-year pilot-scale project that
evaluated methane production and gas enhancement techniques in sanitary landfills.
Sixteen simulated landfills were constructed in 1980 and operated until January 1985.
Data collected during this termination study consisted of characterization of the
trace volatile constituents of the gas generated by the experimental landfills and
microbiological analysis of the refuse.
This work WuS submitted in fulfillment of Contract 68-03-3210-12 by the
University of Cincinnati under sponsorship of the U.S. Environmental Protection
Agency. This report covers a period from May 1985 through September 1985.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b. IDENTIFIERS/OPEN ENDED TERMS
COSATI I i
18. DISTRIBUTION STATEMENT
19 SECunn Y CLASS i7h,s
UNCLASSIFIED
21. NO. OF F A&fcS
95
UNCLASSIFIED
20 SECURITY CLASS (This paft]
UNCLASSIFIED
EP» Form 2220.1 (R.«. <-77) PHEVIOUJ EDI TION i 5 OBSOLE T E
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DISCLAIMER
The information in this document has been funded wholly or in part by
the United States Environmental Protection Agency under Contract 68-03-3210-12
with the University of Cincinnati. It has been subject to the Agency's peer
and administrative review, and it has been approved for publication as an EPA
document.
Mention of trade names or commercial products does not constitute en-
dorsement or recommendation for use.
11
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FOREWORD
Today's rapidly developing and changing technologies ar.d industrial
products and practices frequently carry with them the increased generation of
solid and hazardous wastes. These materials, if improperly dealt with,
can threaten both public health and the environment. Abandoned waste sites
and accidental releases of toxic and hazardous substances to the environment
also have important environmental and public health implications.
The Hazardous Waste Engineering Research Laboratory assists in providing
an authoritative and defensible engineering basis for assessing and solving
these problems. Its products support-the policies, programs, and regulations
of the Environmental Protection Agency, the permitting and otner responsi-
bilities of state and local governments, and the needs of bcth large and
small businesses in handling their wastes responsibly and economically.
This report describes the microbiology of the refuse in ten experimental
landfills that were part of a five-year gas enhancement project. This report
also describes the trace constituents of the gas produced by the lysimeters
after five years. This information will be useful to individuals pursuing
municipal landfill gas utilization, as well as. the engineers end government
officials involved in landfill operation and land reclamation.
For further information, please contact the Land Pollution Control
Division of the Hazardous Waste Engineering Research Laboratory.
William A. Cawley
Acting Laboratory Director
Hazardous Waste Engineering
Research Laboratory
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ABSTRACT
This report describes the termination of a five-year, pilot-scale pro-
ject that evaluated methane production and gas enhancement techniques in
sanitary landfills. Sixteen simulated landfills were constructed in 1980 and
operated until January 198b. Data collected during this termination study
consisted of characterization of the trace volatile constituents of the gas
generated by the experimental landfills and microbiological analysis of the
refuse.
The trace volatile organic compounds were found in higher concentrations
than previously reported in the literature. Xylenes, ethylbenzene, methylene
chloride, toluene, and benzene were found in all of the gas samples analyzed.
Xylenes were found in greatest concentrations of the trace compounds analyzed
ranging from 12 mg/m^ to 500 mg/m^. The levels and types of trace organics
found in the gas indicate that landfill gas could be potentially corrosive and
may contain toxic levels of some compounds.
All samples had relatively high aerobic and anaerobic plate counts,
Clostridium perfringens, and fungi levels. These same samples indicated
relatively low levelsof total coliforms, fecal coliforms, fecal strepto-
cocci, and gram negative rods. Relative numbers and types of microorganisms
seemed to reflect the enhancement technique applied to the cell. For example,
microorganism levels were generally lower in cells that received leachate
recycle as an enhancement technique. The highest level of microorganisms
were found in a cell which had a sewage sludge enhancement.
This work was submitted in fulfillment of Contract 68-03-3210-12 by the
University of Cincinnati under sponsorship of the U.S. Environmental Protec-
tion Agency. This reports covers a period from May 1985 through September
1985.
IV
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TABLE OF CONTENTS
Foreword iii
Abstract i v
Figures vi
Plates vi i
Tables vi i i
Acknowledgment , ix
1. Introduction 1
Background 1
Purpose 4
Objectives/Work Approach 4
2. Conclusions 9
3. Recommendations 11
4. Procedures 12
Prel i mi nary 12
Safety 1 '
Test Cell Content Removal' 1~
Sampling 13
Methods of Analysis 17
5. Data and Discussion 21
GC/MS Analysis of Gas 21
Microbiology of Refuse.. 31
Evaluation of Wastes 42
References - .43
Bibliography 44
Appendices
A. Log of Lysimeter Findings 46
B. Micro Media and Reagents 73
C. Quality Assurance 76
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FIGURES
Number Rage
1. Test cell cross section . 2
2. Test cell location plan 3
3. VOC sampling assembly 14
4. Trace VOC concentrations: dichloromethane ana freon 26
5. Trace VCC concentrations: dichloroethylene,
trichloroethylene, and tetrachloroethylene 27
6. Trace VOC concentrations: pentane and tetrahydrofuran 28
7. Trace VOC concentrations: hexane and propylbenzene 29
8. Trace VOC concentrations: benzene, toluene, and
ethyl benzene 30
9. Trace VOC concentrations: xylenes and carbon disulfide... .31
10. Group 1 organisms: fungi and Clostridium perfringens 34
11. Group 2 organisms: fecal streptococci, clostridia, and
gram negative rods 38
12. Methane bacteria after 60-day incubation 41
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PLATES
Number Page
1. Truckload of coarse ground refuse 16
2. First one-foot lift of refuse compacted ir. test cell 16
VI 1
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TABLES
Number Page
1. Refuse physical composition 4
2. Enhancement techniques 5
3. Target volatile organic compounds 6
4. Cells selected for gas characterization and microbiological
analyses 7
5. Analysis summary and final test cell disposition 8
6. Microbial sample depths 17
7. Media and incubation conditions 20
8. Trace VOC concentrations in blanks 23
9. Trace VOC concentrations, (cells 21, 22, 23) 24
10. Trace VOC concentrations (cells 33 and 35) 25
11. Microbiological sample moisture contents 32
12. Group 1 microorganisms (SPC, CP, Fungi) 35
13. Mean leachate volatile acids, 1984 36
14. 1984 cumulative gas production rates 37
15. Group 2 microorganisms (fungi and Clostridium perfringens)..39
16. Group 2 microorganisms (fecal streptococci, clostridia,
and gram negative rods ~. , 40
vi n
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ACKNOWLEDGMENT
The authors would like to extend their appreciation to those people who
have contributed to this work through their guidance, work effort, and pa-
tience.
A special thanks is given to Joseph Burkart, the project officer, and to
Herbert Pahren, both of the U.S. EPA.
From the University of Cincinnati, the analyst staff and support person-
nel consisted of Susan Pierce, Sam Hayes, Annette DeHaviland, Regina White
and Kevin Frank, the microbiology staff; Bob Mackey, gas sampling; Mildred
Somme, laboratory analyses; and Pat Miller, the Q.A. and procurement officer.
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SECTION 1
INTRODUCTION
This report describes the termination of a five-year, pilot-scale sani-
tary landfill project that evaluated methane production and gas enhancement
techniques in sanitary landfills. The project was housed at the U.S. EPA
Center Hill Solid and Hazardous Waste Research Facility in Cincinnati, Ohio,
but was funded by the Department of Energy (DOE) from February 1980 through
.January 1982, by the University of Cincinnati from February 1982 through
January 1983, and then by the Gas Research Institute (GRI) from February 1983
through April 1985. The termination of the study, which this report de-
scribes, was performed for the U.S EPA oy the University of Cincinnati,
Department of Civil and Environmental Engineering. A final report describing
the results of the five-year gas enhancement study has recently been published
and is available from the Gas Research Institute.1
BACKGROUND
In January 1980, sixtef-n laboratory-scale lysimeters were loaded with
shredded municipal refuse. Each lysimeter was consi-.ucted of steel six feet
(1.83m) high by three feet (0.91m) in diameter and designed to contain one
cubic yard of shredded refuse. The inside steel walls were coated with coal
tar epoxy to prevent corrosion. The lysimeters were set on concrete blocks
to allow convenient access co the leachate drainage systems. A cross section
of the test lysimeters can be seen in Figure 1. Detailed information on the
design and construction of the lysimeters is available in the literature1>^.
The cells were loaded with refuse in a series of one-foot lifts. Table
1 describes the refuse composition as determined from handsorting the refuse
prior to shredding. Gravel was placed at the bottom and top layers to assist
in drainage and in moisture distribution. Complete leachate drainage and gas
monitoring systems were installed as shown in Figure 1. Lysimeter covers were
welded shut and sealed to ensure the eel Is were gastight, as wel 1 as leachate-
tight.
The test lysimeters were located :n the high bay area of the Center Hill
facility, where controlled conditions were monitored at all tiires (Figure 2).
Cells were numbered consecutively from 20 to 35. The enhancement techniques
investigated included rcnsture addition, elevation cf temperature, leachate
recycle, sewage sludge addition, buffer addition, and nutrient addition.
Several years into the study, the cells were reloaded with different or
additional enhancements. Cells were originally paired, each pair receiving
the same enhancement technique. When cells were reloaded, half of the cells
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Figure 1. Test Cell Cross Section
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? Facility High Bay
3 6 3,4 3.3 3 2
2,6 2 7 2.8 V-^V>^V
bod 29 30 31
2 5 Q 23 22^20
24O o^ bo21
Temporary Shed
Office Wing
Figure 2. Test Cell Location Plan
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TABLE 1. REFUSE PHYSICAL COMPOSITION
COMPONENT
Paper
Food Waste
Fines*
Plastic
Glass
Ferrous Metal
Textiles
Garden Waste
Wood
Diapers
Non-Ferrous Metal
.Ash-Rock-Dirt
Rubber-Leather
PERCENT
(Wet Weight
51,70
7.23
6.99
6.79
5.96
5.15
4.74
3.66
3.00
2.23
1.37
0.67
0.54
*Material passing through a ?5mm (1 inch)
sieve
received no change in order to maintain a control for the reloaded cells and
to continue with the original project, started in 1980. Table 2 summarizes
the enhancement t?chniques applied to each of the test lysimeters throughout
the study.
PURPOSE
. The purpose of this lysimeter performance study was to characterize the
quality of the gas produced in specific selected cells, evaluate the number
and groups of active organisms within the municipal solid waste, and to dis-
pose of the contents of the cells which were opened. Six of the sixteen
cells were not opened and remain active for a lime injection/gas production
prevention study.
WORK APPROACH
In order to evaluate the test lysimeters as describod, specific objec-
tives were established. There were three main objectives, or tasks, involved
with this project: 1) gas characterization, 2) microbiological analyses, and
3) cell contents disposal.
The specific cells selected for each task, as well as the detailed work
approach employed, are described below.
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TABLE 2. ENHANCEMENT TECHNIQUES
TEST
CELL
ENHANCEMENT TECHNIQUE
Feb.'80 - Jan.'82
ENHANCEMENT TECHNIQUE
Feb.'83 - Jan.'85
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
Low Infiltration
Low Infiltration
High Infiltration
High Infiltration
High Infiltration, Leachate Recycle
High Infiltration, Leachate Recycle
High Infiltration, Leachate Recycle,
Buffer Addition
High Infiltration, Leachate Recycle,
Buffer Addition
High Infiltration, Leachate Recycle,
Nutrient Addition
High Infiltration, Leachate Recycle,
Nutrient Addition
High Infiltration, Leachate Recycle,
Buffer Addition, Nutrient Addition
High Infiltration, Leachate Recycle,
Buffer Ao cion, Nutrient Addition
Hign Infiltration, Buffer Addition
High Infiltration, Buffer Addition
High Infiltration, Nutrient Addition
High Infiltration, Nutrient Addition
No Change
Increase Moisture Content
No Change
No Change
No Change
Sludge Addition
No Change
Sludge Addition
No Change
Sludge Addition
Temperature Increase
Temperature Increase
No Change
Buffer Slurry Addition
No Change
Nutrient Slurry Addition
Gas Characterization
The five-year gas enhancement project collected large volumes of data on
overall gas composition. Gas samples were monitored monthly for percentage
of 02, N2, C02, and CH4- There was no attempt to analyze the trace consti-
tuents of the gas. Taole 3 lists twenty volatile organic compounds (VOC)
which have been repeatedly observed in landfill gas and which are considered
to be characteristic trace components at full-scale landfill sites. These
VOCs were selected for further investigation during thij lysimeter termina-
tion study and consisted of some priority pollutant compounds, known car-
cinogens, and other compounds of environmental concern. Normal alkanes
(pentane, nonane, etc.) were included to provide baseline data.
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TABLE 3. TARGET VOLATILE ORGANIC COMPOUNDS
COMPOUND NAME SYNONYM MOLECULAR WEIGHT
Pentane
Benzene
Dichloromethane
Hexane
Toluene
1 ,1-Dichloroethylene
1 ,2-Dichloroethylene
1,1-Dichloroethane
m,p-Xylene
o-Xylene
Ethyl benzene
Chlorobsnzene
Iso-Octdne
I sopropyl benzene
Propyl benzene
Naphthalene
Nonane
Trichloroethylene
1 ,1 ,2-Trichloroethane
Tetrachloroethylene
Methylene chloride
Methyl benzene
Vinylidene chloride
Monochlorobenzene
Cumeme
TCE
Vinyl trichloride
Perchluroethylene
72
78
85
86
92
97
97
99
106
106
106
113
114
120
120
128
128
131
133
166
These VOCs were selected for study because it wus felt t'nat they would
provide a characteristic neasure of the potential environmental and health
concerns associated with landfill gas recovery, utilization, and exposure.
Five of the higher gas-producing cells, (as measured by total gas volume
in January 1985) were selected for gas characterization. These cells can be
seen in Table 4. Information on the gas production from the cells can be
found in the five-year report.
Task 2: Microbiological Analyses
Microbiological analyses were performed on samples collected at two
depths from six of the sixteen test lysvneters. These six cells were
selected as representative of the various enhancement techniques used on
the sixteen cells. The six cells selected for microbiological investigations
can be seen in Table 4.
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TABLE 4. CELLS SELECTED FOR GAS CHARACTERIZATION AND MICROBIOLOGICAL ANALYSES
GAS
CHARACTERIZATION
TEST CELLS
ENHANCEMENT TECHNIQUE*
21
22
23
33
35
Control/Increase Moisture0
High Infiltration/No Change
High Infiltration/No Change1"
High Infiltration, Buffer Addition/Buffer Slurry
Addition
High Infiltration, Nutrient Addition/Nutrient Slurry
Addition
MICRO ANALYSIS
TEST CELLS
ENHANCEMENT TECHNIQUE*
20
23
25
26
30
35
Control/No Change0
High Infiltration/No Change
High Infiltration, Leachate Recycle/Sludge Addition
High Infiltration, Leachate Recycle, Buffer Addition/
No Change
High Infiltration, Leachate Recycle, Buffer Addition
Nutrient Addition/Temperature Increase
High Infiltration, Nutrient Addition/Nutrient Slurry
Addi tion
*0riginal Loading/Reloading
'-Waste spiked with benzene, toluene, and ethyl benzene
"'"Only one gas sample taken; cell emptied prior to second sampling
The microbiological studies performed included:
1. Enumeration of total het-erotrophic plate count for aerobic and anae-
robic bacteria
2. Examination of- anaerobic bacteria for methane-producing bacteria
3. Examination for and enumeration of Clostridium bacteria
7
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4. Examination and enumeration of fungi
5. Enumeration of the indicator organisms: total coliforms, fecal coli-
forms, and fecal streptococci
Cell Contents Disposal
The contents of the following ten cells were disposed of during this
study: 20, 23, 24, 25, 26, 28, 30, 31, 34, and 35. The waste from each
Iysimeter was carefully examined during th> emptying process. Each emptied
lysimeter was rinsed and cleaned in preparation for storage until needed for
a future project. Six of the sixteen test cells (21, 22, 27, 29, 32, and 33)
remain active for further evaluation as part of a lime injection/gas preven-
tion study. Table 5 summai izes the analyses performed and the final disposi-
tion of each eel 1.
