TEST PROTOCOLS FOR DETERMINING THE "FREE LIOUID"
CONTENT OF HAZARDOUS WASTE
This document £&&*$&&$ was prepared for the Office of Solid Waste
under contract no. 68-01-3911
-V '-v ^
, 1 -Jl 1
U.S. ENVIRONMENTAL PROTECTION AGENCY
December 1983
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57144 - Federal Register / Vol. 48, No. 250 / Wednesday. December 28, 1983 / Proposed R^!e<
jes
ENVIRONMENTAL PROTECTION
AGENCY
40 CFR Parts 264 and 265
[SWH-FRL 2497-1 ]
Hazardous Waste Management
Facilities; Availability of Information
AGENCY: Environmental Protection
Agency.
ACTION: Notice of availability of
information and.request for comments.
SUMMARY: The Environmental Protection
Agency hereby notices the availability
01 a final contractor report. Test
Protocols for Determining the "Free
Liquid" Content of Hazardous Waste
for public comment. The Agency is
preparing a final rule to identify the test
protocol to be used to implement the
rale restricting "free liquids" in
hazardous waste landfills. The report
summarizes the results of laboratory
tests on a number of test protocols,
including the paint filter test that the
Agency proposed in the Federal Register
on February 25.1982. The Agency
requests comments on this report, and
serveral related specific issues.
DATES: Comments on the report must be
submitted on or ber'ore January 27,1984.
ADDRESS: Comments should be
addressed to the Docket Clerk, Office of
Solid Waste (WH-562), U.S.
Environmental Protection Agency, 401 M
Street. SW., Washington, D.C. 20460,
telephone (202) '382^4672. Comments
should identify the regulatory docket
and report title_as follows:
"Section 30T54. Test Protocol for
Determining the "Free Liquid" Content
of Hazardous Waste".
A copy of the report is available for
reading in the EPA Library and the
Subtitle C Docket Room (Room S-212A),
both located at the above address,
dunng the hours of 9:00 a.m. to 4:00 p.m.
Monday through Friday excluding
holidays. Copies of the report are also
available for reading at the EPA
Regional Libraries.
FOR FURTHER INFORMATION CONTACT:
For a single copy of the report contact
the RCRA Hotline at (800) 424-9346 (toll
free) or at (202) 382-3000. For additional
information contact Paul C^jsidv at
(202) 382-4682.
SUPPLEMENTARY INFORMATION: The
Agency promulgated interim status
standards on May 19,1980, in 40 CFR .
265.314 (45 FR 33249-50) that prohibit
the disposal of containerized liquid
waste or waste containing free liquids in
a hazardous waste landfill. This
prohibition went into effect on
November 19,1981. These standards
also require that bulk liquids must not
be placed in a hazardous waste landfill
unless (1) the landfill is equipped with a
liner which is chemically and physically
resistant to the liquid, and a functioning
leachate collection and removal system
with a capacity to remove ail the
leachate produced, or (2) prior to
disposal, the-bulk liquids are treated so
that free liquids are no longer present
when the waste is placed in the landfill.
The date of compliance for this
requirement was also Novmeber 19.
1981. In the May 19, 1980 regulations the
Agency also defined free liquid as
"liquids which readily separate from :he
solid portion of a waste under ambier,:
temperature and pressure" (40 CFR
260.10). In the May 19.1980 preamble {45
FR 332141 the Asency sueeested and
described the use of an "inclined plane"
test as a means to determine (in those
cases where it is not obvious) if a waste
contains "free liquids."
On February 25,1982 (47 FR 8311-13),
the Agency proposed a paint filter test
that could be used to determine the
presence of free liquids. Prior to this
date, the Agency initiated a study to
evaluate all the various test protocols
that could be used to determine the
uxini^rcf1 ei'fr°e liquid" i~ 'lud?/:?
semi-solids, slurries, and other waste
types. The study identified a wide range
of possible test protocols (75 in number)
that could be used. This number was
trimmed down to 19 as potentially useful
for determining the presence of free
liquids in wastes, and was then further
reduced to six for laboratory testing.
The six protocols include an inclined
plane test, a lab press, a filtration test, a
graduated cylinder test, a sieve series.
and a paint filter test.
The report being made available
today, Test Protocols for Determining
:r:e "Free Liquid" Content of Hazardous
Waste, contains the summary and
evaluation of the laboratory test results
of these six test protocols. Five non-
hazardous waste matenals were used to
evaluate the test protocols. The five
materials were selected because their
physical properties are representative of
the physical properties of typical
hazardous waste sludges. The five
waste materials were: drilling mud. air
pollution control sludge, paper sludge,
separator sludge, and paint sludge. The
report also includes an evaluation of the
suitability of various absorbent
matenals to transform a liquid was: ,:
waste with free liquids into a waste trial
no longer contains free flowing iiquics.
The Agency specifically requests
comments on the accuracy and
completeness of the information
presented in the report, especially
regarding the paint filter test parts of the
report. EPA encourages commenters to
suggest remedies or alternatives should
any inaccuracy or incompleteness be
identified. The Agency is particularly
interested in specific comments on the
following issues addressed in the report.
(1) Whether five minutes is an adequate
test period for determining the presence
of absence of free liquids in a waste. (2)
Should a standard watchglass be used
in the test and would the use of a
standard watchglass present any
problems? (3) Should the funnel used in
the paint filter test be fluted to facilitate
moisture flow?
Under Executive Order 12291, EPA
must judge whether a regulation or rule.
including any implementation guidance.
is "Major" and therefore subject to the
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SW-969
TEST PROTOCOLS FOR DETERMINING THE "FREE LIQUID"
CONTENT OF HAZARDOUS WASTE
This document (SW-969) was prepared for the Office of Solid Wast,e
under contract no. 68-01-3911
C... _'., .'.;_::,;, oUb04 ,
U.S. ENVIRONMENTAL PROTECTION AGENCY
December 1983
-------
u.
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THE EFFECT OF FLY ASH ON THE
"FREE LIQUID" CONTENT OF AIR POLLUTION
CONTROL EQUIPMENT SLUDGE
Test
Number
Fly Ash(g)
40
5 min.
15 min.
30 min.
5 min.
15 min.
30 min.
39
37
Replication
1
2
1
2
1
2
3
1
2
3
1
2
3
1
2
1
2
1
2
" Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
trace
2.0*
0.0
1.0*
2.0*
0.0
1.0*
trace
trace
1.0*
3.0
1.0*
3.0
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF FLY ASH ON THE
"FREE LIQUID" CONTENT OF SEPARATOR SLUDGE
Test
Number
Time
5 min.
15 min.
5 min.
15 min.
5 min.
15 min.