TABLE 5. ANALYSIS SUMMARY AND FINAL TEST CELL DISPOSITION
TEST
CELL MICRO
20 M
21
22
23 M
24
25 M
26 M
27
28
29
30 M
31
32
33
34
35 M
GC/MS DISPOSAL LIME INJECTION STUDY
D
G L
G L
G D
D
D
D
L
D
L
D
D
L
G L
D
G D
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SECTION 2
OBSERVATIONS AND CONCLUSIONS
CELL CONTENTS
1. All test cells were in excellent condition. Seals were intact and the
cells were yastiyht. Copper fittings had a buildup of sulfide on them.
Bottom and top gravel removed from the cells was clean and in excellent
condition.
2. There was settlement in each of the lysimeters. The greatest settlement
observed was five inches, which occurred in test coll 25.
3. Only a small fraction of the total ground refuse mass was decomposed
after five years in the test cells. This fraction was believed to be
the food wastes. Refuse in test cell 25, which had received leachate
recycle and anerobically digested sludge, appeared to be the most de-
graded.
4. Artifacts were difficult to isolate and identify in the ground refuse.
However, those artifacts tnat were found documented the resistance to
biological attack of plastic, paper, rubber, leather, dyes, synthetics,
metal, plated metal, stainless steel, wood, glass, stone, and combina-
tions of these materials.
5. All of the test cells had bits and pieces of readily biodegradable
material that had been protected by the plastics and paper. Pieces of
newsprint could still be read, although biological attack was noted on
some. Cloth materials were still strong and retained their colors.
LYSIMETER GAS j
6. Trace volatile organic compounds were found in higher concentrations
than previously reported in the literature.
7. Xylenes were found in greatest concentrations as determined by GC/MS
analysis of the lysimeter gas for trace volatile organic compounds.
Concentrations ranged from 12 mg/m^ to 500 my/m^ in the gas samples
analyzed.
8. Xylenes, ethyl benzene, dichloromethane (methylene chloride), toluene,
and benzene were found in every gas sample analyzed.
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9. Concentrations of 1,1-dichloroethane, chlorobenzene, iso-octane, iso-
propylbenzene, naphthalene, nonane, and 1,1,2-trichloroethane were below
detectable limits in the gas samples from all lysimeters tested.
10. GC/MS analysis confirmed the presence of chlorinated volatile trace
organic compounds in landfill gas generated from municipal refuse.
MICROBIOLOGY
11. Relative levels and types of microorganisms found in those cells ana-
lyzed seemed to reflect the enhancement technique applied to the cell.
The highest levels and the most different types of microorganisms were
found in cell 25, which had a sludge addition enhancement, and then in
cell 35., which had a nutrient addition enhancement.
12. Microorganisms evaluated were generally lower in concentration in the
leachate recycle cells. This suggests that toxicity effects were
exerted after the leachate was recycled many times.
13. Total coliforms, fecal coliforms, and fecal streptococci were found in
the lowest levels of the microorganisms evaluated. Most of the samples
analyzed indicated no counts for these organisms at the lowest dilutions
tested.
14. There were relatively high levels of both aerobic and anaerobic patho-
genic and non-pa'thooenic microorganisms present in the refuse after five
years of disposal.
10
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SECTION 3
RECOMMENDATIONS
1. Sewage sludge should be evaluated further for methane gas enhancement in
municipal landfills.
2. Protective mechanisms which prevent readily biodegradable material from
biological attack should be evaluated.
3. Volatile organic compounds in landfill gas should be studied over a
longer time period.
4, Corrosion effects from burning landfill gas with the trace chlorinated
organic compounds should be evaluated.
5. Landfill gas combustion decomposition products should be evaluated for
their toxicity effects.
6. Leachate recycle needs further evaluation to determine at what number
of recycles the toxicity effects come into play.
7. Concentrations of VOCs observed should be evaluated as to their health
effects in processing and in use of the gas.
11
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SECTION 4
PROCEDURES
PRELIMINARY
Prior to opening any of the test cells, they were moved from the Center
Hill high bay area to a temporary shed located outside of the high bay over-
head door. The plywood shed was built for lysimeter unloading activities
from a previous project and offered a protected work area and secure storage
for the opened cells. Each cell was moved, opened, unloaded, and rinsed prior
to beginning the sequence on the next cell.
Moving Test Cells
Before the cells could be moved, all electrical probes, outer gas lines,
and gas collection baes were removed. The fiberglass insulation that sur-
rounded the cells was also removed. The cell was lifted off its cement block
supports using hydraulic jacks. Two steel I-beams were set under the cell
and run to a heavy-duty cart positioned next to the cell. The test cell was
Carefully rolled across the I-beams onto the cart. Cement blocks were repo-
sitioned under the cell, and the I-beams were removed. The cart was then
slowly rolled out of the high bay area into the temporary storage shed. The
cell remained on the cart throughout the unloading activities.
SAFETY
After the cell was in the shed it was filled with water via the water
inlet line to force methane gas from the cell. This was done to eliminate
potentially explosive levels of methane prior to cutting the lysimeter lids
off with an acetylene torch. While the lids were actually being cut, the
base of the cell was continually hosed with water to cool hot metal scrap
from the lid. A fire extinguisher was kept on hand at all times.
Protective clothing worn for the excavatior procedures consisted of
steel-toed rubber boots, coveralls, particle masks, and disposable poly-
ethylene gloves under cotton work gloves. After work each day, all clothing
was removed on-site at the decontamination station.
Portable stairs were placed next to tne cell being emptied for easy
access from the ground to the top of the cell. A step ladder was used to
actually enter or exit the cell. A wood beans with a line was placed over the
cell being emptied as an emergency evacuation aid.
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ir.. »«_ ,
TEST CELL CONTENT REMOVAL
Once the lids cf the test cells were opened, the copper probes and the
water infiltration hose and ring were disconnected and removed from the cell.
Notations were made on the conditions of these probes, the appearance of the
coarse gravel at the top of the cell, and the conditions of the tank side-
walls. The distance from the top of the cell to the top of the gravel was
measured. The water was drained from the cell through the leachate drainage
system. The gravel was removed by digging it out with a shovel and hand-
picking the remainder. The gravel was placed in containers on a skid held by
a forklift next to the cell. Once all the gravel was removed, it was trans-
ported to a dumpster on the Center Hill site. After all of the cells were
emptied, the dumpster was transported to a sanitary landfill for final dis-
posal .
When all of the gravel was removed, the distance from the top of the
lysimeter to tne top of the refuse was measured. The refuse was removed in
layers by scraping the contents with a pitch fork or cultivator. The loose
refuse was piled toward the center of the cell. The excavator would then
pick up the loose refuse by hand and place it into a trash container on a
skid set on the forklift. Once the refuse was on the skid, another person
would sort through the contents for artifacts as well as note conditions of
waste materials. Once these containers were full, they were transported to
the dumpster.
After the refuse was removed, a final measurement was made from the top
of the lysimeter to the top of the bottom gravel layer. The bottom gravel
was removed from the cell in buckets much the same as the other materials and
transported to the dumpster with the forklift. The cell was triple-rinsed
with water after all contents had been removed.
SAMPLING
Gas Sampling
The gas sampling of tha test cells for the target VOCs used absorbent
resin columns termed Tenax traps. These Tenax traps were clear glass cylin-
ders approximately 1.5 cm in diametor and 14 cm long. They were furnished by
Pedco Environmental, Incorporated (PEI), who was subcontracted to perform the
GC/MS analyses. The traps were picked up from PEI the day prior to sampling
and returned the next day immediately after sampling was completed. The
traps were prepared by heating to 180°C with flow for sixteen hours. They
were then placed in individual glass vials, wrapped with tissue paper, and
placed in a ran containing activated carbon and silica gel. Each trap had
its own number etched into it, and the same number was found on the outside
of the glass vial that contained it.
The equipment used tor the sampling included'teflon tubing, fine meter-
ing valve, toggle shutctf valve, bubble flow meter, pump and Tenax traps.
Figure 3 illustrates the entire^ VOC sampling assembly. A portable vacuum
pump was only used for -the sampling of a blank air sample for analysis. Due
13
-------
Test
Cell
Fine
Metering
Valve
-1X3
Toggle
Shut-Off
Valve
0
Teflon Tubing
Tenax Trap
Pump
Bubble
Flowmeter
Figure 3. VOC sampling assembly
to difficulties encountered eliminating leaks between the different tubing
for the pump, the decision was made to delete the pump in the assembly.
Since the sample volume was very small and the test cell had sufficient
pressure to furnish its own flow, the pump was r^t needed.
A gas chromatcgraphy-type bubble flow meter was used to calibrate the
gas flow through the Tenax trap. A 10 ml bubble flow meter allowed for
accurate measurement of the desired 7 ml to 30 ml/minute sampling flow rate.
The initial setup of the assembly did not include the trap. All lines
were connected and the flow was adjusted with the fine metering valve to give
an accuraie flow measurement using the bubble flowmeter. Water was found in
most of the regular gas measuring ports, and concern for any damage to the
sample traps warranted use cf the water inlet line for this sample procedure.
In the final setup the Tenax trap was added and the toggle valve opened,
A flew rate was taken every minute anci recorded. Temperature and barometric
pressure at the time of sampling were also noted. The toggle valve was turned
off when the desired volume of gas had passed through the trap.
14
-------
The first gas samples were collected on May 22, 1985, and again on May
29, 1985. Each sampling day provided samples from the five test cells desig-
nated for gas cnaracterization (21, 22, 23, 33, and 25), one randomly selected
duplicate, and a blank.
At first, 2-liter gas samples were collected at ambient conditions. The
selection of the 2-liter volume was based on similar gas sampling from an
on-going lysimeter study at the U.S. EPA Test and Evaluation Facility in
Cincinnati, Ohio. Actual original gas sam;-le volumes at standard temperature
and pressure ranged from 1.6 to 1.9 liter's. Initial GC/MS results from two
of the five samples (cells 21 and 23) obtained May 22, 1985, indicated that
the 2-liter sample volume was too high. Many of the compounds of interest
were present in concentrations that were too high to quantify in those sam-
ples. Furthermore, the samples were very "dirty" and the GC/MS nnccjntered
difficulties actually analyzing the samples. Therefore, new gas samples of
lower volumes were collected on June 26, 1985, and July 1, 1985. Unfortu-
nately cell 23 was emptied prior to the decision to take lower volume gas
samples. It was analyzed at the higher sample volume, however, so some
characterization data was obtained for that cell.
An additional piece of information taken into consideration in determin-
ing the sample volume of the second set of gas samples was the fact that cell
21 had been spiked with 39 grams of benzene, 37 grams of ethylbenzene, and 32
grams of toluene when the cell was originally loaded. All of these compounds
were designated as target VOCs for this project. This spiking was done in
conjunction with Ph.D. dissertation research by Janet Rickabaugh, which is
expected to be published in the Spring of 1986. Gas sample volumes collected
during the second sampling period were 25 ml for cell 21 and 100 ml for cells
22, 33, and 35. A second gas sample set contained samples from cells 22 and 33
only.
After samples were collected, they were sealed in a metal can containing
silica gel and delivered to PEI by U.C. sampling personnel.
Microbiological Sampling
Samples were taken at two levels in each of six test cells. A top
sample was taken approximately 12 inches (30 cm) into the refuse. A .-econd
sample was taken at approximately 45 inches (114 cm) -'nto the refuse, near
the bottom gravel. These samples were1 described as top and bottom, respec-
tively. Table 6 contains the tesf cell sample numhpr and the -Itpth into the
refuse for each sample.
All of the micro samples were a composite of five grab sample? which
were taken at different locations across the sampled layer. This wa? accom-
plished by peeling back the layer to be sampled and quickly grabbing a sample.
It should be noted here that although the refuse was ground, this was a coarse
grinding that maintained a particle size of about 1-1/2 to 2-1/2 inches (3.8
to 6.4 cm) (Plates 1 and 2). Furthermore, large items such as cans, plastic
bottles, etc., were not necessarily shredded into neat 2-1/2 (6.4 cm) inch
pieces. Often the items were balled into fist-sized clumps which were then
15
-------
small enough to pass through the grinder. These 1ar\e inert items were
intentionally avoided in the micro sampling. The total composite sample was
approximately 1 kilogram. As soon as the sample was taken, it was placed in a
new zip-lock plastic bay. Air was squeezed out of the bag to minimize oxygen.
Samples were transported to the University of Cincinnati in coolers, where
any oxygen in the sample was displaced with nitrogen. All samples were
processed within 96 hours.
l\ -IZtiWiF,
!.*.••* tf-tffe
$£»&$.&
Ti5g^
*-' •.-?-w>;
f^i^s^
m^^^^^^MS^w^
mP"^^.i'-^ ; -^ --'. ,: ^/?-** ^-r -g
Nl^^;-:.,,fl;_ft?^.
"•-.V-"i;^i?"
:>;;^
-• > <^
«-;->s -• -••"••
.&
1
Plate 1. Truckload of coarse ground
refuse
Plate 2. First one-foot lift of
refuse compacted in test
cell
16
-------
TABLE 6. MICROBIAL SAMPLE DEPTHS
TEST
CELL
20
23
25
26
30
35
DEPTH
TO
(inches)
15
16
19
15
16
16
FROM TOP
REFUSE
(cm)
38
41
48
38
41
41
SAMPLE
DEPTH INTO
(inches)
12
18
13
11
11
11
A
REFUSE
(cm)
30
46
33
28
28
28
SAMPLE
DEPTH INTO
(inches)
45
44
41
45
44
44
B
REKUSE
(cm)
114
112
104
114
112
112
METHODS OF ANALYSIS
Gas Characterization
The volatile organic compounds were analyzed by GC/MS using EPA Method
624. The contents of the sample traps were spiked with 5 microliters of
internal standard. This internal standard was composed of bromochloromethane,
1 ,4-dif lourobenzene, and d5-chlorobenzene. After the traps were spiked with
the internal standard, they were thermally desorbed for ten minutes at 180°C
with organic-free nitrogen bubbled through 5 ml of organic-free water and
trapped on an analytical trap. After the ten-minute desorption, the analyti-
cal adsorbent trap was rapidly heated to 180°C with carrier gas flow reversed
so that the effluent flow from the analytical trap was directed onto a 6-foot
glass column packed with SP-1000 on Carbopack D. The volatile organic com-
pounds were separated by temperature-programmed gas chromatbgraphy and de-
tected by low resolution mass spectometry. The mass of the compounds present
was calculated using the internal standard technique.
Microbiology of Refuse
Biological Safety Hood. An anaerobic safety hood consisting of a plas-
tic cabinet with aluminum framing and outside dimensions of 60 x 92 x 46 cm
was used for this study. The unit contained several gas port holes, two
rubber gloves, a clear viewing plastic window, and two zippered entrances.
During use, the cabinet was filled with carbon dioxide to lessen the effect
of oxygen on the solid waste sample. All samples were weighed and homo-
genized in a Waring blender within the hood and alU'wed to sit for one-half
hour to permit, condensation of atomized water dropi-ts. Before opening the
cabinet doors, the gas was vented into an icdine-fil li'd flask to decrease the
danger of worker pathogen inhalation.
17
-------
Sample Homogenization and Diluents. For microbial studies, solid waste
initially blended with sterile 0.1% peptone water (Standard Methods,
1981) for a 1:9 (10%) dilution. Thus, 30 or 40 grams of solids were added to
270 or 360 ml of sterile diluent. When early results indicated no organism
growth, a lower dilution was used. Sixty or eighty grams of solids were
added to 240 or 320 ml of sterile diluents for a 1:4 (20%) dilution. Samples
were homogenized in the Waring blender at high speed for fifteen seconds
within the nitrogen-filled anaerobic hood. The homogenate was allow to sit for
thirty minutes to permit condensation of atomized water droplets. The hood
was then evacuated, and the air forced through an iodine trap to remove any
pathogen-containing water droplets. Following this, the waste samples were
serially diluted with 0.1% sterile peptone water in preparation for the inocu-
lations .