Fly Ash(g)
20
18
17
Replication
1
2
1
2
1
2
1
2
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
trace
trace
-------
Table of Contents
EXECUTIVE SUMMARY 1
1.0 INTRODUCTION 2
2.0 TESTING METHODOLOGY 5
2.1 Test Materials 5
2.1.1 Introduction 5
2.1.2 Drilling Mud 5
2.1.3 Air Pollution Control Equipment
Sludge 5
2.1.4 Paint Sludge 6
2.1.5 API Separator Sludge 6
2.1.6 Paper Sludge 7
2.2 Test Protocols 8
2.2.1 Introduction 8
2.2.2 Inclined Plane 8
2.2.3 Lab Press 13
2.2.4 Filtration Unit 16
2.2.5 Graduated Cylinder Test 21
2.2.6 Sieve Series 22
2.2.7 Paint Filter Test 24
3.0 EVALUATION OF SELECTED TEST PROTOCOLS 27
3.1 Inclined Plane 27
3.2 Lab Press 28
3.3 Filtration Unit 29
3.4 Graduated Cylinder Test 30
3.5 Sieve Series 31
3.6 Paint Filter 32
4.0 EVALUATION OF SELECTED ABSORBENT MATERIALS 36
4.1 Introduction 36
4.2 Permasorb #29 37
4.3 TriPak Solidification Medium 38
4.4 Drilling Mud 39
4.5 Safe-N-Dri 41
4.6 Vermiculite 43
4.7 Cement Kiln Dust 44
4.8 Hazorb 45
4.9 Fly Ash 46
CONCLUSIONS 49
RECOMMENDATIONS 53
APPENDICES
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EXECUTIVE SUMMARY
Six test protocols were laboratory tested and evaluated
by SMC Martin to determine the "free liquid" content of five
waste materials. The test protocols evaluated included an
inclined plane test, a lab press, a filtratioh test, a
graduated cylinder test, a sieve test, and a paint filter
test. The paint filter test was proposed on February 25,
1982 by the U.S. Environmental Protection Agency (EPA) to be
used as a pass/fail test to determine the presence of "free
liquid" in sludges and semisolids.
Five waste materials were used to evaluate the test
methods selected for laboratory testing. Waste materials
were also used to evaluate the suitability of various absorb-
ent materials. The selected wastes encompassed a variety of
textural types and included drilling mud, air pollution
control equipment sludge, paint sludge, separator, and paper
sludge.
The absorbent materials tested included drilling mud,
fly ash, vermiculite, cement kiln dust, Hazorb, Safe-N-Dri,
Permasorb #29, and TriPak Solidification Medium. Various
amounts of each absorbent material were added to the wastes
until no "free liquid" was present when tested with the
paint filter test. In general, Permasorb #29 was the most
absorbent material tested and fly ash was the least absorbent.
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1.0 INTRODUCTION
On December 18, 1978 the U.S. Environmental Protection
Agency (EPA) proposed minimum national standards for hazardous
waste disposal facilities under Section 3004 of the Resource
Conservation and Recovery Act (RCRA). In an attempt to
maximize the containment of wastes in a landfill, EPA proposed
in the regulations that liquid hazardous wastes not be
disposed of in a landfill unless the wastes were treated
(i.e., mixed with absorbent material) prior to landfilling,
or were treated by in-situ absorbtion in the landfill until
a nonflowing consistency was achieved.
EPA promulgated interim status regulations on May 19,
1980 which prohibited the disposal of containerized liquid
hazardous wastes or waste containing "free liquids" in a
landfill on or after November 19, 1981. At this time, EPA
also defined "free liquids" as "liquids which readily separate
from the solid portion of a waste under ambient temperature
and pressure." The use of an inclined plane test was also
suggested to be used to determine if specific wastes contained
"free liquids."
Wastes or "free liquids" not absorbed or attenuated in
a landfill can migrate through the landfill producing leachate.
In an unlined landfill, leachate will percolate downward
through the waste-soil matrix to the water table. The
leachate then forms a plume of contamination which joins the
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ground-water flow system and may ultimately discharge to
surface waters.
On February 25, 1982, EPA proposed an alternative
standard for limiting the landfilling of containerized "free
liquid" waste. The proposed standard limited the amount of
containerized "free liquids" that could be placed in a
landfill. These containerized "free liquids" could be
landfilled provided that the volume of such containers did
not exceed a formula-determined fraction of the total volume
of wastes, and reasonable intermediate cover to be placed in
the landfill. EPA also proposed the use of a paint filter
test to determine the presence of "free liquid" in individual
wastes. In order to encourage compliance with the regulations,
EPA also exempted from the requirements of the hazardous
waste management regulations, the acts of adding absorbent
material to hazardous wastes in containers and adding hazardous
waste to absorbent material in a container, at the time
waste is first placed in the container, in order to reduce
the "free liquids" in a container. On March 22, 1982, EPA
once again promulgated interim restrictions prohibiting the
landfilling of containers holding "free liquids" unless
1) all free standing liquids have been removed by decanting,
or other methods; 2) have been mixed with an absorbent or
solidified so that free standing liquid is not longer ob-
served; or 3) have been otherwise eliminated.
-------
SMC Martin was retained to evaluate testing methods
which could determine the amount of "free liquid" in waste
materials. The study also evaluated the ability of selected
materials to absorb "free liquid" in wastes. This report is
a summary of the testing program and is submitted as a
supplement to the interim reports previously completed.
Details of individual tests, previously submitted to EPA,
are not included in this report.
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2.0 TESTING METHODOLOGY
2.1 Test Materials
2.1.1 Introduct ion
EPA and SMC Martin selected five nonhazardous
waste materials to evaluate test protocols selected for
laboratory testing. Wastes were selected with a variety of
textural characteristics in order to evaluate the test
protocols under varying test conditions. The selected
materials included those which could be classified as gela-
tinous, granular, oily, and fibrous in nature. The materials
chosen for testing were drilling mud, air pollution control
equipment sludge, paint sludge, separator sludge, and paper
sludge.
2.1.2 Drilling Mud
Drilling mud is a finely-ground, sodium-based
montmorillonite, western bentonite and is composed of mont-
morillonite, quartz, feldspar, cristobalite, illite, calcium,
and gypsum. Water was added to the drilling mud until the
mixture consisted of 89 percent water by weight. It is a
gelatinous type of material capable of absorbing large
quantities of water over time. When the drilling mud and
water were thoroughly mixed, no phase separation was observed.
2.1.3 Air Pollution Control Equipment Sludge
Air pollution control equipment sludge is formed
from dust collected from baghouse fabric filters, which are
5
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a part of the air pollution control program for steel mills.
Dust-bearing gases produced during scrap metal melting pass
through filters which trap dust particles. The dust is a
granular-type of material containing a high percentage of
metals and inorganic particles. Since the dust is dry when
collected, water is added to create a waste suitable for
testing. It readily absorbs water and does not exhibit a
phase separation unless the mixture is mixed vigorously for
an extended period of time. The waste material used in the
study consisted of 34.5 percent water by weight.
2.1.4 Paint Sludge
Paint sludge is composed of water-based acrylic
spray paint used at a metal fabrication plant. During
painting, overspray is trapped in recirculated water and
accumulates in a sump as sludge. The paint sludge was
received as a dry solid mass of material; it was crushed
into a granular material to which water was added, producing
a suitable waste similar in nature to the original waste.
The final testing material was 26 percent water by weight
and a phase separation was noted.
2.1.5 API Separator Sludge
API separator sludge is a by-product of the purifi-
cation process of waste water produced from the production
of gasoline and gasoline additives. The waste consists of
silts and heavy metals from waste water which are collected
from a settling tank. The sludge used for testing contained
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a large quantity of oil liquid which readily separated from
the solids. Each time a sample was collected from the drum,
the waste was mixed thoroughly to obtain a representative
sample.
2.1.6 Paper Sludge
Paper sludge is dewatered Kraft bleached paper
board sludge and contains the following process wastes from
Kraft pulping: slaker rejects, burned lime rejects, and
green liquor dregs. The solids are composed of fiber,
filler, and coating clays. During collection, the sludge is
dosed with one percent (by volume) commercial formaldehyde
to inhibit biological activity.
The sludge is very dense and fibrous in nature. A
phase separation was visible in the drum and the solids
remained in the center of the drum surrounded by liquid.
Because of the high density of the material, it was difficult
to thoroughly mix the sludge to obtain a representative
sample.
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2.2 Test Protocols
2.2.1 Introduction
An in-depth literature search was conducted to
identify and evaluate test methodologies which could be used
to determine the "free liquid" content of hazardous wastes.