Anaerobic Cultivation Techniques. All plates used for anaerobic studies
(blood, Standard Methods, and egg yolk agars) were pre-reduced with carbon
dioxide in a sealed container for at least two hours. Following sample
inoculation, these plates were returned to the carbon dioxide gas chamber in
an upright position for one-half hour, allowing the agar time to absorb the
inoculum. Then plates were inverted and incubated in a BBL GasPak (BBL) jar
for 24 to 48 hours. All GasPak (BBL) jars were made anaerobic with dispos-
able BBL hydrogen/carbon dioxide generator envelopes.
When tubed media were to be incubated anaerobically, they were first
heated in a boiling water bath and cooled. Following the tube inoculation,
sterile mineral oil was added to the media surface to a .height of at least
1 cm to maintain anaerobic conditions.
Microbiological Enumeration Procedures
Total and Feca'l Coliforms (Standard Methods - 909). Total and fecal
coliforms were determined by the most probable number (MPN) procedures (Stan-
•dard Methods - 909). Ten ml to 10"^ ml of the diluted homogenized sample were
inoculated into five tubes per dilution of lauryl sulfate broth. Following a
48-hour incubation at 35°C, two drops from each positive tube were inoculated
into brilliant green bile broth and EC tubes. All media were incubated using
the procedure described in Standard Methods (1981). The completed test was
carried out for all positive tubes of all samples. To determine final concen-
trations, the number of positive tuoes were converted to MPN values using the
Standard Methods (1976) MPN Index Table.
Fecal Streptococci (Standard Methods - 910).. Five tubes per dilution of
azide dextrose were inoculated with 1.0 ml to 10"^ ml of homogenized sample.
Following the 48-hour incubati-on, ?11 positive tubes were streaked onto PSE
agar. The confirmatory test and final streptococcal concentration calcula-
tions were carried out according to procedures described in Standard Methods,
and the number of positive tubes were converted to MPN values using the
Standard Methods (1976) MPN Index Table.
"- 18
-------
Clostridium perfringens (Koneman et al ., 1979; Dowel 1 and Hawkins, 1976).
Stormy fermentation of iron milk was used as an MPN fecal indicator test to
determine the concentration of anaerobes, especially of Clostridium perfrin-
gens , in solid waste (Donnelly and Scarpino, 1984). The medium chosen was iron
skim milk (Bonde, 1963; Dowel 1 and Hawkins, 1976). This was a five-tube test
to which 1.0 to 10~5 ml of diluted inoculum was added, followed by the aseptic
addition of sterile mineral oil to eaoh tube to a 1 cir. height. Tubes were
incubated at 35°C for 48 hours and read for coagulation and gas production.
To confirm the presence of Clostrtdiurr, perfringens. lOi to 20% of positive
tubes per sample were streak~e3onto blood agar plates and examined for the
presence of double-zone hemolysis, signaling the presence of this anaerobe.
Plate Count Procedures. All plate counts were made by the spread plate
technique. In preparation for plating, the diluted homogenates were Vortex-
mixed. A 0.1 solution portion from each dilution tube was added to duplicate
plates and spread with a sterile bent glass rod (Cordner et al., 1979; Koch,
1981). A one-half hour incubation period at room temperature followed the
inoculations, allowing the agar media time to absorb the inoculum. Then the
plates were inverted and incubated at 35°C for a 48-hour period. Anaerobic
plates were kept in a carbon dioxide chamber during this half-hour period
prior to anaerobic incubation in a GasPak jar. All plates and incubation
periods are listed in Table 7.
Total PI .te Counts. Standard Methods agar was the medium used for total
plate counts.Following inoculation with the serially diluted samples,
plates were incubated both aerobically and anaerobically to give some measure
of total aerobic and anaerobic bacterial counts.
Clostridium (Duncan and Harmon, 1976). Tryptone sulfite cycloserine
agar served as the growth medium for Clostridium plate counts.
Fungi. All fungi, including both yeasts and molds, were enumerated on
rose beogal agar. This medium and the procedure for its use are given in
Standard Methods (1981).
Gram Negative Rods. MacCorikey agar was used to determine the gran
negative rod plate counts. Following the sample inoculation, the plates were
incubated at 35°C for a 24-hour period.
Additional Hicrobial Analyses
Methane-Producing Bacteria. A rnethanogenesis medium was used to detect
methane yas (Donnelly and Scarpino, 1984). The inoculum added to this medium
contained 5 grams of solid waste, or 5 mis of the serially diluted homoqenate,
to a final dilution of 10. Escherichia coli inoculum and NaHCOj were also
19
-------
TABLE 7. MEDIA AND INCUBATION CONDITIONS
TYPE OF MEDIUM
TYPE OF MICROORGANISM SELECTED
MPN Test Broths/Agar
Lauryl sulfate3
Brilliant greer. bile3
ECb
Azide dextrose3
PSEb
Iron milk
Total and fecal coliform
Total coliform
Fecal coliform
Fecal Streptococcus
Fecal Streptococcus
Clostridium perfringens
Enrichment Broths
Methanogenesisc
Methane-producing bacteria
Enumeration Agars
Standard Methods - aerobic3
- anaerobic3
MacConkey"
Tryptone sulfite cycloserine3
Rose bengald
Total plate counts - aerobic
Total plate counts - anaerobic
Gram negative rods
Clostridia
Fungi
3 35°C, 48 hours
b 35°C, 24 hours
c 35°C, 30-90 days
d rooi; temperature, one week
added at this time, as described in Appendix B. The £. coli was added to
metabolize food materials and to deplete oxygen levels. Following these
additions, vials were flushed with 30% hydrogen gas and 70% carbon dioxide
for thirty seconds, sealed, and incubated at 35°C for one to three months.
Duplicate vials were used for each dilution.
The gases in these vials were measured using a Perkin-Elmer 900 chroma-
tograph. For the analysis, up to three-milliliter-volumes of sample gas were
compared to the same volume of a standard gas. The standard gas used was
from Matheson Gas Co. (Dayton, Ohio) and contained 16.47% N2, 4.15% 02, 34.71%
C02, and 44.67% CK4- The analysis was normalized to 100%, based on the pre-
sence of CH4, C02, 02, and N2 in the sample (McNair and Bonelli, 1969). A
computer program was used for individual sample calculations.
20
-------
SECTION 5
DATA AND DISCUSSION
GAS ANALYSIS
Landfill gas may be used as an alternate source of energy in order to
conserve natural gas reserves. The purpose of the original project was to
enhance the quantity and quality of the gas produced in the anaerobic land-
fill setting. One problem with landfill gas is that it may contain trace
gases that will not support combustion and may in fact create problems from
incomplete combustion products. These problems may range from simple lower-
Ing of gas BTU values to complex thermal decomposition products that would
pose a threat to users of the landfill gas. Hence the rationale for GC/MS
anal 'sis of the trace organics in the gases from these experimental land-
fill:,.
A spike of volatile organic compounds was placed in test cells 20 and 21
to provide a baseline for the GC analysis and GC/MS analysis reported here.
Thtc» two test cells received a spike which consisted of 39 grams of benzene,
37 orams of ethylbenzene, and 32 grams of toluene. Glass vials sealed with
gelatin were used to distribute the compounds throughout the top layer of the
first one-foot lift of refuse in these two cells. This provided a known
quantity of material to follow through the history of the project and three
individual compounds whose peaks and GC retention times are well known. A
complete report will be available in the Spring of 1986 which will contain
all of the GC data-developed over the five-year project.
A landfill gas may contain a large number of trace impurities, so some
seventeen compounds plus the three included in the spikes were sought in the
GC/MS analysis. These compounds were outlined earlier and can be seen in
Table 3. A brief discussion of the sources of trace landfill gas impurities
is in order before the data developed here may be appreciated. First, it
must be understood that any compound that may be converted to a gas may be
found in landfill gas. So a large number of possible compounds exist. We
shall not take the time here to describe the ways that a compound could be
converted to a gas in the landfill setting and then be found as part of the
landfill gas, but there are many possible ways. Any of the products used by
man may in theory be converted to the gaseous state. Some compounds are by
nature volatile, while others may be partially'decomposed to release gaseous
compounds. Some compounds ?re released by corrosion of the container in the
landfill setting. Many pressurp-can Qases are released ir, this manner.
Since modern man uses such a variety of manufactured and natural products, it
is not surprising that the refuse which is cast off contains such a variety
of chemical compounds.
21
-------
Target volatile organic compounds selected for analysis here represent a
cross section of potential problem-causing compounds. Some may cause corro-
sion of the gas burner and others may produce toxic end products when burned.
Some are thought to be carcinogenic or mutagenic and may cause a health
threat to landfill yas recovery personnel. All of these problems are control-
led by the concentration of the specific impurity in the gas stream. Simply
stated, the effect is concentration-dependent. Therefore, it is necessary to
know the concentrations of important compounds in the gas. These target
compounds are either important themselves, or they represent groups of com-
pounds which are important in overall evaluation of landfill gas recovery and
use.
Table 8 contains the blanks used in thsse analyses and should be discus-
sed first. All gas concentrations have been maintained in units of mass or
mass per volume for ease of comparison throughout the discussion. Appendix
A.contains all results in terms of both mg/m3 and ppm. The column designated
"Blank Trap" represents the values determined from the laboratory equipment
itself. ND values denote that less than five nanograms were detected by the
GC/MS. Notice that only the levels of benzene and methylene chloride (di-
chloromethane) were above this value. Benzene and methylene chloride are
used so routinely in the laboratory that it is hard to totally erase their
presence with the low detection limits of the high resolution GC/MS equipment.
So 6.7 ng benzene and 20 ng dichloromethane (methylene chloride) at STP,
25°C, were found by the GC/MS. Other target compounds were less than 5 nano-
grams and were reported as ND.
The column designated "Air Blank" represents the air values in the high
bay area where the test cells are located. Notice that where only two report-
able concentrations were in the laboratory blank, now there are eight report-
able compounds which were present in the test cell area air. These were in
order of concentration from highest to lowest: xylene, propylbenzene, ethyl
benzene, toluene, hexane, benzene, methylene chloride, and tetrachloroethy-
lene. These compounds were to be expected in the area because of the research
activities in the laboratory high bay setting and the gases which are vented
to the area when gas value measurements are taken on each test cell. This
venting has occurred over a five-year period.
The difference between a relatively clean laboratory setting and a
field-type area is readily apparent. The high bay area has served many
experiments which involved painting, construction, fabrication, grinding of
refuse, storage of refuse samples, leachate sampling, etc. These concentra-
tions of impurities were expected. Xylene was the highest. It is a frequent
constituent of paints and should be expected in all landfill gas and loca-
tions near landfills. Second highest were the benzenes, propylbenzene, and
ethylbenzene. They are widely used compounds and were expected. Toluene is
a paint solvent which is widely used. Next in order of concentration were
hexane, 1.14 mg/nP; benzene, U.67 ing/in^; and methylene chlorine, 0.431 mg/rv*.
These have many possible sources. They are all laboratory solvents that have
been used at some tine in the Center Hill laboratories. They are also consti-
tuents of the compounds in the refuse, so again they should be expected in
22
-------
TABLE 8. TRACE VOC CONCENTRATIONS IN BLANKS
AIR BLANK
COMPOUND BLANK TRAP 6/20/85
ng_ mg/nP at 25°C
Pentane
Tetrahydrofuran
Freon
Benzene
Dichloromethane
Hexane
Toluene
1 ,1-D'ichloroethylene
1 ,2-Dichloroethylene
1 ,1-Dichloroethane
o,m,p-Xylenes
Ethylbenzene
Chlorobenzene
Iso-octane
Isopropylbenzene
Propyl benzene
Carbon Disulfide
Naphthalene
Nonane
Trichl oroethylene
1 ,1 ,2-Trichloroethane
Tetrac.il oroethylene
ND
ND
ND
6.7
20
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
0.675
0.435
1.14
3.78
ND
ND
ND
18.3
8.37
ND
ND
ND
8.01
0.503
ND
ND
ND
ND
0.039
ND Not detected, <5 ng in sample trap
landfill gas. The compound found in Uie least concentration, tetrachloroeth-
ylene at 0.04 ng/nr*, is widely used in dry cleaning operations and may be
expected in the refuse and gas from refuse.
Tables 9 and 10 contain the concentrations of impurities found in the
gas from the test cells. Both tables list the VOCs in order of increasing
molecular weight. It should be noted that three additional VOCs, tetrahydro-
furan, freon, and carbon disulfide, were found in relatively high levels in
many of the samples and therefore have been included.
23
-------
TABLE 9. TRACE VOC CONCENTRATIONS, mg/m3 at 25°C
LYSI METER
SAMPLE DATE
COMPOUND
Pentane
Tetrahydrofuran
Freon
Benzene
Dichloromethane
Hexane
Toluene
1 ,1-Dichloroethylene
1 ,2-DichloroethyTene
1 ,1-Dichloroethylene
o,m,p-Xylenes
Ethylbenzene
Chlorobenzene
Iso-octane
Isopropyl benzene
Propyl benzene
Carbon Disul fide
Naphthalene
Nonane
Tricliloroethylene
1 ,1 ,2-Trirhloroetha'ne
Tetrachloroethylene
2i*T
5/22/85
mg/m3
ND
NO
ND
12.2
0.05
P
11.2
0.04
0.99
ND
13.3
8.78
ND
ND
ND
P
ND
ND
ND
0.149
ND
0.292
21*
6/20/85
mg/m3
6.42
ND
67.7
12.1
27.7
101
128
ND
0.54
ND
175
105
ND
ND
ND
33.7
67.7
ND
ND
0.506
ND
ND
2?
6/20/85
mg/m3
0.20
0.406
0.203
1.02
0.71
1.02
20.3
ND
1.31
ND
112
24.4
ND
ND
ND
8.11
0.965
ND
ND
0.193
ND
ND
22
7/01/85
mg/m3
1.33
ND
13.3
1.05
54.1
26.4
21.1
ND
1.85
ND
118
25.1
ND
ND
ND
11.8
128
ND
ND
0.185
ND
0.146
23*
5/22/85
mg/m3
P
ND
ND
0.40
0.017
P
3.62
0.032
1.27
ND
12.2
4.58
ND
ND
ND
ND
0.018
NO
ND
0.389
ND
0.155
* High sample volume, results tend to be low
P Identified, but not quantified
ND Not detected, <5 ng in sample trap
t Waste spiked with benzene, toluene, and ethylbenzene
Note that all of the samples from the test cells contained the three
compounds used in the spike: benzene, ethyl be/izene, and toluene. Concen-
benzene were about one fourth of fhat in the spiked cell. Toluene
exceeded one of-the spiked cell concentrations in some of the
i.vMj .uv.,....-..^ also exceeatJ the spike cell levels in some of the
This is not surprising when the mass of material is taken into con-
- ' -- — about 1,000 pounds in each test cell. The mass
trations of
concentrations
samples. Ethylbenzene
samples
sideration. Refuse mass
of the spike compounds was only a few grams
spike compounds was about one quarter pound.
was
was
The total mass of the three
So the ratio of refuse mass to
-------
TABLE 10. TRACE VOC CONCENTRATIONS, mg/m3 at 25°C
LYSIMETEK
SAMPLE DATE
COMPOUND
Pentane
Tetrahydrofuran
Freon
Benzene
Dichloromethane
Hexane
Toluene
1 ,1-Dichloroethylene
1 ,2-Dichloroethylene
1 ,1-Dichloroethylene
o,m,p-Xylenes
Ethylbenzene
Chlorobenzene
Iso-octane
Isopropyl benzene
Propyl benzene
Carbon Di sul fi de
Naphthalene
Nonane
Trich'.oroethylene
1 ,1 ,2-Trichloroethane
Tetrachloroethylene
33
6/20/85
mg/m3
NO
0.653
1.08
1.30
2.71
1.08
33.5
NO
NO
ND
249
68.3
ND
ND
ND
ND
8.02
ND
ND
ND
ND
ND
33
7/01/85
mg/m3
ND
0.626
31.3
0.725
115
30.5
20.8
ND
0.061
ND
9.14
25.6
ND
ND
ND
3.66
112
ND
ND
0.165
ND
0.032
35
6/20/85
mg/m3
2.13
0.408
ND
0.821
0.321
2.00
48.00
ND
0.651
ND
120
97.1
ND
ND
ND
3.00
10.8
ND
ND
0.13
ND
ND
35
(dupl icate)
6/20/85
mg/m3
0.90
1.08
9.71
1.18
38.4
10.7
65.2
ND
1.50
ND
513
138
ND
NO
ND
5.34
0.142
ND
ND
0.171
ND
ND
* High sample volume, results tend to be low
P Identified, but not quantified
ND Not detected, <5 ng in sample trap
spike mass was greater than 4000:1. Only seven of the original twenty target
compounds were not found in any of the samples taken. These compounds were
1,1-dichloroethane, chlorobenzene, iso-octane, isopropylbenzene, naphthalene,
nonane, and 1,1,2-trichloroethane. Most of these compounds would be used in
much higher quantities by '•ndusrry than they would be used by the average
family. So again, their absence here is not surprising.