Sources of information included computerized data bases,
libraries, and professional contacts. Over 75 test protocols
were evaluated and 100 researchers were contacted for the
study. Specific protocols were selected and evaluated in
extensive laboratory testing with hazardous waste materials.
The tests chosen had to be safe, quick, and easy
to implement by the waste generator and/or landfill operator.
The test equipment had to be relatively inexpensive, readily
available, and applicable to all hazardous wastes. It was
also important to select tests which could simulate landfill
conditions with reproducible results.
Based on the above criteria, EPA and SMC Martin
chose the following six protocols for laboratory evalua-
tion: the inclined plane, lab press, filtration unit,
graduated cylinder, sieve series, the paint filter test.
The criteria for selection of each protocol is summarized in
Table 1.
2.2.2 Inclined Plane
The inclined plane was designed by EPA to determine
if sludges and semisolids contain "free liquid." It is a
simple phase separation test in which a 1-5 kilogram (Kg)
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sample is placed on a flat, smooth surface, cither level or
slightly sloping, for a test duration of at least five
minutes (see Appendix A). Testing apparatus is shown in
Figure 1. "Free liquid" is defined as any moisture which
separates from the sample and is collected and quantified in
milliliters (ml).
The test was selected for laboratory evaluation
since it is easily implemented by waste generators and/or
disposal operators and requires minimal operator training.
Test duration is short and equipment is readily available at
minimal costs. The surface of the tray used in the test was
glass, and collection/quantification apparatus were of
stainless steel. Testing materials used with the inclined
plane included drilling mud, air pollution control equipment
sludge, paint sludge, and separator sludge.
A phase separation of liquids and solids was
observed for the air pollution control equipment sludge,
paint sludge, and separator sludge. However, only the paint
sludge generated sufficient quantities of "free liquid" to
be quantified. Though a liquid/solid phase separation was
visible in most wastes, the liquid often remained on the
test surface and did not flow into the collection tray.
Therefore, the "free liquid" for drilling mud, air pollution
control equipment sludge, and separator sludge were recorded
as the movement of liquids and/or solids.
10
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Figure 1
INCLINED PLANE
LIQUID
COLLECTION
TRAY
13cm
ANGLE
ADJUSTER
BASE
38cm
11
-------
Since drilling mud is a gelatinous type of material
and phase separation of liquids and solids did not occur at
atmospheric pressure, movement of solids on the inclined
plane was recorded for each trial. As the angle increased,
the movement of drilling mud also increased.
"Free liquid" for the air pollution control equipment
sludge was recorded as the movement of liquids on the inclined
plane. The solid portion of each sample remained stationary
during testing. The movement of "free liquid" for all of
the tests, except one, flowed into the collection tray.
However, the liquid consisted of only a few drops which were
insufficient to quantify. As the angle increased, the
amount of time required for the liquid to reach the collection
tray decreased. Only one replication required more than
20 minutes for "free liquid" to reach the collection tray.
The paint sludge readily generated "free liquid"
which flowed into the collection tray and was quantified.
The liquid was cloudy and contained many solids. As the
angle increased, the percent "free liquid" generated also
increased, since pockets of liquid could separate from the
sample. The liquid separated from most of the solids within
20 minutes. The percent "free liquid" generated ranged from
40 percent at the highest angle to less than 1 percent at
the lowest angle.
The separator sludge contained "free liquid" which
consisted of both liquids and solids. While liquid did not
12
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enter the collection tray for all the test samples, the
entire sample moved along the plane for every test. The
movement of liquid and solids increased proportionally with
increasing the angles.
A drawback of the inclined plane deals with the
collection and quantification of "free liquid." Frequently,
liquids which reached the bottom of the plane adhered to the
bottom edge of the glass surface, and ran underneath the
glass. This liquid could not be collected for quantification
for any of the tests. Also bulk movement of the entire test
sample inhibited the separation process of liquids and
solids. Refinements of the testing apparatus would minimize
these problems.
2.2.3 Lab Press
The lab press is a pressure-dependent, phase
separation test. The test sample is placed in a test cylinder,
equipped with filtration screens, and pressure is applied by
a piston between two platen heads (see Figure 2). A pressure
gauge is used to regulate pressure throughout the test.
Liquid which is extracted within the 5-minute test duration
is trapped in a collection pan and quantified.
The test procedure is easily implemented by waste
generators and/or disposal operators. Some operator training
is required for applying and regulating the pressure from
the platen heads. Since pressure can be regulated, the test
is ideal for simulating pressures found in a landfill at
13
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Figure 2
LAB PRESS
PLATEN
HEAD
PLATEN
GAUGE
PLUNGER
. TEST
CYLINDER
^COLLECTION PAN
HYDRAULIC JACK
PUMP
HANDLE
-RELEASE VALVE
14
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The air pollution control equipment sludge generated
"free liquid" at the three highest pressures but not at the
two lowest pressures. A clear liquid was observed at the
top of the test cylinder at the conclusion of each test.
The "free liquid" generated by the air pollution control
equipment sludge ranged from 4 percent of the total weight
to less than 1 percent throughout the range of testing
pressures.
The paint sludge generated a cloudy, colorless
liquid at each of the test pressures which occurred in the
collection pan as well as the top of the test cylinder. The
solids remaining in the test cylinder were quite dense and
retained the shape of test cylinder. The "free liquid"
content of the waste ranged from 30 percent of the total
weight for the highest test pressure to 7 percent for the
lowest test pressure.
The "free liquid" generated by the separator
sludge collected at the top of the test cylinder but did not
pass through the filter plate into the collection pan at the
base of the cylinder. The liquid consisted of a colorless,
cloudy liquid and a brown oil-like liquid. The solids
remaining in the test cylinder formed a small dense layer of
sludge on the surface and bottom of the sample. The portion
of the sample between these dense layers appeared to be
unchanged. The "free liquid" generated by this test ranged
15
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from 12 percent of the total weight at the highest pressure
to 3 percent at the lowest pressure.
Several drawbacks were noted during the lab press
evaluation. During individual tests, it became difficult to
maintain a constant pressure on each test sample. As liquid
was extracted from the solids, the volume of the material
decreased and, therefore, the pressure also decreased,
requiring frequent adjustments. Furthermore, due to the
inherent inaccuracy of the gauge, all pressures were
approximate.
An additional difficulty observed during testing
involved the alignment of the plunger and the cylinder.
Many times, the plunger jammed against the side of the test
cylinder, preventing an even pressure distribution on the
test material, even though pressure registered on the gauge.
Reaction of wastes with the test cylinder was also
observed during the study. During the testing of the air
pollution control equipment sludge, the waste reacted with
the test cylinder and plunger, resulting in corrosion of the
cylinder.
2.2.4 Filtration Dnit
The filtration unit is a pressure-dependent phase
separation test originally developed for the extraction
procedure (EP) toxicity test (see Figure 3). The test
sample is placed in a test cylinder with a 0.45 micrometer
pore-size filter membrane. Pressure is applied to the test
16
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Figure 3
FILTRATION UNIT
TRI-CLAMP
TEST
CYLINDER-
r1
HOSE TO
NITROGEN TANK
OUTLET
RELIEF VALVE
HAND WHEEL
BOLTS
TOP PLATE
-BOTTOM PLATE
17
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sample by a compressed inert gas (see Appendix C). A gauge
is used to maintain a constant pressure throughout the test.
Any liquid extracted in the 30-ininute test duration is
collected and quantified.
Some operator training is required to operate the
unit. The test is easily implemented by the waste generator
and/or disposal operator and pressures encountered in landfills
at various depths can be simulated. Although the cost of
the filtration unit was greater than the other test protocol
methods evaluated, it is readily available and required only
routine maintenance. The internal parts of the filtration
unit used in this study were teflon coated to minimize
reaction with the wastes.