Of those compounds found, concentrations were higher than has been
reponed in the literature. The primary reason for this was a controlled
setting in the lysimeter. Most literature data comes from sites where the
25
-------
gas r?1.3ase cannot be controlled, such as large landfills or hazardous waste
sites. The landfill is exposed to atmospheric changes. Anbient air moves
to and from the landfill as pressure increases or decreases. This causes
dilution and dispersion of the gas within the landfill. The lysimeter gas
was taken directly fron the test cell piping. There was no dilution of the
sample by ambient air. The concentrations reflect different release patterns
over time. This was to be expected due to the lanje number of complex biolo-
gical, chemical, and pnysical phenomena involved in the release of these
compounds.
Figures 4 through 9 have the compounds grouped according to relative
concentrations found in the gas. It should be emphasized here that none of
the VOC analyses was performed on recycle cells. Each of these cells was
watered once each month witn 31 liters of Cincinnati tap water. None of these
cells received 'nunicipal sewage sludge, which contains many of these same
compounds. So the source of these compounds was either from the water or
the refuse. Concentrations are such that they appear to be mainly from the
decomposing refuse.
TRACE VOC CONCENTRATIONS
n
E
l^U -
110 -
100 -
90 -
80 -
70 -
60 -
50 -
40 -
30 -
20 -
10 -
n _j
\ .-
K/
\/
-
,
"71
/,/
//
/,
f
r/
93
\\
sV.
.__, r/Tvxi
^
^
V,
//
;/
/,
y
^
/
'/>
r/\
1 ^
^
-------
TRACE VOC CONCENTRATIONS
D>
E
1 9 -i
1.8 -
1.7 -
1.6 -
1.5 -
1.4 -
1.3 -
1.2 -
1.1 -
1.0 -
0.9 -
0.8 -
0.7 -
0.6 -
0.5 -
0.4 -
0.3 -
0.2 -
0.1 -
0.0 -
\^ 1 I
/
/
/
/
/
/
/
RSI
/^
£1
-------
TRACE VOC CONCENTRATIONS
6 -
5 -
4 -
2 -
1 -
'l.
Air
21
21
—n
23
LYSIMETER
Pentane
35
Figure 6. Pentane and tetrahydrofuran concentrations
Pentane and tetrahydrofuran (Figure 6) are tv/o widely used solvents
wnich appeared in all but two of the samples. These compounds are extremely
flammable and are widely used in the manufacture of products that are in
the home. For example, the pentane is widely used in lighter fluids and
portable stove fuels. Tetrahydrofuran is widely used as a solvent in print-
ing inks. Fifty-one percent cf the refuse mass was paper. Much of it was
printed newspaper. The highest concentration for the pentane was 6.42 mg/rn-'
and the highest concentration for the THF was 1.08 mg/m .
Hexane and propyl benzene (Figure 7} are two more widely used solvents
for routine household products. Hexane was found at 101 mcj/m3 in the highest
sample, and propyl benzene was found at 33.7 nig/m^ in test cell 21 for the
high value. These compounds were found in seven of the nine samples.
— i-.-W-.ir.rlii
-------
TRACE VOC CONCENTRATIONS
E
1 1 w —
100 -
90 -
80 -
70 -
60 -
50 -
40 -
30 -
20 -
10 -
0 -
l^j
r--.
//
' /
/;
//
\
^
i
V
^ U\
^ ^
-------
TRACE VOC CONCENTRATIONS
ro
o>
E
140-i
130 -
120 -
110 -
100 -
90 -
80 -
70 -
60 -
50 -
40 -
30 -
20 -
10 -
0 -
^m?
S
^
|
5s
X
S
x
N;
N;
1
I
X
X
X
X
X
X
X
X
X
oix
'/////////////////A
X
X
X
X
X
X
X
X
X
rs ri ^
n_ 'y' r>p \^ ^\
\\ ^\ \\ /"\ Os
xX xX x
V X* V V^ V
_^X ^^X _K-C^ ^
x
X
x
[XXXXXXXXX
KX
N;
$
(^
^x ^
V'N \-
Xixj ^
;*:
X
X
X
X
x
x
X
Y
X
X
X
x
x
X
X
X
X
^
^
X
X
x
X
X
x
x
x
X
x
x
x
X
X
x
x
xxxxxxxx>:
1 1 I 1 1 I 1 I I 1
Air 21 21 22 22 23 33 33 35 35
Benzene
LYSIMETER
Toluane
......
JKX] Et. benzene
Figure 8. Benzene, toluene, and ethylbenzene concentrations
Analysis of the VOC data indicate that many of these trace organic
compounds which may pose a threat to processors and users of landfill gas are
in the gas in various concentrations. Many of the concentrations observe^
here are much higher than previously reported. This suggests that aaditio>-
trace volatile organic compound monitoring should be carried out. This ecu.
be done in landfill studies similar to this one and at gas recovery facili-
ties. Concentr tions observed \ .re should be evaluated as to their health
effects in processing anl in use of the gas.
30
-------
TRACh. VOC CONCENTRATION
600
500 -
400 -
\ 300 -
DI
E
100 -I
100 -
[71
21
21 22
[771 Xylenes
22 23
LYSIMETER
35
Figure 9. Xylenes and carbon disulfide concentrations
MICROBIOLOGY
In order to determine which oryanisms were actively stabilizing the
waste, tne refuse from six of the test cells was examined for the presence of
aerobic and anaerobic bacteria, fungi, total col i form, fecal coliforms,
fecal streptococci, gram negative rods and clostridia. Since the refuse was
saturated prior to removal to eliminate explosive levels of methane, the re-
fuse moisture contents were relatively high (Table 11). Therefore, all micro-
biological results are reported on a dry weight basis.
The majority of the analyses were performed on an 'litial homogenized
sample that consisted of 80 grams of coarsely ground refub • and 320 ml of
0.1% peptone water. It should be emphasized that the refuse was coarsely
ground and therefore was present in relatively large pieces. This resulted in
a thick slurry-like sample that was difficult to work with. Unfortunately,
of the analyses showed no microbial growth at
These results can therefore only be reported in
of organisms present. That is, results are re-
value. When dilutions and moisture contents are
values are often rather high. Typically tr.ese
at this .sample level many
the lowest dilutions used.
terms of a maximum number
ported as "less than" some
taken into account these
31
-------
TABLE 11. Microbiological Sample Moisture Contents
SAMPLE % MOISTURE
20T
20B
23T
238
25T
25B
26T
26B
30T
30B
35T
35B
65.5
66.4
63.5
68.8
64.3
67.9
73.3
75.2
62.6
63.9
72.8
69.3
"maximums" ranged from 200 to 800 MPN/100 grams dry weight for the coliforms
to 3,000 to 65,000 CFU/100 grams for the gram negative rods. While these
possible "maximums" are often rather large, it should be kept in mind that
although the number of organisms present could be as high as 65,000 CFU/100
grams, it could also be as low is 0 CFU/100 grams. The analysis simply did
not allow for a more conclusive description of these organisms. Due to the
nature of the homogenized sample consisting of 80 grams of sample and 320 ml
of liquid, it was not possible to increase the weight of refuse use without
encountering serious subsampling and analytical difficulties. For example,
the solids tended to settle out very quickly and made obtaining a representa-
tive subsamr/ie nearly impossible. Also, when performing MPN determinations,
the high solids tended to form a cap on the top of the tubes. In some cases
this resulted in false positives on the presumptive portion of the analysis.
On plate counts, the lower dilution samples tended to leave debris on the
plate which could be difficult to distinguish from organism growth. There-
fore, the 80-gram refuse sample was considered the maximum weight that could
be reliably sampled and provide acceptable results. These problems emphasize
the inadequacy of using standard water and wastewater microbiological analyses
on solid waste samples. Development ot microbiological methods for solid
waste is clearly needed in order to obtain the most conclusive and comparable
data.
Before looking at the microbiological res.Us, it is important to point
out two factors relating to the.original gas enhancement study that undoubted-
ly had a significant aVthough non-quantifiable impact on the microbiology of
32
-------
the test cells. First, the refuse was delivered directly from city collec-
tion vehicles, and after a sore sample was analyzed, the refuse was transfer-
red to Columbus, Ohio, where it was weighed and shredded. The grinding
process involves extremely high temperatures which can and probably did
destroy some of the microbial population. Since there was no microbiology on
the original refuse or on the shredded refuse, there is no way to determine
whether this was in fact the case. Second, the experimental landfills were
loaded without a clay liner on the top of the refuse as would be found in an
actual landfill situation and is commonly done in experimental landfill
design. This was purposely omitted in order to concentrate on the enhance-
ment techniques applied; however, the result to the lysimeters was the lack
of a source of microorganisms available to reseed the refuse. Since some
fraction of the microbial population was undoubtably destroyed in the grind-
ing process, this lack of a source of microorganisms probably slowed the
decomposition process and perhaps limited the level of organisms found in the
refuse during this study. With these limitations in mind, the results ob-
tained can be put into a workable perspective.
Clostridium Perfrinyens, Total Plate Counts, Fungi
The microbiological analyses can be viewed in three distinct groups.
The first group (Group 1) represents the organisms found in relatively high
numbers in all samples and consists of the fungi, Clostridium perfringens,
and both the aerobic and anaerobic standard plate counts. The next group
(Group 2) represents the organisms which were generally found in lower
numbers and often not found in many of the samples. Organisms in this
group are the gram negative rods, total and fecal coliforms, fecal strep-
tococci, and the clostridia as determined by tryptone sulfite cycloserine
agar plate counts. The last group (Group 3) consists solely of the methane
bacteri a.
Figure 10 graphically depicts the result of the first group: Clostri•
dium perfringens, the standard plate counts, and the fungi. Actual results
for these analyses can be seen in Table 12.
Cell 20 was considered a control cell throughout the five-year study,
rrceiving low infiltration only. Clostridium perfringens and anaerobic
organism levels decreased from the topsample to thebottle sample, while
fungi and aerobic organism levels stayed the same. Clostridium perfringens
seemed to predominate the sample from the top of the cell at 3.45xlOa MPN/1GO
yrams. All of the Group 1 organism types were present at similar levels in
the bottom sample, ranging from the anaerobic plate counts at 2.34x10^ CPU/
100 grams to the aerobic plate counts at 1.53xl06 CFU/100 grams.
Cell 23 received only high infiltration throughout the study. The two
types of organisms that decreased in cell 20 as well as the aerobic plate
count levels increased from the top to the bottom sample in this cell. As in
cell 20, fungi levels were essentially the same in both top and bottom sam-
ples. Relative levels of organisms were not too different between the bottom
sample of cell 20 and the top sample from cell 23. Clostridium perfringens
was the most prevalent in both the top and bottom samples in this cell with
33
-------
12.0
11.0 -
10.0 -
9.0 -
^^
I 8>°~
o. 7.0 -
o
° 6.0 H
0.
5.0 -
4.0 -
3.0 -
2.0 -
1.0 -
0.0
GROUP 1 ORGANISMS
C. perfrlngens. Plate Counts
-------
TABLE 12. GROUP 1 MICROORGANISMS (STANDARD PLATE COUNTS,
CLOSTRIDIUM PERFRINGENS, FUNGI)
SAMPLE
20T
20B
23T
238
25T
25B
26T
26B
30T
308
35T
35B
1.80xl06
1.53xl06
6.98xl05
3.66xl06
>2.60xlU11
2.86xl05
3..13xl04
9.66xl05
7.44xl04
7.85xl06
Z.OlxlO8
1.47xl09
STANDARD PLATE COUNT
(CFU/100 g dry)
Aerobic Anaerobic
3.88xl06
2.34xl05
1.60xl06
1.05xl()7
3.98xl07
3.17xl06
1.01x105
4.41xl05
<1.36xl04
8.83xlU5
2.78xl08
9.90xl06
CLOSTRIDIUM
PERFRINGENS FUNGI
(MPN/100 g dry) (CFU/100 g dry)
3.45xl08
5.22xl05
1.95xI06
2.98xl07
1.28xl09
7.62xlGG
1.63xl06
4.86xl06
9.47xl05
4.38xl06
1.68xl08
8.6U1U7
1.57xl05
1.38xl06
5.58xl05
6.47xl05
<8.64xl03
3.43xl06
4.41xlQ6
2.53xi06
3.25xl06
<5.48xl03
1.35xl06
2.42xl06
refuse that has been in contact with soil or a similar favorable medium for
fungi. The bottom sample from cell 25 snowed all Group 1 organisms present
in levels similar to both cell 20 and cell 23, including the fungi, which
showed the second, highest level of all organisms tested in this sample.
Cell 26 organism levels for Clostridium perfringens, aerobic and anae-
robic plate counts behaved similarly to those seen in cell 23. That is,
levels of these organisms increased from the top sample to the bottom sample.
However, organism levels ranged from one to two orders of magnitude lower
than in cell 23. In cell 23 the fungi were found at the lowest levels in
both the top and bottom samples. Conversely, in cell 26 the fungi were found
in the highest levels of the Group 1 organisms. This cell received high
infiltration, as did cell 23, but this infiltration was received in the form
of leachate recycle. Cell 26 also received a calcium carbonate buffer addi-
tion at the time of original cell loading. The relative levels of the fungi
with respect to the bacteria in these two cells may reflect the pH of the
refuse within each cell. That is, the leachate recycling in cell 26 would
tend to lower the pH, making conditions less favorable for bacterial growtn
and survival. The fungi would continue to grow in the lower pH environment.
Calcium carbonate buffer was added to cell 26 to prevent such a decrease in
pH levels; however, this data would tend to suggest that the buffer addition
was not capable of reversing the effect of leachate recycling on refuse pH.
Tne leachate recycling would also increase the 'level of toxics (volatile
35
-------
adds) which would inhibit methane production. Cell 23 infiltration water
was composed of Cincinnati tap water, therefore the pH of the refuse was
probably higher and the level of volatile acids was probably lower. Unf r-
tunately, the pH of these samples was not measured. However, the levels of
volatile acids in the leachate clearly demonstrates the buildup of these
toxics in the leachate recycle cells (Table 13).
TABLE 13. MEAN LEACHATE VOLATILE ACIDS, 1984
TEST
20
21
22
23
24
25
26
27
CELL
L.
L.
L.
L.
Recycle
Recycle
Recycle
Recycle
VOLATILE ACIDS
(mg/1)
11,600
11,800
7,660
8,060
24,100
18,900
25,600
15,100
TEST
28
29
30
31
32
33
34
35
CELL
L.
L.
L.
L.