The filtration unit is a phase separation test
which simulates pressures found in a landfill at 100, 80,
60, 40, and 20-foot depths. Compressed nitrogen acts as a
piston-like force, extracting "free liquid" from the test
sample. The filtration unit was evaluated by testing drilling
mud, air pollution control equipment sludge, paint sludge,
and separator sludge. Phase separation of liquids and
solids was both waste and pressure dependent. The drilling
mud was the only waste which could be tested at the five
pressures for the specified 30-minute test duration. During
the air pollution control equipment sludge and the paint
sludge testing, pressures greater than 22 psi (simulated
18
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landfill pressure at a 60-foot depth), caused the nitrogen
to pass through the sample and out the base of the filtration
unit. As a result, no pressure was applied to the test
material. A similar situation occurred with the separator
sludge, wherein nitrogen would pass through the sample for
test durations greater than several minutes.
During testing of the drilling mud, the "free
liquid" extracted varied proportionally with pressure through
the lowest pressures. However, "free liquid" extracted at
the two highest pressures (80-foot and 100-foot depth pressures)
was less than the "free liquid" extracted at the simulated
landfill depths of 40 and 60 feet. The drilling mud remaining
in the filtration unit maintained fluid-like characteristics
at the completion of the test. The "free liquid" extracted
from the test samples ranged from 5.69 percent at the highest
pressure to less than 1 percent at the lowest pressure.
Air pollution control equipment sludge was only
tested for the two lowest pressures to prevent nitrogen
channeling through and around the samples. The average
"free liquid" extracted at these two pressures ranged from
9 percent for the lower pressure to 12 percent for the
higher pressure. After testing, the remaining sample formed
a crusty layer at the surface and no longer exhibited a
phase separation.
The paint sludge was also tested for only the two
lowest pressures. The results for both tests were quite
19
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variable and in general, more "free liquid" was extracted
during the lower pressure test than the higher pressure
test. The "free liquid" ranged from 19 percent at the lower
pressure to 24 percent for the higher pressure. The paint
sludge remaining in the unit no longer exhibited a phase
separation and was granular in texture.
The separator sludge was tested at all pressures
but only for a test duration of 20 minutes. As the pressure
increased, the amount of "free liquid" extracted also in
creased. The "free liquid" ranged from 11 percent at the
lowest pressure to 23 percent at the highest pressure. The
separator sludge remaining in the unit maintained fluid-like
characteristics.
Drawbacks encountered when testing with the filtra-
tion method included: nitrogen passing through the test
sample, quantification of "free liquid", and clogging of the
membrane filters. The unit is designed with a slight depres-
sion on the base plate of the unit. Liquid collects in this
depression and does not readily drain from the unit into the
collection beaker. However, this liquid can be poured into
the collection beaker at the completion of each test.
Visible clogging of the membranes was observed for the
separator sludge. The results for drilling mud indicate
that clogging occurred for the two highest pressures.
20
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2.2.5 Graduated Cylinder Test
The graduated cylinder test is a gravity-dependent
phase separation test developed by EPA. A 100-ml representative
sample is placed in a 100-ml graduated cylinder. The cylinder
is capped and agitated until it is well mixed. Any liquid
which separates from the solids in a 24-hour test duration
is considered "free liquid" and is quantified in milliliters
(see Appendix D).
The test procedure is very simple and easily
implemented by waste generators and/or disposal operators.
The test equipment is readily available at minimal cost and
minimal operator training is required. Graduated cylinders
constructed of glass provide nonreactive surfaces and are
recommended for testing to prevent reaction with the samples.
Two trials were performed for each waste. Drilling
mud was not tested since drilling mud is gelatinous in
nature and typically exhibits a phase separation only under
pressure. Air pollution control equipment sludge, paint
sludge, separator sludge, and paper sludge were used to
evaluate the graduated cylinder test.
A phase separation of liquids and solids was
observed for all the wastes except the paper sludge. Solids
from the air pollution control equipment sludge settled
unevenly during the test. The "free liquid" ranged from
4.5 percent to 5 percent by volume.
21
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"Free liquid" from separator sludge ranged from
3 percent to 4 percent of the test sample.
Only one trial of the paint sludge produced "free
liquid"; in the remaining test, the solids did not settle
after agitation and adhered to the sides of the cylinder
above the 100-ml mark. However, after tapping the base of
the cylinder, the solids settled and 5 percent "free liquid"
was observed.
The quantity of "free liquid" produced by each
waste was also time-dependent. Each waste produced various
amounts of "free liquid" at different intervals. "Free
liquid" was first observed for the air pollution control
equipment sludge after 15 minutes and stabilized after four
hours. The paint sludge exhibited "free liquid" after ten
minutes of testing and also stabilized after four hours.
"Free liquid" was not observed for the separator sludge
until 30 minutes of testing had elapsed and did not stabilize
until after six hours of testing.
2.2.6 Sieve Series
The sieve test is a gravity-dependent phase separa-
tion test recommended by EPA. A 200-ml representative
sample of a waste is placed in a series of 10, 18, 35, and
60-mesh screens. The sieves were agitated for a 5-minute
test duration. Any liquid which penetrated the bottom
screen (60-mesh) was collected and quantified in milliliters
(see Appendix E).
22
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The test is simple, requiring minimal operator
training and suitable for either the waste generator and/or
disposal operator. The test attempts to simulate conditions
found in transporting wastes and addresses the problem of
"free liquid" settling from solids due to agitation. The
equipment is readily available but should be constructed of
a nonreactive material.
In this test, liquid is separated from solids by
shaking and gravity. Since drilling mud is gelatinous in
nature and only exhibits a phase separation under pressure,
it was not evaluated with the sieve series. Test materials
evaluated included air pollution control equipment sludge,
paint sludge, separator sludge, and paper sludge.
Phase separation of liquids and solids was observed
for all the test materials. However, liquid produced by the
paint sludge did not pass through the final (60 mesh) sieve
while liquid produced by the paper sludge did not pass
through the 60 or 35-mesh sieves.
Liquid produced by the air pollution control
equipment sludge and the separator sludge did pass through
the final sieve and was considered "free liquid." However,
the results were variable for both wastes; therefore, four
replications were conducted for the air pollution control
equipment sludge and five replications were conducted for
the separator sludge. The "free liquid" that was quantified
for the air pollution control equipment sludge constituted
23
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less than 2 percent of the total test material. "Free
liquid" for the separator sludge ranged from less than
2 percent to 5 percent of the total amount of material
tested.
2.2.7 Paint Filter Test
The paint filter test is a gravity-dependent phase
separation test developed by EPA (see Figure 4). A representa-
tive, 100 ml sample of a waste is placed in a paint filter
which in tarn is placed in a funnel. The funnel is supported
by a graduated cylinder and covered with a watch glass. Any
liquid which drains into the graduated cylinder in a 15-minute
test duration is quantified in milliliters (see Appendix F).
Liquid which passes through a paint filter is collected in a
graduated cylinder and quantified at 15-minute intervals;
the test continues until the change in "free liquid" per
interval is less than 10 percent.
The paint filter test is easily implemented by
waste generators and/or disposal operators. Since the
procedure is simple, minimal operator training is required.
Equipment is readily available, and the cost is minimal.
The funnel and graduated cylinder were constructed of glass.
Air pollution control equipment sludge, paint sludge, separator
sludge, and paper sludge were employed in this test. A
phase separation of liquids and solids was observed for all
the wastes.
24
-------
RING STAND
PAINT FILTER
FUNNEL
JBJ
-GRADUATED CYLINDER
PAINT FILTER TEST
Figure 4
25
-------
The air pollution control equipment sludge generated
only a trace of "free liquid" during one replication. No
"free liquid" was generated in the second replication.