Recycle
Recycle
Recycle
Recycle
VOLATILE ACIDS
(mg/1)
18,500
19,800
21,700
21,300
1,240
1,090
7,441
10,300
Data from "Demonstration of Landfill Gas Enhancement Techniques in Landfill
Simulators"
The effects of a buildup of volatile acids can be estimated by comparing
the relative levels of methane produced from each cell. At a low pH with
high levels of volatile acids, the methane bacteria would have difficulty
surviving; therefore, methane levels would be expected to be lower. This
is in fact the case as can be seen in Table 14, which shows the cumulative
methane gas production rates for 1984, the final year of the study. Cells
24 through 31 were all leachate recycle cells, and these cells clearly
have the highest levels of volatile acids. Cells 25, 27, and 29, which all
received sludge as an enhancement technique at the time of cell reloading,
had the highest methane levels of all of the cells. Apparently sufficient
microorganisms were re-seeded in these cells to allow conversion of the high
concentrations of volatile acids to methane. However, the other five leach-
ate recycle cells were the lowest methane gas producers.
The increase in organism levels from the top sample to the bottom sample
may reflect conditions that were less affected by the leachate recycle and
therefore more favorable to bacterial survival in the bottom of the cell.
This could be the result of a natural layering effect of the leachate. That
is, the majority of the toxics would tend to stay in the upper portions of
the refuse so the effects of the volatile acid concentrations would decrease
as sample depth increased.
36
\
-------
TABLE 14. 1984 CUMULATIVE GAS PRODUCTION. RATES
TEST CELL
20
21
22
23
24
25 .
26
2?
GAS PRODUCTION
(1/kg/yr)
0.22
0.57
0.41
2.20
0.19
11.40
0.21
11.30
TEST CELL
28
29
30
31
32
33
34
35
GAS PRODUCTION
(1/kq/yr)
0.08
11.60
0.18
0.09
8.42
5.43
0.20
4.32
Data from "Demonstration of Landfill Gas Enhancement Techniques in Landfill
Simulators"
Cell 30 organism levels were similar to cell 26. This is not unexpected
since cell 30 received the same enhancement techniques as cell 26, with the
addition of the nutrient supplement, ammonium phosphate ([Nh^^PO/}), at the
time of original loading, and the temperature of the cell was increased at the
time of cell reloading. The fungi were the most prevalent organisms in the
top sample from this ce'l, which may again reflect the low pH and high vola-
tile acid level in the refuse resulting from from leachate recycle. There
were no anaerobic bacteria found at the lowest dilutions used from this sample.
In the bottom sample the anaerobic plate counts were found to be 8.83x10=
CFU/100 grams, and no fungi were found at the lowest sample dilutions ana-
lyzed. An additional interesting difference between the top and bottom
samples was the increase in the aerobic plate counts from the top sample
(7.44xl04 CFU/100 grams) to the bottom sample (8.83xl05 CFU/100 grams). Ine
increase in microbial levels from the top sample to the bottom sample may
again reflect the layering out of the toxics introduced to the cell by leachate
recycle. Since the funH levels were very low, it may also suggest that
conditions were not only less hostile for the bacteria, but actually favored
populations in the bottom of the cell would
effects from the leachate recycle and would
to the ' nutrient/buffer addition and/or the
bacterial growth. MicroDial
receive the minimum negative
perhaps be able to respond
increase in cell temperature.
Test cell 35 organism levels differed somewhat from the other five
cells. Fungi levels were similar to the other cells and increased slightly
from the top sample to the bottom sample. Cell 35 showed a decrease in
levels from top to bottom for Clostridium perfringens and
standard plate count, but showed an increase in aerobic counts
were generally higher than counts from the other cells when
samples arvd bottom samples. This could be the result of the
the anaerobic
These counts
comparing top
nutrient addi-
tion enhancement applied to this cell both at the initial loading and at the
reloading in February 1933. The addition of a nutrient slurry would ensure
37
-------
that nutrient concentrations were not a limiting factor to the growth of the
microorganisms.
Total and Fees! Coliforms, Fecal Streptococci. Clostridia, and Gram Negative
Rods
The second group organisms: total coliforms, fecal coliforms, fecal
streptococci, clostridia, and the gram negative rods can be seen in Figure 11.
Actual results for these analyses can be seen in Table 15.
None of the samples had counts for all of these organisms. In fact,
cell 26 did not show the presence of any of the organisms at the lowest dilu-
tions used. Included in this group are the traditional indicator organisms
which were only present in high enough levels to quantify in three of the
twelve samples. The grinding process would have destroyed or removed many of
the original microbes, and the environment found in the lysimeter would have
GROUP 2 ORGANISIMS
Indicator Organisms it Clostridia
*-~N
£
o>
0
0
z
Q.
2
Ol
3
1 4..U -
11.0 -
10.0 -
9.0 -
8.0 -
7.0 -
C.O -
5.0 -
4.0 -
3.0 -
2.0 -
1.0 -
o
-K
^v$
+ A
* \
\
\ X
A « \
V
+ Clostriaia (TSC) A
* Gram Negative Rods
A Fecal Streptococci
X Total Colifcrms
v Focal Coliforms
• U — | 1 1 1 1 1 |~ 1 1 1 1 1 1 1 1 1 I 1
20T20B 23T23B 25T25B 26T26B 30T30B 35T35B
Sample
Figure 11. Fecal streptococci, Clostridia"/ and gram negative rods
38
-------
TABLE 15. GROUP 2 MICROORGANISMS (TOTAL AND FECAL COLIFORMS,
FECAL STREPTOCOCCI)
SAMPLE
20T
20B
23T
23B
25T
25B
26T
26B
SOT
30B
35T
358
TOTAl ~ ~
COLIFORMS
(MPN/100 g)
<2.87xl02
<2.98xl02
<5.53xl02
<6.47xl02
9.57xl04
<6. 34x10?
<5.98xl02
<6.46xl02
<5.40xl02
<5.49xl02
<3.64xl02
1.26K104
FECAL
COLIFORMS
(MPN/100 g)
<2.87xl02
<2.98xlQ2
<5. 53x10-
<6.47xl02
<7.98xl02
<6.34xl02
<5.98xl02
<6.4bxl02
<5.40xl02
<5.49xl02
<3.64xl02
<3.17xl02
FECAL
STREPTOCOCCI
(MPN/lUO gj
4.74/103
<2.98xl02
<5.53xl02
<6.47xl()2
<7.98xl02
<6.34xl02
<5.98xl02
<6.46xl02
<5.40xl02
<5.49xl02
1.45/106
4.78xl02
been so different from the natural environnent of the indicator organisms
that conditions would not have been amenable to survival and growth of these
populations. This is clearly demonstrated through the fecal colifom levels.
None of the samples shov/ed any indication of the presence of fecal coliforms
at the lowest dilutions used. Even if some of these organisms survived the
grinding process, the substrate necessary for their survival would have been
exposed and decomposed relatively quickly in the lysimeter environment. It
is not surprising then that no fecal coliforns were detected after five years
of disposal. It was also not surprising to see which samples did have quanti-
fiable levels of these organisms. Cell 20, the control cell; the top sample
from cell 25, where the sludge was added; and cell 3b, with nutrient addi-
tion, all showed the presence of the indicator organisms. This further
supports the discussion on the relative levels of the Group 1 organisms.
Gram negative rods were found in the top sample from cell 25 and the
bottom in cell 35. Again, these particular cells had conditions that were
more favorable to the growth and survival of the gram negative rods. The
Clostridia as determined by TSC were present in all cells although not every
sample, except cell 26. Based on the relatively high results of the iron milk
MPN for CJostridium perfringens, at least similar levels would be anticipated
from the pi ate counts'] The actual TSC plate counts are lower than the MPN
results, probably because of the different sample size used for each analysis.
Plate counts were done using 0.1 ml of the 20i homogenized sample. MPfis were
done using from 10 ml per tube down to 10"-" ml. Since the blended sample was
39
-------
TABLE 16. GROUP 2 MICROORGANISMS (CLOSTRIUIA, GRAM NEGATIVE RODS)
SAMPLE
20T
2 OB
23T
23B
25T
258
26T
26B
30T
30B
35T
35B
CLOSTRID1A
TSC AGAR
(MPN/100 g)
5.93x10^
4.H4xl04
1.26xl04
<3.20xl04
1.60xl05
<1 .62xl04
j.jn? 12 indicates that the additional
-------
incubation did, in fact, show methane production in more of the samples. All
samples with the exception of the top sample from cell 30 and the bottom
sample from cell 35 showed some level of methane production after the longer
Incubation period.
METHANE BACTERIA ANALYSIS
OO Day Inoutoatlon
3O H
20 -4
no
1
2OT 200
23T 23B
2OT 2BB
2BT 2BB
3OT30B
3OT 3OB
pla Numt»«r
o.o g
Figure 12. Methane bacteria after 60-day incubation
The absence of methane in the gas generally indicates the absence of
methane-forming bacteria in the samples. Based on the 60 day incubation it
is difficult to say whether the methane bacteria are truly absent from the
samples or if a 90 day incubation, had it been possible within the time
constraints of this project, might have indicated methane production in these
samples.
Absolute percentages of methane when present varied from sample to
sample. This variation may be due to many factors which were either not
measured or were not measurable. For example, the anount of substrate avail-
able to the bacteria in the small microbiological samples taken may have been
limiting to the bacteria. The key point to be obtained from this data is
that the methane bacteria were present in each, of the cells tested.
41
-------
EVALUATION OF MSW IN TEST CELLS
The refuse had been ground before placing it in the lysimeters; therefore,
the refuse was well nixed in the cells. No layering nor pockets of materials
were noted. Some recognizable items such as coins (pennies) were found to be
protected fron attack. This protection was provided by paper and plastic
items surrounding the coins.
Very little to no settling had occurred in the test cells over the five-
year period. It appeared that any settling that did occur could be attribut-
ted to differences in the amount of moist'ire added to the cells. The more
fresh water added to the cell, the greater the decomposition and settling.
Biological decomposition seemed to be inhibited and there was less settlement
In the- cells where the leachate was recycled. Since writer was added to all of
th& cells to prevent methane ignition when the cells were opened and since
the effect this saturation had on settlement was unknown no firm conclusions
could be drawn concerning settlement
Analysis of Waste Materials
Although the refuse was ground before placement into the test cells,
marsy items survived this process and were able to be identified. These
artifacts were physically examined, photographed, and noted as to condition.
These artifacts documented the resistance to biological attack of plastic,
paper, rubber, dyes, synthetic fabrics, bulk metal, plated metal, stainless
steel, wood, glass, stone, and combinations of these materials.
Other items which are readily biodegradable when exposed to attack were
protected from biological activity. These items were noted in several of the
test cells. Bits of cheese, corn kernels, corn cobs, bread, green twigs,
grass, and orange peels, which should be readily biodegradable, were pro-
tected to a small extent by plastic and paper surrounding them. A few dispos-
able diapers survived the grinder, sone with fecal natter in them. The odor
jpon opening the cells was fairly strong. Leachate recycle cells had a dif-
ferent odor than non-recycle cells. Many labels, newspapers, and book
pages showed evidence of some attack, but within the same cell some were
found to be easily read. Some clothing materials were still strong, while
others had weakened from biodegradation. Metal objects were under varying
degrees of attack. Visible attack on some copper pennies was noted. Pennies
were found with copper sulfi.ie deposits and copper sulfate deposits. Even
though the refuse was ground and thoroughly mixed, there was evidence of
protection of some items. In the rive-year period, decomposition was evident
but slow. Most of the 800 pounds of refuse originally placed in the cells
was sti11 evident.
42
-------
REFERENCES
Stamm, J., G. Vocjt, and J. Walsh. "Demonstration of Landfill Gas Enhance-
ment Techniques in Landfill Simulators", Report No. GRI-85/0116, Final
report for Gas Research Institute, Chicago, Illinois (May, 1985), 164 pp.
2. Kinman, R.N., J.
of Landfi!1 Gas
Rickabaugh, W.G. Vogt, and J.J. Walsh. "Demonstration
Enhancement Technique in Landfill Si>..jlators". Final
report for Department of Energy, February 1982,
43
-------
BIBLIOGRAPHY
Bordner, R., J. Winter, and P.V. Scarpino. Microbiological Methods for
Monitoring the Environment. U.S. Environmental Protection Agency,
Cincinnati, Ohio, 1978.
Buchanan, R.E., and N.E. Gibbons (eds). 1974 Bergy's Manual of Determinative
Bacteriology, 8th Ed.. The Williams & Wilkins Co., Baltimore, Maryland.
Donnelly, J.A. and P.V. Scarpino. Isolation, Characterization, and Identi-
fication of Microorganisms for Laboratory and Full-Scale Landfills.
EPA-600/S2-84-119, U.S. Environmental Protection Agency, Municipal
Environmental Research Laboratory,"Cincinnati, Ohio, 1984.
Dowell, V.R., and T.M. Hawkins. Laboratory Methods in Anerobic Bacteriology.
CDC Laboratory Manual, HEW Publication No. (CDC)77-8272, 1974.
Duncan, C.L. and S.M. Harmon. Clostridium Perfringens. In: Compendium of
Methods for the Microbiological Examination of Foods, M.L. Speck (ed.).
American Public Health Association Intersociety/Agency Committee on
Microbiological Methods for Foods, 1976.
Handbook for Sampling and Sample Preservation of Water and Wastewater. EPA-
600/4-82-029, EMSL, U.S. Environmental Protection Agency, Cincinnati,
Ohio, 1982.
Kinman, R.N., J. Rickabaugh, W.G. Vogt, and J.J. Walsh, "Demonstration of
Landfill Gas Enhancement Technique in Landfill Simulators,"^: Proceed-
ings of the Fifth Madison Conference on Municipal and Industrial Waste.
Madison, Wisconsin; September 1982.
Kinman, R.N., J. Rickabaugh, W.G. Vogt, and J.J. Walsh. "Demons- ration of
Landfill Gas Enhancement Technique in Landfill Simulators," _l£: Proceed-
ings of the Sixth Madison Conference on Municipal and Industrial Waste.
Madison, Wisconsin; September 1983.
Kinman, R.N., J. Rickabaugh, W.G. Vogt, and J.J. Walsh. "Demonstration of
Landfill Gas Enhancement Technique in Landfill Simulators," jji_: Proceed-
ings of the Seventh Madison Conference on Municipal and Industrial Waste.
Madison, Wisconsin; September 1984.
Kinman, R.N., J. Rickabaugh, W.G. Vogt, and J.J. Walsh. "Demonstration of
Landfill Gas Enhancement Technique in Landfill Simulators," _I_n_: Proceed-
ings of the Eighth Madison Conference on Municipal and Industrial Waste.
Madison, Wisconsin; September 1985.
44
-------
Koch, A.L. Growth Measurement. In: Manual of Methods for General Micro-
biology, P. Gebhardt et al (eds.) American Society for Microbiology,
Washington, D.C., 1981. pp. 179-207.
Koneman, E.W., et al. Color Atlas and Textbook of Diagnostic Microbiology.
J.B. Lippincott Co., Philadelphia, Pennsylvania, 1983.
Koneman, E.W., G.D. Roberts, and S.F. Wright. Practical Laboratory Mycology,
2nd Edition. The Williams and Wilkins Co., Baltimore, Maryland, 1978.
Standard Methods for the Examination of Water and Wastewater, 14th Ed., APHA,
AWWA, WPCF, 1975.
Standard Methods for the Examination of Water and Wastewater, 15th Ed. APHA,
AWWA, WPCF, 1980.
Test Methods for Evaluating Solid Waste, Physical/Chemical Methods. SW-846,
U.S. Environmental Protection Agency, 1982.
Young, P.J., and A. Parker. "The Identification and Possible Environmental
Impact of Trace Gases and Vapours irrLandfill Gases". Waste Management
and Research. Vol. 1 (1983). pp 213-226.