The paint sludge produced "free liquid" for both
trials. The liquid constituted 6 percent of the test sample
volume. For the paint sludge, both tests were conducted for
45 minutes.
"Free liquid" was also noted in both trials of the
separator sludge. The liquid ranged from 5.5 percent and
6.5 percent of the test sample. The test duration for the
separator sludge was one hour.
The paper sludge produced the largest quantity of
"free liquid", and the test encompassed the longest period
of time. After a duration of one hour and 45 minutes,
8.5 percent and 9.5 percent of the sample volume was generated
as "free liquid."
26
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3.0 EVALUATION OF SELECTED TEST PROTOCOLS
3.1 Inclined Plane
The inclined plane was capable of determining the
presence of "free liquid" in several wastes. A phase separa-
tion of liquid and solids was observed for granular and oily
types of wastes (paint sludge, air pollution control equipment
sludge, and separator sludge). The gelatinous type of waste
(drilling mud) did not exhibit any phase separation. However,
it did exhibit fluid-like characteristics by moving down the
surface of the plane as a cohesive unit of liquids and
solids. Only the paint sludge generated sufficient quantities
of "free liquid" to be quantified.
The test procedure is simple and easy to implement;
materials required for construction of the inclined plane
are readily available and inexpensive. The test duration
was waste dependent. The granular wastes (air pollution
control equipment sludge and paint sludge) required less
time for "free liquid" to reach the collection tray than the
oily waste. As the angle increased, the time required for
"free liquid" to reach the collection tray decreased for all
the wastes. However, testing angles of 35° and 45° proved
to be excessive, since solids were observed moving down the
plane and into the collection tray.
The reproducibility of the test results were waste and
angle dependent. As the angle increased for testing drilling
27
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mud and paint sludge, the results became more variable. The
reverse was true for the air pollution control equipment
sludge and separator sludge; as the angle increased, the
test results became less variable.
Accurate quantification of "free liquid" proved to be
difficult in several test cases. Also, movement along the
plane of entire test samples occurred several tines, espe-
cially at steep test angles. Both problems are due at least
in part to design flaws in the construction of the inclined
plane. A barrier to prevent bulk movement of the sample
would minimize the drawbacks of the test. If the sample was
also contained within a porous material (e.g. filter paper
or screen), the separation of liquids from the sample could
be increased. One-piece construction of the plane and
collection tray, possibly constructed of glass, polycarbonate,
or similar material, would eliminate any losses of "free
liquid."
3.2 Lab Press
The lab press was capable of determining the "free
liquid" content of test materials at various simulated
landfill depths. "Free liquid" was quantified for all four
wastes tested with drilling mud being the only waste which
generated solids. The lab press is relatively simple to
operate with a short test duration. The required equipment
is readily available, though the initial capital investment
is relatively high.
28
-------
Although the procedure is simple and the test duration
is short, several drawbacks were encountered during testing.
Proper alignment of the piston and test cylinder is critical
to proper execution of the test. When the alignment was not
perfect, the test plunger would jam against the sides of the
test cylinder. Though this situation can be minimized
through operator experience, it remains a liability of the
test. The test cylinder must be cleaned after every test,
which is a cumbersome job given the numerous parts which
comprise the cylinder. If the test cylinder is not thoroughly
cleaned between trials, accuracy of the test would be severely
impaired, an additional liability.
Another problem affecting the efficiency of the lab
press is potential reaction of the test cylinder with certain
wastes. In this study, the air pollution control equipment
sludge reacted with the test cylinder producing slight
corrosion. To limit this possibility, test cylinders con-
structed of less reactive materials should be employed.
3.3 Filtration Unit
Although the test procedure is fairly simple, the
initial capital investment is high. Prefilter and membrane
filters must be replaced for every test and are relatively
expensive. The 30-minute test duration required for the
majority of "free liquid" to be extracted from the sample is
marginally acceptable.
29
-------
At the lower range of testing pressures, the unit
performed well, yielding satisfactory results for most
wastes. However, it cannot be expected to successfully
simulate the range of landfill pressures.
Since the prefilters and membrane filters must be
replaced after each test, cleaning of the unit itself is
relatively simple and should not limit accuracy through
long-term use. The cost of the expendable filters will add
considerably to annual operating cost for the unit and will
pose an additional, although minor, problem concerning
disposal of the spent filters.
The filtration unit was not capable of adequately
testing any of the wastes for free liquid. The gelatinous
material (drilling mud) clogged the membrane filters at the
higher testing pressures. The granular materials (air
pollution control equipment sludge and paint sludge) could
not be tested at the higher testing pressures since the
compressed nitrogen passed through the test sample and out
the base of the unit. The oily type of waste (separator
sludge) was tested for all the simulated landfill depths,
however, after 20 minutes of testing, the compressed nitrogen
passed through the test sample and out the base of unit.
3.4 Graduated Cylinder Test
The graduated cylinder test is an adequate test for
determining the "free liquid" for certain types of wastes.
A phase separation of liquids and solids was observed for
30
-------
the granular wastes (air pollution control equipment sludge
and paint sludge) and the oily waste (separator sludge).
However, the fibrous material (paper sludge) did not generate
any "free liquid." The gelatinous type of testing material
(drilling mud) was not tested since a phase separation will
only occur under pressure.
The test is very simple and easy to implement. Supplies
are readily available, inexpensive, and test results were
quite reproducible. The test duration employed in this
study (24 hours) is impractical for use by either the waste
generator or disposal operator. It should be noted that in
most of the testing, the majority of the "free liquid"
separated from the solid portion of the sample within 4 to
6 hours. It is possible that for the purposes of field
testing, the test duration could be shortened without sacri-
ficing accuracy. Given the overall simplicity of the test
and reproducibility of the trials, the test should be given
serious consideration.
3.5 Sieve Series
The sieve series test was capable of determining the
"free liquid" content of specific wastes. A phase separation
of liquids and solids was observed for all the test materials,
however, only the liquids generated from the air pollution
control equipment sludge and separator sludge penetrated the
final (60-mesh) screen. "Free liquid" was quantified for
both wastes.
31
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The test is very simple, easy to implement, and supplies
are readily available at moderate cost. The test duration
is short and practical for use by the waste generator or
landfill operator. It simulates the effect of agitation on
the potential phase separation of the waste. The results of
the test were erratic, however, and were not reproducible
for the wastes tested. Also, it should be noted that the
wastes could clog the screens making thorough cleaning of
the screens difficult. The inconsistent results obtained
from this test eliminate the sieve series test from further
consideration.
3.6 Paint Filter
The paint filter test was capable of determining the
presence of "free liquid" for all the wastes tested. A
liquid/solid phase separation was observed for each waste
and was sufficient to quantify for each waste with the
exception of the air pollution control equipment sludge.
This waste only produced a trace of "free liquid" during
only one of the trials.
The test procedure is simple and easy to implement by
the waste generator or landfill operator. Supplies are
inexpensive and readily available. Though the paint filters
must be replaced after each trial, their cost is low (generally
between $0.07 and $0.89) and they are generally available at
local paint stores. The least expensive filters are paper
32
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and are disposable, and the finest mesh size available is a
60 mesh. These are the type of filters used in the testing
program. The higher priced filters are of a plastic material,
are a much finer mesh (200 mesh), and can be reused if the
waste tested can permit thorough and proper cleaning.
Because of these low costs, no serious financial burden will
be placed on the waste generators or disposal operators.
The test duration is waste dependent with a minimum length
of 15 minutes for the initial procedures tested, including
Modification No. 1. Modification No. 2 had no specific time
limit applied and the results were generally reproducible.