45
^
-------
APPENDIX A
LOG OF LYSIMETER FINDINGS: TEST CELL 20
PHYSICAL CONDITIONS
Cell Additives (Original): Low infiltration
Cell Additives (Reloading): No change
Refuse Moisture Content (June 1985): Top, 65.5%
Bottom, 66.4%
Test Cell Artifacts:
Belt
Slipper
Leather shoe
Tire tread piece '
Magazine - decomposed, lettering
legible, colors faded
Underwear
Sock
Fork - stainless
Bic pen
Metal nook - brass
Metal pieces
Rubber pieces
Rubber bands
Plastic ccmb
Metal comb
Tooth brush
Pen cartridge
Hair curlers
Plastic fork
Perfume bottle
Heart (jewelry)
Credit card
Y - plastic letter toy
' Pencil eraser
Metal tag
Queen of spades
Pepper shaker - plastic
Metal antennae
Pearl button
Belt
Cheese
Metal objects
Whistle - plastic
Artificial plant
Prescription bottle
Plastic gun
Paint brush (for models)
Spring - metal
Plastic tip to mustard bottle
Shoe belt and-buckle
Coins
46
HTMiMflL
-------
LOG OF LYSIMETER FINDINGS:
Microbiology
TEST CELL 20
ORGANISM ENUMERATIONS
Top Sample Bottom Sample
Inches Into Refuse
Std. Plate Count (aerobic)
•Std. Plate Count (anaerobic)
Clostridium perfringens
Fungi
Total Col i forms
Fecal Col i forms
Fecal Streptococci
Clostridium (TSC agar)
Gram Negative Rods
1.80xl06
3.88xl06
3.45xl08
1.57xl06
<2.87xl02
<2.87xl02
4.74xl03
5.93xl05
<7.22xl03
1.53xl06
2.34xl05
5.22xl05
1.38xl06
<2.98xl02
<2.98xl02
<2.98xl02
4.84xl04
3.75xl03
METHANE BACTERIA ANALYSIS
Composition o,c Gas in Via's
SAMPLE WEIGHT % C02 i 02
(Grams)
30 Day
Top
5.0
0.5
0.05
0.005
Bottom
5.0
0.5
0.05
0.005
60 Day
Top
5.0
Bottom
5.0
44.85
41.27
61.96
67.07
58.87
77.43
50.65
56.86
20.12
0.93
1.86
0.91
1.24
1.97
1.83
0.59
0.36
0.44
6.59
13.26
% N2
28.52
33.12
21.46
30.96
39.30
19.24
13.78
17.20
67.05
79.40
% CH4
24.77
24.70
15.34
0.00
0.00
2.74
35.21
25.50
6.24
6.40
47
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 21
PHYSICAL CONDITIONS
Cell Additives (Original): Low infiltration
Cell Additives (Reloading): No change
NOTE: Cell was not opened for study during this project. This cell is
currently part of a recently initiated gas inhibition study using lime
or lime/fly ash injection to stop landfill gas production.
48
-------
GC/MS ANALYSIS:
Concentration, at
SAMPLE
Cell 21
STP, 25°C
1
5/22/85
VOLUME, ml at STP
TEMPERATURE, °C
Pentane
Tetrahydrofuran
Freon
Benzene
Dichloromethane
Hexane
Toluene
1 ,1-Dichloroethylene
1 ,2-Dichloroethylene
1 ,1-Dichloroethane
o,m,p-Xylenes
Ethyl benzeiie
Cnlorobenzene
iso-octane
Isopropyl benzene
Propyl benzene
Carbon Disulfide
Naphthalene
Nonane
Trichloroethylene
1 ,1 ,2-Trichloroethane
Tetrachloroethylene
1851
19
mg/rn^
ND
ND
ND
12.2
0.05
P
11.2
0.04
0.99
ND
13.3
8.78
ND
ND
ND
P
ND
ND
ND
0.15
ND
0.29
ppm
ND
ND
ND
3.77
0.01
P
2.93
0.01
0.25
ND
3.00
1.99
ND
ND
ND
P
ND
ND
ND
0.03
ND ' ,
0.04
-.SAMPLE
2
6/20/65
30.2
19.4
mg/m^
6.42
ND
67.7
12.1
27.7
101
128
ND
0.54
ND
175
105
ND
ND
ND
33.7
67.7
ND
ND
0.51
ND
ND
ppm
2.14
ND
13.4
3.74
7.84
28.3
33.6
ND
0.13
ND
39.8
23.8
ND
ND
ND
6.76
21.4
ND
ND
0.09
ND
ND
ND: Not detected, <5 ng on sample trap
P: Present but not quantified
49
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 22
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltration
Cell Additives (Reloading): No change
NOTE: Cell was not opened for study during this project. This cell is
currently part of a recently initiated gas inhibition study using lime
or lime/fly ash injection to stop landfill gas production.
-------
GC/MS ANALYSIS:
Concentration, at
SAMPLE
Cell 22
STP, 25°C
1
6/20/85
VOLUME, ml at STP
TEMPERATURE, °C
Pentane
Tetrahydrofuran
Freon
Benzene
Dichloromethane
Hexane
Toluene
1 ,1-Dichloroethylene
1 ,2-Dichloroethylene
1 ,1-Oichloroethane
o,m,p-Xylenes
Ethyl benzene
Chlorobenzene
Iso-octane
Isopropylbenzene
Propyl benzene
Carbon Disulfide
Naphthalene
Nonane
Trichloroethylene
1 ,1 ,2-Trichloroethane
Tetrachloroethylene
100
19.4
mg/m^
0.20
0.41
0.20
1.02
0.71
1.02
20.3
ND
1.31
ND
112
24.4
ND
ND
ND
8.11
0.97
ND j
ND ;
0.19
ND
ND
ppm
0.07
0.14
0.04
0.31
0.20
0.28
5.30
ND
0.33
ND
25.4
5.b2
NO
ND
ND
1.63
0.30
ND
ND
0.04
ND
ND
SAMPLE 2
7/01
76.
26.
mg/m^
1.33
ND
13.3
1.05
54.1
26.4
21.1
ND
1.85
ND
118
25.1
ND
ND
ND
11.8
128
NO
ND
0.19
ND
0.15
/85
6
9
ppm
0.44
ND
2.63
0.33
15.4
7.44
5.57
ND
0.46
ND
27.0
5.73
ND
ND
ND
2.39
40.3
ND
ND
0.03
ND
0.02
ND: Not detected, <5 ng on sample trap
P: Present but not quantified
51
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 23
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltration
Cell Additives (Reloading): No change
Refuse Moisture Content (June 1985): Top, 63.5%
Bottom, 68.8%
Test Cell Artifacts:
Aluminum wire
Golf ball
Handle of tooth brush
Paper wrapper - legible label
Athletic shoe
Plastic bottle - legible label
Metal cans - rusted, obvious
degradation, balled up from
grinding process
Legible print on paper items
Envelope - a lot of attack
except where pl-astic
protected address
Magazine pages - some print
legible, colors faded and
stained
Piece of rubber car tire
Slipper - obvious decomposition
Yog art lid - cardboard, shows
attack
Pair of jeans - shows decomposi-
tion
Aluminum chain - no attack
Pepsi can - red and blue colors
vivid
Plasiic comb
Bottle cap - label legible
Piece of a thong
Pieces of plastic credit cards
Plastic bass
Cigarette lighter (plastic)
Bristle brush (plastic)
Hair curler (plastic)
Batteries
Artificial plants
Heel of shoe
Plastic 'lisc
Artificial plant - pine
7-Up can - vivid colors
Prescription bottle
Jeans - material strong
Chain (metal) - rusted
Metal cans - various degrees
of decomposition
Miracle Whip "lid - legible
print, paint over metal
preserved i t
Plastic bottle - legible print.
Pencil
Coins
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 23
Microbiology
ORGANISM ENUMERATIONS
Top Sample
Bottom Sample
Inches Into Refuse
Std. Plate Count (?erobic)
Std. Plate Count (anaerobic)
Clostridium perfringens
Fungi
Total Coliforms
Fecal Coliforms
Fecal Streptococci
Clostridium (TSC agar)
Gram Negative Rods
6.98xl05
1.60xl06
1.95xl06
<5.53xl02
<5.53xl02
<5.53xl02
1.26xl04
<1.40xl04
3.66xl06
1.05x10'
2.98xl07
6.47xl05'
<6.47xl02
<6.*7xl02
<6,47xlO?
<3.20xl04
<6.48xl04
METHANE BACTERIA
ANALYSIS
Composition of Gas in Vials
SAMPLE WEIGHT % C02
(Gram:)
30 Day
Top
5.0
0.5
0.05
0.005
Bottom
5.0
0.5
0,05
0.005
60 Day
Top
5.0
Bottom
5.0
1.34
0.0
2.28
0.0
0.0
4.73
1.81
0.0
2.04
21.87
% 02
17.52
20.08
17.62
18.80
19.52
17.20
17.20
18.18
3.81
0.60
% Np
81.14
79.92
80.10
81.20
80.48
78.07
80.99
81.82
94.11
63.16
% CH4
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.04
14.37
53
-------
VOLUME, ml at STP
TEMPERATURE, °C
Pentane
Tetrahydrofuran
Freon
Benzene
Dichloromethane
Hexane
Toluene
1 , 1-Dichloroethylene
1 ,2-Dich luroethylene
1 ,1-Dichloroethanc
o,ir,p-Xylenes
Ethyl benzene
Chlorobenzene
Iso-octane
I sopropy "(benzene
Propyl benzene
Carbon Distil fide
Naphthalene
Nonane
Trichloroethylene
1 ,1 ,2-Trichlorcethane
Tetrachloroethylene
GC/MS ANALYSIS: Cell 23
Concentration, at STP, 25°C
SAMPLE 1
5/22/85
1914
18.9
ir.g/n>3
P
ND
NO
0.40
0.02
P
3.6?
0.03
1.28
ND
12.2
4.58
ND
ND
ND
ND
0.02
ND
I ND
'0.39
ND
0.16
ppm
P
ND
ND
0.12
0.01
P
0.95
0.01
0.32
ND
2.77
1.04
ND
ND
ND
ND
0.01
ND
ND
0.07
ND
0.02
ND: Not detected,
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 24
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltreticn, leachatc recycle
Cell Additives (Reloading): No change
Refuse Moisture Content (June 1985): Top, 65.7%
Bottom, 60.7%
Test Cell Artifacts:
Batteries
Plastic bottles - print barely
legible to legible
Plastic letters - to a game
Metal cans - varying degrees
of degradation
Sole of a shoe (rubber)
Lipstick caps - some degradation
of metal surface
Plastic credit card piece
Button - red, white, and blue
colors vivid and protecting
metal
Hypodermic syringe
Plastic - artificial plants,
leaves
Sponge
Coffee grounds holder for
coffee pot- - no degradation
evident
Sock - maroon color strong and
material strong
Coi ns
Rock
Fork (stainless steel) - no
attack
Crest toothpaste tube - strong
color and label good
Piece of ceramic pottery dish
Bones
Hair comb
Metal key - coated with residue
Doll leg (plastic)
Ribbon - green
Bic pen
Plastic toys - army man, wheels,
Batman figure
Copper metal di sk
Brass screw - rusted
Brass buttons - no rust
Seeds
Hose fitting (brass) - rusted
Metal chain - sulfide stain
Aluminum metal object - no attack
Corn cob
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 25
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltration, leachate recycle
Cell Additives (Reloading): SV'dge addition
Refuse Moisture Content (June 1985): Top, 64.31
Bottom, 67.9%
Test Cel1 Artifacts:
Inflatable plastic toy
Plastic bottles - labels under
attack, barely legible
Belt
Metal can top - label legible
Sock - arterial under attack
Plastic credit cards
Plastic tooth brush
Rubber bank
Bal loon
Plastic plate - toy
Rubber toy dinosaur
Watch bank
Artificial plants
Lego block (plastic)
Aluminum wire - shows attack
Lipstick lid - rust
Popsicle stick (wood)
Battery
Piece of plastic brush handle
Plastic wrapper - label legible
Stamp on letter - no attack on
stamp, colors vivid, letter's
paper shows attack
Piece of plastic toy horn
Coi ns
56
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 25
Microbiology
ORGANISM ENUMERATIONS
Top Sample Bottom Sample
Inches Into Refuse
Std. Plate Count (aerobic)
Std. Plate Count (anaerobic)
Clostridium perfringens
Fungi
Total Col i forms
Fecal Col i forms
Fecal Streptococci
Clostridium (TSC agar)
Gram Negative Rods
>2.60xl011
3.98xl07
1.28xl09
<8.64xl03
9.57xl04
<7.98xl02
<7.98xl02
1.60xl05
2.40xl08
2.86xl05
3.17xl05
7.62xl06
3.43xl06
<6.34xl02
<6.34xl02
<6.34xl02
<1.62xl04
<1.58xl04
METHANE BACTERIA ANALYSIS
Composition of Gas in Vials
SAMPLE. WEIGHT % C02 % 02
(Grams)
30 Day
Top
5.0
0.5
0.05
0.005
Bottom
5.0
0.5
0.05
0.005
60 Day
Top
5.0
Bottom
5.0
55.13
39.18
18.96
26.76
15.26
20.00
8.22
12.77
3.02
1.72
7.84
19.74
17.98
1 32.75
18.56
27.16
25.50
0.62
% N2
39.70
51.07
60.52
54.76
51.99
60.17
64.22
61.67
49.60
% CH4
3.45
l.«M
0.78
0.50
0.0
1.27
0.40
0.06
46.76
Not Analyzed
57
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 26
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltration, leachate recycle, buffer
addition
Cell Additives (Reloading): No change
Refuse Moisture Content (June 1985): Top, 75.3%
Bottom, 75.2%
Test Cell Artifacts:
Piece of umbrella - cloth strong,
colors faded
Rubber bulb
Metal cans - rusted
Aluminum metal can - some attack,
label legible
Milk carton - shows some attack,
label legible
Plastic balloon wrapper - shows
attack, but label legible
Rubber elephant toy
Prescription bottles (plastic) -
.abels legible
Cotton glove - darkened, material
strong
Glasses case
Batteries
Cigarette pack (Kool) - shows
attack on label
Plastic credit card
Lego block (plastic)
Plastic toy top
Plastic artificial strawberry
Artificial plant leaf
Marble
Rubber band
Piece of garden hose
Plastic doll arm
Plastic cap
Die
Plastic hair curler
Metal button - colors vivid,
paint protected metal surface
Pierced earring
Cotter pin (aluminum) - no
attack
Corn cob - some attack
Bones
Balloon
Wiring (copper and aluminum)
Metal (brass) - rusted
Negative film
Metal cans - various degrees
of decomposition (aluminum
cans hold up better)
Metal piece - rusted
Plastic bottle - paint faded,
barely legible
Metal clip
Coins
58
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 26
Microbiology
ORGANISM ENUMERATIONS
Top Sample
Bottom Sample
Inches Into Refuse
Std. Plate Count (aerobic)
Std. Plate Count (anaerobic)
Clostridium perfringens
Fungi
Total Coliforms
Fecal Coliforms
Fecal Streptococci
Clostridium (TSC agar)
Gram Negative Rods
3.13x104
l.OlxlO5
1.63xl06
4.41x10°
<5.98xl02
<5.98xl02
<5.98xl02
T.03xl07
<9.15xl03
9.66xl05
4.41xl05
4.86xl06
2.53xl06
<6.46xl02
<6.46xl02
<6.46xl02
2.89xl06
3.78xl06
METHANE BACTERIA ANALYSIS
Composition
SAMPLE WEIGHT % CQz
(Grams) •
30 Day
Top
5.0
0.5
0.05
0.005
Bottom
5.0
0.5
0.05
0.005
60 Day
Top
5.0
Bottom
5.0
2.98
0.0
0.0
0.0
0.0
3.54
0.0
3.73
1.74
3.84
of Gas in Vials
% 02
19.08
10.66
21.33
20.14
18.44
17.39
20.03
16.68
12.43
10.90
% N£
77.94
89.34 '
78.67
79.86
81.50
79.07
79.97
79.59
83.41
81.15
% CH4
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
2.42
4.11
59
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 27
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltration, leachate recycle, buffer
addition
Cell Additives (Reloading): Sludge addition
NOTE: Cell was not opened for study during this project. This cell is
currently part of a recently initiated gas inhibition study using
lime or lime/fly ash injection to stop landfill gas production.
60
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 28
PHYSICAL CONDITIONS
Cell Additives (Original}:
High infiltration, leachate recycle, nutrient
addition
Cell Additives (Reloading): No change
Refuse Moisture Content (June 1985): Top, 54.5%
Bottom, 61.7%
Test Ce\l Artifacts:
Raisin box - some attack
Coffee tin lid - no attack
Coin purse (rubber)
Tire piece
Sole of shoe
Leather shoe
Plastic plate
Wood pieces
Curlers (plastic)
Paint brush
Straw (plastic)
Artificial flower (plastic)
Metal zipper
Metal Cans - various degrees
of attack
Rope
Brass rod - some rust
Glasses case
Magazine - showed attack, but
print fairly legible
Cigar holder (plastic)
Sock
Cotton clcth
Rubber tubing
Plastic medicine bottle
Plastic heart - bottle stop
Light bulb base
Rubber toy cowboy
Knife blade
Plastic card/calendar -
legible
Toe of shoe
Cans (metal) - various degrees
of degradation
Paper cups - legible print
Rubber ball
Envelope - legible address
Leather strap
Coins
61
^
-------
LOG OF LYSIKETER FINDINGS: TEST CELL 29
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltration, leachate recycle, nutrient
addition
Cell Additives (Reloading): Sludge addition
NOTE: Cell was not opened for study during this project. This cell is
currently part of a recently initiated gas inhibition study using
lime or lime/fly ash injection to stop landfill gas production.
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 30
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltration, 'leachate recycle, buffer
addition, nutrient addition
Cell Additives (Reloading): Temperature increase
Refuse Moisture Content (June 1985): Top, 62.6%
Bottom, 63.9%
iest Cell Artifacts:
Glove - strong material
Tennis hat (cotton^ - strong
material
Shoe (leather) - strong material
Metal cans - various degrees of
attack - some labels legible
Polaroid photo - faded but image
legible
Glasses case
Batteries
Rubber band
Bone
Wood clothespin
Plastic toys - dog
- skull
- cherries
- spider (rubber)
- letter
- teeth
- number 8
Cotton patch (Arthur Treacher's
Fish and Chips) - strong
material
Hair curler
Artificial flowers (plastic)
Razor blade
Stainless steel knife handle
Business card (paper) - legible
Orange peel
Hair band
Syringe
Metal plated object
Copper wire
Plastic money holder
Plastic bottle - legible label
Bank key holder (rubber/plastic)
Bread in plastic bag
Candy cane handle (plastic)
Metal spring
Rubber bath mat
Metal cans - various degrees of
decomposition
Plastic bottle
Tube
Plasma bag
63
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 30
Microbiology
ORGANISM ENUMERATIONS
Top Sample
Bottom Sample
Inches Into Refuse
Std. Plate Count (aerobic)
Std. Plate Count (anaerobic)
Clostridium perfringens
Fungi
Total Coliforms
Fecal Coliforms
Fecal Streptococci
Clostridium (TSC agar)
Gram Negative Rods
7.44xl04
<1.36xl04
9.47xl05
3.25xl06
<5.40xl02
<5.40xl02
<5.40xl02
1.35xl05
<1.36xl04
7.85xl06
8.83xl05
4.38xlO<>
<5.48xl03
<5.49xl02
<5.49xl02
<5.49xl02
<1.37xl04
<1.37xl04
1
METHANE BACTERIA ANALYSIS
Composition
SAMPLE WEIGHT % C02
(Gramsj
30 Day
Top
5.0
0.5
0.05
0.005
Bottom
5.0
0.5
0.05
O.OU5
60 Day
Top
5.0
Bottom
5.0
79.67
66.04
83.93
64.44
65.08
56.30
40.92
40.52
0.0
3.81
of Gas in Vials
% 02
2.05
4.50
1.42
2.91
2.74
4.03
4.54
5.96
11.32
6.46
% N2
18.28
29.46
14.65
32.65
32.18
39.67
54.54
53.52
88.68
77.94
% CH4
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
11.79
64
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 31
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltration, leachate recycle, buffer
buffer addition, nutrient addition
Cell Additives (Reloading): Temperature increase
Refuse Moisture Content (June 1985): Top, 57.1%
Bottom, 54.2*
Test Cell Artifacts:
Plestic bottles - some labels
legible, some not
Plastic baby shoe
Plastic toy (fist)
Toothpaste tube - label vivid
Comb
Piece of plastic coat hanger
Nail polish cep and brush
Artificial plant
Lego block (plastic)
Razor bla^e - no rust
Doll leg
Cigar ho-der
Plastic credit card
Wine bottle cap (plastic)
Hair band
Hair c.irlers
Blush compact (makeup)
Metal faucet - not rusted
Battery
Plastic mustard bottle
Plastic doll foot
Orange juice carton - label
legible
Slipper
Sock
Honey pack (plastic) - label
legible
Various metals pieces, cans,
wires - various degrees of
decomposi tion
Plastic devil toy
Glove
Hair clip (metal)
Kiboon (pink)
Bone
Coins
65
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 32
PHYSICAL CONDITIONS
Cell Additive-.; (Original): High infiltration, buffer addition
Cell Additives (Reloading); ho change
NOTE: Cell was not opened for stin.y during this project- Thv-, cell 1s
currently part of a recently initiated yas inhibition study using
lime or lime/fly ash inject:cn to stop landfill gas production.
66
'iH rfthhif T.te
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 33
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltration, buffer addition
Cell Additives (Reloading): Buffer slurry addition
NOTE: Cell was not opened for study during this project. This cell is
currently part of a recently initiated gas inhibition study using
lime or lime fly/ash injection to stop landfill gas production.
67
-------
GC/MS ANALYSIS:
Concentration, at
SAMPLE
Cell 33
STP, 25°C
1
SAMPLE 2
6/20/85
VOLUME, ml at STP
TEMPERATURE, °C
Pentane
Tetrahydrofuran
Freon
Benzene
Dichloromethane
Hexane
Toluene
1 ,1-Dichloroethylene
1 ,2-Dichloroethylene
1 ,1-Dichloroethane
o,m,p-Xylenes
Ethylbenzene
Chlorobenzene
Iso-octane
Isopropylbenzene
Propylbenzene
Carbon Oisulfide
Naphthalene
Nonane
Trichloroethylene
1 ,1 ,2-Trichloroethape
Tetrachloroethylene
94.
21.
mg/m^
ND
0.65
1.08
1.30
2.71
1.08
33.5
ND
ND
ND
249
68.3
ND
ND
ND
ND
8.02
ND
ND 1
ND '
ND
ND
1
T
ppm
ND
0.22
0.21
0.40
0.77
0.30
8.76
ND
NO
ND
56.4
15.5
ND
ND
ND
ND
2.53
ND
ND
ND
ND
ND
mg/m
ND
0.63
31.3
0.73
115
30.5
20.8
ND
0.06
ND
91.4
25.6
ND
ND
ND
3.66
112
ND
ND
0.16
ND
0.03
7/01/85
163
26.9
3 ppm
ND
0.21
6.22
0.23
33.4
8.74
5.57
ND
0.02
ND
21.3
5.96
ND
ND
ND
0.75
35.4
ND
ND
0.03
ND
<0.01
ND: Not detected,
-------
LOG OF LYSIKETER FINDINGS: TEST CELL 34
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltration, nutrient addition
Cell Additives (Reloading): No change
Refuse Moisture Content (June 1985): Top, 64.2%
Bottom, 64.3%
Test Cell Artifacts:
Glasses cases
Brass tube - discolored
Piece of mirror
Metal perfume bottle caps
Metal button (WLW) - rusted
Coin purse
Battery
Clothes pins (wooden)
Bra
Newspaper - decomposed, some
print legible
Key holder (metal)
Deodorant roller head
Watch band piece
Necklace (plastic)
Metal play penny
Lighter
Piece of comb
Plastic and metal pieces
Cotton glove
Piece of rubber tire
Makeup tube
Coi ns
Sole of shoe - leather
Plastic bottles - print and
colors vivid
Plastic doll leg
Doll head
Bones - piece of pelvis
and vertebrate
Ceramic boot
Baby bottle nipples
Piece of brick
Hair curler
Plastic letter G
Rubber ball
Holy card - image visible
Stainless steel spoon
Artificial plant
Toothpaste tube
Leather strap
Stainless knife b^de - one end
discolored
Syri nge
Pencil
69
-------
LOG OF LYSIMETER FINDINGS: TEST CELL 35
PHYSICAL CONDITIONS
Cell Additives (Original): High infiltration, nutrient addition
Cell Additives (Reloading): Nutrient slurry addition
Refuse Moisture Content (June 1985): Top, 72.8%
Bottom, 69.3%
Test Cell Artifacts:
- Golf ball
Batteries
Hair band
Spool
Spool of thread
Thong piece
Hose clamp
Latch lock (iietal)
Chain link
Spring (metal)
Tennis shoes
Brass hose end (male)
Lighter
Cork
Plastic candy cane
(-1 ove
Plastic inflatible
Leather purse
Slipper
Copper wiring
Coi ns
70
-------
LOG OF LYSIMETER FINDINGS:
Microbiology
TEST CELL 35
ORGANISM ENUMERATIONS
Top Sample Bottom Sample
Inches Into Refuse
Std. Plate Count (aerobic)
Std. Plate Count (anaerobic)
Clostridium perfringens
Fungi
Total Coliforms
Fecal Coliforms
Fecal Streptococci
Clostridium (TSC agar)
Gram Negative Rods
2.01xl08
2.78xl08
1.68xl08
1.35xl06
<3.64xl02
<3.64xl02
1.45xl05
1.03xl07
<9.15xl03
1.47xl09
9.90xl06
8.61xl07
2.42xl06
1.26xl04
<3.17xl02
4.78xl02
2.89xl06
3.78xl06
METHANE BACTERIA ANALYSIS
Composition
SAMPLE WEIGHT % C02
(Grams)
30 Day
Top
5.0
0.5
0.05
0.005
Bottom
5.0
0.5
0.05
0.005
60 Day
Top
5.0
Bottom
5.0
60.08
44.39
44.94
45.50
73.04
64.03
78.58
34.92
0.06
0.0
of Gas in Vial s
% 02
2.46
4.20
5.30
4.12
1
! 3.22
' 2.38
1.05
6.31
11.47
11.51
% N2
27.42
51.41
49.76
50.38
23.74
33.59
20.37
58.77
41.64
88.49
% CH4
10.04
0.0
0.0
0.0
0.0
0.0
0.0
0.0
46.83
0.0
71
-------
GC/MS ANALYSIS: Cell 35
VOLUME, ml at STP
TEMPERATURE, °C
Pentane
Tetrahydrofuran
Freon
Benzer. ^
Dichloromethane
Hexane
Toluene
1 ,1-Dichloroethylene
1 ,2-Dichloroethylene
1 ,1-Dichloroethane
o,m,p-Xylenes
Ethyl benzene
Chlorobenzene
Iso-octane
Isopropylbenzene
Propyl benzene
Carbon Bisulfide
Naphthalene
Nonane
Trichloroethylene
1 ,1 ,2-Trichloroethane
Tetrachloroethylene
Concentration
mg/m^
2.13
0.41
NO
0.82
0.32
2.00
48.0
ND
0.65
ND
120
97.1
ND
ND
ND
3.00
10.8
ND
ND
0.13
ND
ND
, at STP, 25°C
SAMPLE 1
6/20/85
100
21.7
ppm
0.72
0.14
ND
0.26
0.09
0.56
12.6
ND
0.16
ND
27.5
22.2
ND
ND
ND
0.61
3.42
ND
NO
0.02
ND
ND
SAMPLE
1 Dup *
6/20/85
94.6
21.7
mg/m^
0.90
1.08
9.71
1.18
38.4
10.7
65.2
ND
1.50
ND
513
138
ND
ND
ND
5.34
0.14
ND
ND
0.17
ND
ND
ppm
0.30
0.36
1.93
0.36
10.9
3.02
17.2
ND
0.37
ND
117
31.7
ND
ND
ND
1.08
0.04
ND
ND
0.03
ND
ND
W: Not detected, <5 ng on sample trap
P: Present but not quantified
*: Duplicate sample taken at first sampling, Cell dismantled prior to
ser.ond sampling
72
-------
APPENDIX B. MICROBIOLOGICAL MEDIA AND REAGENTS
MEDIA AND REAGENTS
Azide Dextrose Broth
*
Difco Laboratories, Detroit, Michigan.
Blood Agar
• Blood agar base (Difco) 40 g
Deionized distilled water 1 L
Sterilized at 121°C for 15 minutes. Cool to 50°C and add 50 ml of
sheep defibrinated blood froiTi Flow Laboratories, McLean, Virginia
22102.
For anaerobic bacteria, incubate in a GasPak (BBL) jar.
Blood Agar for Streptococci and Clostridia
• Blood agar base (heart infusion, Difco), prepared 1 L
• Sheep blood (Flow Laboratories) 50 ml
Mix aseptically.
Brilliant Green Bile 20% (Difco)
EC Medium (Difco)
Eosin Methylene Blue Agar (Difco)
Ethyl Violet Azide Broth (Difco)
Gases
To grow clostridia and methane bacteria.
• Carbon dioxide, +99% pure
• Hydrogen, 99.95% pure
These were purchased from the Linde Division, Union Carbide
Corporation, Charleston, West Virginia.
73
-------
Gases - Standards used in gas chromatograph
Mixture:
• Carbon dioxide, mole percentage, 34.71%
• Oxygen, 4.15%
• Methane, mole percentage, 44.67%
• Nitrogen, 16.47%
Matheson Gas Co., Dayton, Ohio
Iron Milk
Qowell and Hawkins (1976)
• Skim milk powder (BBL) 100 g
Iron wire, 2 cm 1 per tube
Deionized distilled water 1 L
Sterilize at 115°C for 20 minutes.
Lauryl Sulfate Broth (BBL)
MacConkey Agar (3BL)
Methanogenesis Medium
Donnelly and Scarpino (1984)
Enrichment broth for methane-producing bacteria.
Sewage Sludge 300 ml
KH2P04 0.5 g
K2HP04 . 0.5 g
NaCl 1.0 g
(NH4)2S04 0.5 g
MgS04'7H?0 6.2 g
CaClo-2HoO 0.13 g
Reasurin 0.001 g
MnS04'H20 0.5 g
FeS04'7R?0 0.2 g
CoCl2'6H20 0.17 g
7.nS04'7HoO 0.18 g
CuS04'5HoO 0.02 g
Na2S04J12H 0 0.018 g
H3B04 (Bone Acid) 0.01 g
Na2Mo04'2H20 0.01 g
Trypticase (or tryptone) 2.0 g
Yeast Extract 2.0 g
Na Formate 2.0 g
Na Acetate 2.0 g
Water 700 ml
74
-------
Place 100 ml of medium in 150 ml glass vials and flush with oxygen-
free nitrogen. Sterilize at 121°C for 15 minutes. Re-fluch "^h
oxygen-free nitrogen and secure mouth of vials with serum
rubber stoppers. Cool.
with
sleeve
' 50% NaHCOj
• Eschericlm coT_i_ ATCC 13706, overnight culture
grown at 37°C in brain heart infusion broth.
Mineral Oil
Society of American Bacteriologists (1957)
Sterilize in 100 ml amounts at 121°C for 60 minutes.
(0.1%) Peptone VJater
Standard Methods (1980)
A diluent for bacterial cultures
• Bacto-peptone (Difco)
Deionized distilled, water
Sterilized at 121°C for 15 minutes.
0.25
0.50
1.0
1
Trypticase soy broth (BBL)
Sodium metabisulfite
Ferric ammonium citrate
Agar (Difco)
Yeast extract
Distil led water
30.0
1.83
1.0
20.0
5.0
1
ml
ml
9
L
PSE Agar - (Bile Esculin Azide Agar- Gibco Laboratories, Madison, WI
53713)
Standard Methods Agar (BBL)
Tryptone Sulfite Cycloserine (TSC) Agar
Duncan and Harmon (1976)
To enumerate Clostridium perfringens
9
9
g
g
g
L
Heat to dissolve ingredients. Adjust pH to 7.6. Sterilize at 121°C
for 10 minutes. Cool to 50°C. To each liter of medium, add 10 ml
of 4.0% D-cycloserine (sterilized by the membrane filter) and 80 ml
of sterile 50% egg yolk in saline.