In this study, the test performed well for all wastes
with the exception of the air pollution control equipment
sludge; when this waste was tested, a small amount of liquid
collected on the top surface of the waste and did not percolate
through the sample. However, when downward pressure was
applied to the watch glass, liquid filtered into the graduated
cylinder.
Modification No. 2 of the paint filter test appears to
be an adequate, quick, and simple test for determining the
presence of "free liquid" in varying waste types. A waiting
period of 15 minutes is suggested to determine if any "free
liquid" is present in the waste. Since the paint filter
test generally satisfies the requirements set by EPA for the
selection of a test protocol to determine the presence of
33
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"free liquid" in hazardous waste, it was selected by EPA for
further testing with absorbent materials.
At this time, it appears that several revisions to the
testing procedure could improve the overall reliability of
the paint filter test. For example, the test could be
evaluated with weights of varying sizes placed on the watch
glass. Pressure exerted by a weight on the watch glass
could: 1) simulate landfill pressures, and 2) generate a
more representative quantity of "free liquid" for each test.
Also, the funnel used for testing could be slotted or perfor-
ated, promoting drainage of "free liquid" from the test
sample.
34
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35
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4.0 EVALUATION OF SELECTED ABSORBENT MATERIALS
4.1 Introduction
EPA and SMC Martin selected the following absorbent
materials to be tested for determination of absorbtive
characteristics for "free liquid" of hazardous wastes:
Permasorb #29, TriPak Solidification Medium/ Quik-Gel drilling
mud, Safe-N-Dri, vermiculite, cement kiln dust, Hazorb, and
fly ash. The selection was based on the. following criteria:
1. Materials are easily obtained by most waste generators
and/or disposal operators.
2. Similarity of relative costs.
3. Ability to attenuate leachate.
4. Degree of absorbency, ratio of milliliters of
"free liquid" absorbed per ml of absorbent material.
The waste material selected for testing included paint
sludge, air pollution control equipment sludge, separator
sludge, and paper sludge. Since the air pollution control
equipment sludge did not generate sufficient quantities of
"free liquid" when tested with the paint filter test, additional
water was added to the waste prior to testing, resulting in
a test material consisting of 37 percent water by weight.
The four waste materials were tested with varying amounts of
each absorbent material to determine the amount of each
material required to reach the physical conditions where no
"free liquid" was present. This was determined by the paint
36
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filter test using a 15-minute test duration. The test was
directed at maximizing "free liquid" absorption while minimizing
the amount of absorbent material used.
4.2 Permasorb 129
Permasorb 129 is an industrial grade synthetic polymer
manufactured by National Starch and Chemical Corporation.
It is a granular solid which converts many aqueous-based
liquid wastes to solid gels and is capable of absorbing up
to 200 times its weight in water. The efficiency of the
product is dependent upon the ionic strength and pH of the
waste; high ionic concentrations and extreme pHs reduce the
absorbent capacity.
As illustrated in Figure 5, Permasborb 129 was an
efficient absorbent material for each waste tested. The
degree of absorbency varied with each waste and ranged from
9.10 to 1.28 ml absorbed per ml of absorbent (see Appendix G).
The effect Permasorb #29 had on the physical characteristics
of the wastes also varied with each waste.
The mixing of Permasorb #29 with the waste materials
prior to testing had various effects on the wastes. The
paint sludge, which required the least amount of Permasorb #29
to absorb the "free liquid," appeared granular and dry after
mixing. The air pollution control equipment sludge, separator
sludge, and paper sludge all appeared smooth and gelatinous
after mixing and did not appear as dry as the paint sludge.
However, they appeared to firm up over time.
37
-------
The paint sludge required the least amount of Permasorb #29
per ml of "free liquid" absorbed and had an absorbency ratio
of 9.1 ml absorbed per ml of absorbent. The air pollution
control equipment sludge required more Permasorb 129 to
absorb the "free liquid" and had an absorbent ratio of
2.8 ml absorbed per ml of absorbent. Both the separator
sludge and paper sludge generated less free liquid than the
paint sludge, but required more Permasorb |29 to absorb that
liquid. The absorbency ratios for the separator sludge and
paper sludge were 1.28 and 2.73 ml absorbed per ml of absorbent,
respectively.
Since a price was not available from the manufacturer
for Permasorb #29, it cannot be completely evaluated.
However, it is a valuable absorbent material for numerous
reasons, including its ability to increase the viscosity of
wastes over time, which in turn increases the ability of the
waste to retain "free liquid" under landfill pressure.
4.3 TriPak Solidification Medium
TriPak Solidification Medium is manufactured by Tri Resource
Industries as an absorbent for hazardous wastes and is a
composite of fullers earth, opal claystone, and other inert
absorbent materials. It is available in 50-pound bags or
steel and plastic 55-gallon drums. The price per bag is
approximately $7.50.
38
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The physical characteristics for each waste changed
with the addition of TriPak Solidification Medium. The air
pollution control equipment sludge and separator sludge had
a smooth paste-like texture after mixing. The granular
paint sludge also became paste-like but maintained visible
granules. The paper sludge remained fibrous but was drier.
The highest degree of absorbency for TriPak was
noted when testing with the granular, water-based, paint
sludge (sec Appendix H). Although the waste contains the
second highest percent "free liquid" for the wastes tested,
the absorbency ratio was 1.88 ml absorbed per ml of absorbent.
The granular, water-based, air pollution control equipment
sludge, and oily separator sludge, which contained the
highest and the lowest percent "free liquid" respectively,
had the lowest absorbency ratios for TriPak at 0.55 and
0.54 ml absorbed per ml of absorbent, respectively. The
fibrous paper sludge had an absorbency ratio of 0.71 ml
absorbed per ml of absorbent.
4.4 Drilling Mud
Quik-Gel drilling mud is a finely-ground, premium-grade,
sodium-based montmorillonite, western bentonite manufactured
by NL Baroid/NL Industries. It is a nontoxic viscosic
material used in fresh water or fresh water-based drilling.
Its physical composition consists of montmorillonite, quartz,
feldspar, cristobalite, ellite, calcium, and gypsum. It is
39
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readily available and costs approximately $8.17 per 50-pound
bag.
In general, the degree of absorbency for drilling mud
varied with each waste, but the effects on the physical
characteristics of each waste were similar. Although each
waste maintained its invididual characteristics after mixing
with the drilling mud (i.e. granular, oily, or fibrous),
they all appeared gelatinous-like in nature. The paint
sludge maintained its coarse granular but texture was held
together in a paste-like gelatinous medium. As the material
was being tested using the paint filter method, it appeared
to become drier over time. The air pollution control equipment
sludge appeared very smooth and gelatinous but after mixing,
it appeared wet at the surface. The wetness was absorbed
with mixing but reappeared when the material was being
tested in the paint filter. The separator sludge appeared
gelatinous and oily in nature, while the paper sludge was
gelatinous and fibrous. The paper sludge also appeared to
be wetter than the other wastes tested.
The highest absorbency ratio for drilling mud was
2.08 ml absorbed per ml of absorbent and was recorded for
the air pollution control equipment sludge, which generated
the most "free liquid" per 100 ml of waste material tested
(see Appendix I). Drilling mud had the lowest absorbency, a
ratio of 0.28 ml absorbed per ml of absorbent, for the paper
sludge. The paint sludge and separator sludge had absorbency
40
-------
ratios of 1.67 and 0.83 ml absorbed per ml of absorbent,
respectively.
Although the ability of drilling mud to attenuate "free
liquid" was waste dependent and highly variable, the absorbency
ratios for the individual wastes were relatively high in
comparison with the majority of the absorbent materials.