75
-------
APPENDIX C. QUALITY ASSURANCE
The data quality criteria that were of concern in this project and
which are addressed in this appendix are precision, accuracy, completeness,
representativeness and comparability of the data. Each of the following
sections describes one of these criteria. The final section summarizes the
data quality for all analyses including those analyses without corresponding
QA information. This summary discusses problems that were encountered and
the overall usability of all of the data.
PRECISION
Precision is defined as the measure of mutual agreement among individual
measurements of the same property. This is monitored by comparing the re-
sults pf split or duplicate samples. The goal is always to minimize the
difference between the replicate results. Precision for all analyses has
been evaluated in one of two ways. In most cases the precision has been
evaluated as described in "Calculation of Precision, Bias and Method Detec-
tion Limit for Chemical and Physical Measurements". The replicate analyses
were evaluated for any apparent trends between the mean values and the stand-
ard deviation and/or the coefficient of variation
licates. In all cases, the standard deviations
decreased with decreasing concentrations. The
showed no clear relationship across concentration
of the data pairs or trip-
of the replicate results
coefficient of variation
ranges. Therefore, pre-
cision for most analyses has been expressed as a standard deviation derived
from the mean coefficient of variation from each data set. The standard
deviation is derived from the coefficient of variation according to the
following equation:
s = CV X / 100
where: s = standard deviation
CV = coefficient of variation
X = sample concentration
For the microbiological analyses at least two plates per dilution were
set up for each plate count procedure. These replicate plates were simply
sub-samples of the same homogenized sample. Evaluating the results of these
replicates provides information on the variability associated with the method
and the analyst technique. In many cases even at the lowest dilution used
(IxlO'l) there were no colonies formed. When no colonies were formed the
results were not included in any of the QC calculations.
In order to estimate the effect sub-sampling had on result variability
76
-------
one duplicate sample was analyzed on each microbiological sampling day. This
duplicate was a separate sub-sample of the bulk (1 kg) micro sample taken at
each lysimeter sampling location. This duplicate was then homogenized and
diluted as necessary for analysis. Since there were only three actual dupli-
cate samples and since so many of the results showed no microbial populations
at the lowest dilutions used it was not meaningful to determine the standard
deviation of the results. It is helpful to examine these results in teais of
the deviation about the mean. This provides some direct indication of how
far two duplicate results differ from the reported mean value.
%D = I - Xn
_ x 100
X
where: %D_ = % Deviation from the mean
X = Mean Concentration of duplicate results
Xn = One of the duplicate results
This information can be loosely interpreted in the following manner- An
overall average deviation about the mean of 51% suggests that a mean colony
count of 53, for example, is derived from duplicate values of 26 and 80.
When applied to an entire data set, it could be said that for any duplicate
analyses performed of this particular analysis, the reported mean value will,
on the average, be +_ 5A% of the actual values obtained.
Gas Analysis
In order to obtain some feel for the precision of fhe gas analysis
duplicate samples were taken from a randomly selected lysimeter on one of the
sampling days. This was a field duplicate which takes into consideration
variability resulting from sampling technique, sample transport, sample
storage, sample preparation and sample analysis. The duplicate results
obtained for the two samples taken from cell 35 on 6/20/85 were presented on
page 25. Twelve of the tarcet compounds were found in both samples. One
compound, freon, was reported present in one of the samples but not in the
other. Nine of the compounds were not detected in either sample. The esti-
mate of intralaboratory short term precision for all compounds detected in
both samples is s - 0.61X where X is the mean concentration of the duplicate
results and CD represents the concentration units.
Standard Plate Count: Aerobic
Precision measurements of microbiological plate counts are based on the
actual counts prior to dilution corrections of the replicate plates. The
estimate of intralaboratory, short term precision for all aerobic standard
plate counts recorded in the sample lot is s = 0.47X CU, where X is the mean
count of the replicate plates and CU represents colonies counted. This
estimate is based on replicate analysis of fourteen samples which represent
approximately 82% of-the total samples analyzed. The actual plate counts,
not corrected for dilutions, ranged from 1 to 1100 in the refuse samples.
77
-------
Analysis precision based on the deviation about the mean of the actual
duplicate pairs was determined for this analysis. Mean reported values
are, on the average, +_ 48% of the actual duplicate data values obtained.
Standard Plate Count: Anaerobic
The estimate of intralaboratory, short term precision for all counts
recorded in the sample lot is s = 0.38X CU, where X is the mean count of
the replicate plates and CU represents colonies counted. This estimate is
based on replicate analyses of thirteen samples which represent approxi-
mately 76% of the total samples analyzed. The actual plate counts, not
corrected for dilutions, ranged from 4 to 1500 in the refuse samples.
Analysis precision based on the deviation ab jut the mean of the actual
duplicate pairs was determined for this analysis. Mean reported values are,
on the average, +_ 25% of the actual duplicate data values obtained.
Gram Negative Rods: MacConkey Agar
The estimate of intralaboratory, short term precision for all counts
recorded in the sample lot is s = 0.36X CU, where X is the mean count of
the replicate plates and CU represents colonies counted. This estimate is
based on replicate analyses cf two samples which represent approximately 12%
of the total samples analyzed. The actual plate counts, not corrected for
dilutions, ranged from 1 to 237 in the refuse samples.
The samples chosen for duplication all showed no counts at the lowest
dilutions analyzed. Therefore, there was no estimate of actual duplicate
precision.
Clostridium Perfringens; Tryptone Sulfite Cycloserine Agar
The estimate of intralaboratory, short term precision for all counts
recorded in the sample lot is s 0.26X CU, where X is the mean count of the
replicate plates and CU represents colonies counted. This estimate is based
on replicate analyses of nine samples which represent approximately 53%
of thf- total samples analyzed. The actual plate counts, not corrected for
dilutions, ranged from 3 to 2800 in the refuse samples.
Analysis precision based on the deviation about the mean of the actual
duplicates was determined for this analysis. Mean reported values are, on
the average, _+ 50% of the actual duplicate data values obtained.
Fungi: Rose Dengal Agar^
The estimate of intralaboratory, short term precision based on the
standard deviation and coefficient of variation was not determined on this
anaylsis. Analysis precision based on the deviation about the mean of the
78
-------
duplicate pairs was however, determined. Mean reported values are, on
the average, _+ 45% of the actual duplicate data values obtained.
Gas Composition (Methane Producers)
All samples were set up in 2 sample vials for each weight analyzed. Out
of all of the samples analyzed (30 and 60 day incubations) 53% of the samples
showed no methane production in either sample bottle. Another 25% had
methane production in one bottle but not the other. Only 22% of the duplicate
sample bottles had methane production in both bottles. All QC results were
based on this 22% or 13 samples only. The estimate of intralaboratory, short
term precision for each concentration found in the sample lot is s = 0.66X
CD, where X is the mean concentration of the duplicate pairs and CU represents
the concentration units of the result.
ACCURACY
Accuracy is defined as the degree of agreement of a measurement with the
true value of the measurement. Often, a measurement of the accuracy of the
measurement process is obtained through the analysis of QC standards. If the
measurement process is functioning normally, results are expected to fall
very, close to 100% recovery of the standard.
Gas Analysis
All gas samples were spiked with 5 ul of an internal standard solution
prior to sample preparation. This solution not only contained the three
compounds to be used for quantitation but also three surrogate QC standards.
These surrogates were D4-l,2-Dichloroethane, 08-Toluene and 4-Bromofluoroben-
zene. Recoveries of these compounds provide a measure of the accuracy of
the measurement process as well as the extent of interferences introduced
into the process as result of a complex sample matrix. The recoveries
obtained on these compounds for all samples analyzed including field and lab
blanks can be seen in Table C-l. These recoveries suggest that a slight
negative bias exists in the results of the lower molecular weight compounds.
That is, reported values may be lower than actual values. Those compounds
with high molecular weights may relect. a slight positive bias. That is,
reported results may be somewhat higher than true values. Those compounds
remaining show little to no bias in the reported results.
i
Microbiological Analyses
Unfortunately, standards are not available for the microbiological
analyses. There are no standards with known microbial counts to quantitative-
ly assess the validity of the microbial measurements. However, it was possible
to qualitatively evaluate the accuracy of the measurement process by evaluat-
ing the prepared media against reference cultures. These cultures were deriv-
ed directly from the American Type Culture Collection or indirectly from
Difco. These reference cultures can be seen in Table C-2.
79
ilP^flffifefefeli?^
-------
Table C-l. SURROGATE RECOVERIES
Compound
D4-l,2,-Dichloroethane
08-Toluene
4-Bromoflouro benzene
Mean
Recovery
80
99
114
Standard
Deviation
26
6
21
Minimum
Recovery
56
80
70
Maximum
Recovery
170
104
142
TABLE C-2. MICROBIOLOGICAL REFERENCE CULTURES
CULTURE NAME
Acinetobacter calcoaceticus
Clostridium novyi
Clostridium perfringens
Escherichia coli
Pseudomonas aeruginosa
ATCC NUMBER
e23055
e!9402
e3624
25922
27853
a: American Type Culture Collection, Rockville, Maryland 20852
80
qJJ^i^lEiy^
..«
-------
COMPLETENESS
Completeness is defined as the number of usable results obtained expres-
sed in terms of the total number of results expected for each analysis.
Gas analyses were 71% complete. Originally five samples, a duplicate and a
blank were taken on two different days in the early part of the project. Due
to difficulties encountered with the original 2 liter sample volume the entire
gas analysis had to be done again. Gas sample volumes were decreased however,
one cell had been dismantled prior to the first re-sampling. Therefore, only
four samples a duplicate and a blank were obtained. Before a second set of
samples could be obtained it was necessary to dismantle two additional cells.
Only two cells remained to be sampled. Unfortunately, due to the number of
traps used in the original 2 liter sampling (14 traps) and in the first
re-sampling (6 traps) insufficient traps remained to obtain a duplicate and a
blank sample on the second re-sampling day. Therefore, 14 samples were orig-
inally planned for this project but only 10 were actually taken and analyzed.
The micro analyses were 98% complete. Even though many of the results
had to be reported as less than some value, which in some cases was relatively
high, the data generated provided some feel for the relative numbers of the
various types of organisms that were present. Since this fulfilled tha
microbiological objectives for the study the results are considered complete.
The 2% of non-usable results refer to the samples that still had not generated
any methane in the methane former analysis. Since the 90-day incubation was
not completed for the samples it is not possible to say whether there were
really no methane formers present in the samples or if the results simply
reflect the fact that the samples did not incubate for 90 days. Therpfore,
2% of the results are not usable and are not considered complete.
REPRESENTATIVENESS
Representativeness is defined as the degree to which data accurately and
precisely represent a charade, istic of a population. This is generally
addressed through adherence to prescribed sampling procedures which ensure
that samples taken for analysis truly represent the entire material being
sampled. Gas samples were taken directly out of gas lines coming from the
lysimeter. Since there was sufficient pressure in the tanks to push the gas
into the sample traps it was not necessary to use a pump to pull the gas into
the traps. This eliminated one area where air contamination is often
encountered. There were no leaks determined in any of the connections
therefore the samples were truly representative of gas generated in a lysimeter
setting. Since the full-scale landfill is subjected to atmospheric interface
and dispersion of the gas within the landfill the levels of the trace
constituents may be somewhat higher in the lysimeter gas where lateral
dispersion is not possible and atmospheric interface is prevented by the
steel walls of the test ce'il. In spite of possible concentration differences
the actual compounds found in the lysimter gas are certainly representative of
the compounds that would be present in any gas generated by a municipal
waste.
81
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Although every reasonable attempt was made to ensure representativeness
of the waste samples, given the nature of the refuse in the lysin-'fers and
the volume sampled (I kg) relative to the total volume in the lysimeters, it
would be reasonable to assume that obtaining samples representative of the
entire lysimeter would be extremely difficult, if not impossible. The refuse
was clearly heterogeneous throughout and even though samples were taken such
as to minimize this problem, there is undoubtedly still some effect. Further-
more, microbiological samples were taken so that the non-biodegradable consti-
tuents (e g. glass, plastic, etc.) were intentionally excluded. It would be
reasonable to assume that the samples taken represent typical municipal
landfill samples; however, they do not necessarily represent the entire
contents of the lysimeter from which they were obtained.
COMPARABILITY
Comparability is defined as the confidence with which on data set can
be compared to another. Data generated by this project are readily compar-
able to other similar data, since all methods (with the exception of the
methane producer analysis) are standard procedures. Furthermore, all results
have been reported in standard reporting units. All solid waste results have
been reported in terns of dry weight in order to maximize comparability. All
gas results have been reported in terms of mg/m^ as well as ppm so they will
be readily comparable to any data in the literature. When data are compared
with other similar data, the problems encountered with sample representative-
ness should be kept in mind. The overall effect would tend to make data
comparable in a broad, general sense only.
SUMMARY
Gas Analysis
The gas sample matrix was known to be very complex. In fact, the samples
analyzed on 5/20/85 had such high levels of some compounds that the samples
were damaging the instrumentation. Even when the sample volumes were decreas-
ed by a factor of 20 many compounds were present at concentrations that were
near or above the dynamic range of the instrumentation. When this is taken
into account with the bias associated- v»ith the recoveries it is reasonable
to say that the concentrations reported should be regarded as approximate.
Microbiological Analyses
MPN Tests: Total Coliforms, Fecal Coliforms, Fecal Streptococci and
Clostridium perfringens
Even though duplicate samples were analyzed for each.of these tests no
relavent QC information was generated since most of the results had to be
reported as less than some value. No additional QA/QC procedures were per-
formed on the MPN tests beyond those built into a traditional MPN test. Each
82
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MPN analysis 1s designed such that several nested levels of Isolation and
Identification ensure that a high percentage of the results will be accurate.
Even though five fermentation tubes were used, precision of the results
obtained is generally not considered to be of a high order. This can be seen
in the tables of the MPN 95% confidence limits found in Standard Methods for
the Examination of Water and Wastewater. Although the MPN index was used to
estimate the truebacten aTDensity in the samples, the 95% confidence limits
have not been Included herein. Caution must be exercised when interpreting
the significance of the MPN results from this project. It should be stressed
that the most significant information obtained from the MPN tests is that the
indicator organisms survived in relatively low numbers if at all.
Plate Counts: Standard Methods-Aerobic, Standard Methods Anaerobic,
MacConkey, Rose Bengal
Precision for all plate counts is based on the actual number of colonies
counted on replicate plates. Considering the potential variability when
dealing with microorganisms, the duplication seen on this data is not surpris-
ing. The plate counts showed more variability between replicate plates than
anticipated. This can probably be attributed to the fact that almost all
plates that showed growth and could be counted were from the lowest dilutions
used. As discussed in the microbiology discussion of the text (Section 5,
page 31) the original homogenized sample was very difficult to work with.
Homogenization is an attempt to create a homogeneous sub-sample but given 80
g of sample in 320 ml of water it is doubtful that true homogeneity is
achieved. When this homogenized sample is serially diluted it approaches
homogenetiy and therefore less variability is found between replicate plates
at higher dilutions. Conversely, greater variability is experienced between
replicate plates of lower iilutions. This is essentially a reflection of the
method and until microbiological methods are established specifically for
solid waste this level of variability will continue to be seen. Accuracy of
these analyses relied heavily on analyst experience. It is difficult to
eliminate this dependency; however, it is minimized through the use of Stan-
dard Reference Cultures which ensure that the desired organism(s) will, in
fact, grow on the media prepared for that purpose. For the purposes of this
project, the data generated through the plate counts confirms the presence of
many organisms in relatively high numbers.
Enrichment Tests: Methane Producers
The methane producer test was. basically used as a qualitative test for
the presence or absence of methane producing bacteria. This was accomplished
by quantifying methane levels in the test vials. The data generated are
clearly usable for this purpose.
Based on the assumption that the data generated on this project are
intended to be used in a general, relative sense, all of the data can be
considered acceptable for this purpose. Although QC oata was not or could
83
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not be generated for all analyses, this does not seriously effect the use-
ability of this information.
84
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