The product is readily available from the manufacturer and
because of its higher absorbency ratio, it is relatively
inexpensive. It is also a gelatinous type of material, and
like Permasorb #29, it increased the viscosity of the waste
over time, which increases the waste's ability to retain
"free liquid" under landfill pressure.
4.5 Safe-N-Dri
Safe-N-Dri is an absorbent material manufactured by Oil
Dri for the absorption of hazardous liquids. It is composed
of calcium bentonite and is available in three grades:
Safe-N-Dri Special, Safe-N-Dri Standard, and Safe-N-Dri
Powder. The Safe-N-Dri Special has uniform granules.
Safe-N-Dri Standard has large and small granules. Safe-N-Dri
Powder is a powder and has the highest water and oil absorbency
ratio (ml/gm absorbent). The powder was used for all testing.
/
The product is available in 50-pound bags at a cost of
$3.25 per bag.
Safe-N-Dri did not absorb "free liquid" as well as any
of the previously mentioned absorbent materials. However,
41
-------
in general, it was the least expensive absorbent product per
ml of material used, and it was applicable to the various
wastes tested.
The physical characteristics of each waste changed with
the addition of Safe-N-Dri: the paint sludge maintained its
larger granules; the air pollution control equipment sludge
was very smooth in texture; the paper sludge and separator
sludge exhibited a drier, grainy appearance, with a consistency
similar to a paste-like medium. The paper sludge also
maintained its fibrous-like nature.
Safe-N-Dri was up to ten times more absorbent for paint
sludge than for the other wastes tested (see Appendix J).
The air pollution control equipment sludge and separator
sludge had absorbency ratios of 0.19 and 0.17 ml absorbed
per ml of absorbent, respectively. The lowest degree of
absorbency, which was 0.11 ml absorbent per ml of absorbent,
was recorded for the paper sludge.
Safe-N-Dri is an inexpensive absorbent material that is
applicable to various types of wastes. However, the absorbency
ratios are not high, and although no "free liquid" was
observed during testing, two of the wastes appeared wet when
they were tested. Since the material is relatively inexpensive,
more Safe-N-Dri could be added to the wastes to achieve a
firmer, drier material, making Safe-N-Dri more productive.
-------
4.6 Vermiculite
Vermiculite is a granular, lightweight, micaceous clay
mineral. It is a highly absorbent material which is often
used for the absorption of hazardous wastes. It is available
in various grades and all tests were conducted with grade-
three Vermiculite. It is available in four-cubic foot bags
and costs approximately $6.25 per bag.
The absorbency ratio varied with each waste; the granular,
water-based, paint sludge required the least amount of
absorbent material to absorb the "free liquid" present (see
Appendix K). The absorbency ratio for Vermiculite and paint
sludge was 0.8 ml absorbed per ml of absorbent. This was
ten times more efficient than the lowest absorbency ratio of
0.08 ml absorbed per ml of absorbent for the oily separator
sludge. The granular, water-based, air pollution control
equipment sludge and fibrous paper sludge had absorbency
ratios of 0.15 and 0.12 ml absorbed per ml of absorbent,
respectively.
Vermiculite was the most expensive product per ml of
absorbent required to absorb "free liquid" and had low
absorbency ratios for three of the four wastes tested. The
wastes remained wet after the addition of Vermiculite indi-
cating that they would probably not retain potential "free
liquid" under landfill conditions or pressures. The addition
of more Vermiculite to absorb the potential "free liquid" is
43
-------
not considered to be a cost-effective alternative for the
waste generators or disposal operators.
4.7 Cement Kiln Dust
Cement kiln dust is a by-product from the process of
making cement; as limestone is heated in the kiln/ a dust is
generated and collected in stacks. It is a common absorbent
material used for hazardous wastes. The primary composition
is calcium and it is readily available to waste generators
or disposal operators located near a cement plant. The cost
would consist of loading and transportation costs.
The physical characteristics of each waste varied with
the addition of the kiln dust to the waste. The paint
sludge maintained a consistency of coarse granules with a
light and airy-like matrix. The air pollution control
equipment sludge was smooth and appeared wet at the surface.
The separator sludge was grainy, wet, and runny; while the
paper sludge was fibrous and wet.
Cement kiln dust was the only absorbent tested which
was effective for the oily separator sludge. The only
separator sludge generated the least amount of "free liquid"
per 100 ml of sample tested (see Appendix L). The absorbency
ratio for the separator sludge was 0.25 ml absorbed per ml
of absorbent. The lowest degree of absorbency was observed
for the paper sludge which had an absorbency ratio of 0.06 ml
absorbed per ml of absorbent. The air pollution control
44
-------
equipment sludge and paint sludge had absorbency ratios
of 0.09 and 0.13 ml absorbed per ml of absorbent, respectively,
Although the cement kiln dust was inexpensive, it was
also one of the least absorbent materials tested. This
increased volume of absorbent can be of concern when disposing
of wastes in a landfill because as the volume of absorbent
material required by a waste to attenuate "free liquid"
increases, the less space there is available to landfill
more wastes.
4.8 Hazorb
Hazorb is a general, all-purpose sorbent material
manufactured by Diamond Shamrock Corporation. It is comprised
of amorphous, inorganic, foamed silicate glass. It is inert
and will not react with hazardous materials, except hydro-
fluoric acid. Hazorb is formed into lightweight cellular
granules that are available in pillow (17" x 26" x 2") or
loose form. Tests were conducted using the loose form which
is available in cubic-foot bags. The approximate cost per
bag is $10.00.
Hazorb had the highest degree of absorbency for the
paint sludge, 0.28 ml absorbed per ml of absorbent (see
Appendix M). The air pollution control equipment sludge and
separator sludge, which generated the most and least amounts
of "free liquid" per 100 ml of test sample, respectively,
had absorbency ratios of 0.07 and 0.06 ml absorbed per ml or
absorbent, respectively. The absorbency ratio using Hazorb
45
-------
for the paper sludge was 0.08 ml absorbed per ml of absorbent,
After the addition of the Hazorb, the paint sludge remained
granular, but had a light airy matrix of fine paint sludge.
The air pollution control equipment sludge was smooth, runny
and wet at the surface. The separator sludge was grainy but
cohesive and wet, and the paper sludge remained fibrous and
wet.
Hazorb was one of the most expensive materials tested
because it was one of the least absorbent. More Hazorb
absorbent material was required to absorb 1 ml of "free
liquid" than compared to the other absorbents. It did not
demonstrate any particular affinity to one type of waste,
but had similar results for the granular, oily, and fibrous
type wastes.
4.9 Fly Ash
Fly ash is a fine-grained, amorphous, glassy material
generated by coal-burning power plants and is commonly used
as an absorbent material for hazardous wastes. Its elemental
composition varies with the parent coal and operational
characteristics. Fly ash is considered a waste product and
is readily available to many landfill operators and waste
generators. Much of the cost associated with using fly ash
would consist of loading and transportation charges.
t The fly ash had the most consistent absorbency ratio
observed in the course of the study (see Appendix N). The
46
-------
abosrbency ratio only ranged from 0.11 to 0.05 ml with air
pollution control equipment sludge, paint sludge, and separator
sludge being very similar to each other.
While the absorbency ratio was not waste dependent, the
physical effect the fly ash had on the wastes varied with
each waste material. After mixing with the fly ash, the
paint sludge was gritty and dry with less granules than when
mixed with other absorbent materials. The air pollution
control equipment sludge was smooth with fine grains, while
the seprator sludge was grainy and wet but held together as
a cohesive unit. The paper sludge was similar to the separator
sludge but was fibrous instead of grainy. Although each
waste increased in viscosity with the addition of fly ash,
only the paint sludge became dry in appearance; the other
wastes maintained some flowing or liquid-like characteristics.
The highest degree of absorbency for fly ash was recorded
for the air pollution control equipment sludge with a ratio
of 0.11 ml absorbed per ml of absorbent. However, the paint
sludge and separator sludge were very similar to the air
pollution control equipment sludge, with absorbency ratios
of 0.10 ml absorbed per ml of absorbent. These wastes had
an absorbency ratio twice that of the fibrous paper sludge
which was 0.05 ml absorbed per ml of absorbent.
Fly ash is similar to the cement kiln dust since it is
readily available and inexpensive to generators located in
47
-------
the vicinity of coal-burning power plants. Therefore, the
cost of adding larger quantities of fly ash to the waste
maintaining liquid-like characteristics should not pose a
problem. However, when there is concern with landfill
volumes, a more efficient absorbent material should be
utilized.
48
-------
CONCLUSIONS
The primary purpose of this study was to develop a test
method which could accurately determine the "free liquid"
content of hazardous wastes. However, the results of this
study indicate that no single test method described in this
report could accurately determine the "free liquid" content
of all wastes with reproducible results for all cases. The
four wastes tested with each protocol (excluding drilling
mud) represents a very small percentage of the numerous
types of hazardous wastes produced by the industrial sector.
Several test methods show promise for use as indicators
of the "free liquid" in wastes; however, the tests require
improvements in their design and/or test procedures to
increase their reliability. Modifications to the inclined
plane which would eliminate bulk movement of the sample down
the plane, and which would increase the efficiency of the
"free liquid" collection procedure, would considerably
improve the reliability of the inclined plane test. The
test does have potential and should be considered for any
future testing by EPA. Its low cost and ease of implementation
would minimize operator error and the costs incurred to
those required to use this test.
The filtration unit, which had the advantage of being
able to simulate landfill pressures, could not be used for
testing at the high pressures expected in deep landfills.
49
-------
However, testing at lower pressures was quick, fairly reliable
and the results were generally reproducible. The filtration
unit is expensive to purchase and maintain, especially given
that the prefilters and membrane filters must be changed
after each test at considerable cost.
The laboratory press is commercially available, but at
a high cost. Mechanical drawbacks were evident in this
test, especially during the alignment of the test sample
with the piston of the laboratory press. One of the wastes
used in this study reacted with the material of the test
cylinder producing corrosion. The complex assembly of the
test cylinder required very thorough cleaning which would be
time consuming. If the thorough cleaning was not followed
after each test, reliability of succeeding tests would be
questionable.
The graduated cylinder was inexpensive to purchase and
maintain, and the test methodology was simple and required
little operator training. Results were generally reproducible,
though the 24-hour test duration used in this study was
excessive and may not be feasible for operators and generators.
However, as shown in the testing, most of the "free liquid"
which was generated in each test, separated from the solids
within several hours. This test could warrant further
consideration by EPA.
The sieve series used for this study is available at
moderate cost from many commercial establishments. Though
50
-------
of short duration, the test generally did not yield reproduci-
ble results. Also, the test was only marginally successful
in separating "free liquid" from the remainder of the sample.
Since the sieve series did not yield reproducible results
for the waste materials evaluated, it should not be given
further consideration by EPA.
The paint filter was generally satisfactory in deter-
mining the "free liquid" content of all the wastes tested in
this study. Its success in the preliminary phases of the
study warranted using the paint filter for the latter stages
of the study in testing the absorbent materials. The paint
filter as tested in this study could not simulate landfill
pressures, which could limit its utility for EPA.
Eight absorbent materials were evaluated in this study
using the paint filter test. The absorbent materials were
selected to attempt to produce a variety of synthetic and
natural materials for testing. All the absorbent materials
tested were capable of absorbing various amounts of "free
liquid" present in the waste material. In general, Permasorb
No. 29 was the most absorbent material tested in this study
and fly ash, the least absorbent. The results for each
waste, using these materials, were reproducible, however, in
all cases. Vermiculite and Hazorb proved to be the most
espensive absorbent products per volume used in the study.
The least expensive absorbent materials on a volumetric
basis were Safe-N-Dri and drilling mud. Though not the most
51
-------
absorbent materials by volume, cement kiln dust and fly ash
should also be seriously considered since the cost of obtaining
these products is minimal/ and usually only dependent on the
transportation charges.
52
-------
RECOMMENDATIONS
Several of the test protocols evaluated in this study
warrant consideration by EPA for possible implementation.
Several of the test methods evaluated, such as the graduated
cylinder, inclined plane, and paint filter, provided accurate
reproducible data which could be used as a pass/fail basis
for "free liquid" determination. Furthermore, refinement of
these test protocols could lead to a more accurate determina-
tion of the "free liquid" content of these wastes. In this
regard, we recommend that EPA should select one or more of
these test methods for refinement and further testing.
While the five test materials used in this study encom-
passed a variety of textural types, further testing should
consider the selection of additional wastes to provide a
more rigorous evaluation of the test protocol selected by
EPA. For example, wastes which are corrosive or highly
reactive would certainly impact the selection of a test
protocol to evaluate "free liquid" of that waste.
The absorbent materials evaluated in this project
included varieties of synthetic and natural materials. No
recommendation for any one particular absorbent material
used in this study can be made. Of equal or greater importance
to the volumetric absorbtive capacity of absorbent material
used is a consideration of the compatibility of the hazardous
waste and the absorbent material used for codisposal.
53
-------
Further, the cost effectiveness of each absorbent material
is not only determined by the current retail price, but also
by the geographic location of the particular disposal site
in question. The location of any particular site will
answer questions regarding the transportation costs of
particular absorbent materials. A large quantity of the
various absorbent materials should be readily available to a
disposal operation, either by their proximity to a cement
plant or a coal-fired power plant, in the case of cement
kiln dust and fly ash, or by their easy accessability in the
market place.
54
-------
APPENDIX A
TEST PROTOCOL RESULTS FOR THE DETERMINATION
OF "FREE LIQUID" BY THE INCLINED PLANE
-------
THE DETERMINATION OF "FREE LIQUID"
BY THE INCLINED PLANE
Test Procedure
Summary of Method
A sample of test material is placed on an inclined
plane. "Free liquid" drains from the test material by
gravity. The liquid is collected and quantified.
Apparatus
1. Inclined plane: An inclined plane from 0° to 45°
and capable of supporting a 1 kg test sample.
2. Collection tray: A collection tray capable of
collecting any "free liquid" that separates from the test
material.
3. Surface: A nonreactive surface which can be
removed from the inclined plane for cleaning.
General Procedure
1. Adjust the inclined plan to the desired angle.
2. Weigh 1 Kg of testing material
3. Place the sample along a straight line (parallel
to the top and bottom of the plane) on the surface of the
plane.
4. Record any linear movement, change in movement, or
phase separation of the test material over a predetermined
test duration (durations from 5 to 30 minutes were used).
-------
5. Collect all the "free liquid" that has separated
from the solids.
6. Calculate the "free liquid" in the original test
sample:
weight of "free liquid" x 100 = % "free liquid" of
weight of original test sample
test sample
-------
MOVEMENT OF DRILLING MUD ON THE INCLINED PLANE
Angle
5°
5°
5°
5°
5°
10°
10°
10°
10°
10°
15°
Replication
1
2
3
4
5
1
2
3
4
5
1
TjLme
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
Movement
1.5
NC
NC
2.0
NC
NC
2.0
NC
KG
1.0
1.25
KG
1.5
NC
NC
5.0
5.75
NC
4.5
NC
NC
6.0
NC
NC
7.0
8.5
NC
5.75
NC
NC
13.0
15.0
NC
-------
MOVEMENT OF DRILLING MUD ON THE INCLINED PLANE
(coninued)
Angle
15°
15°
15°
15°
20°
20°
20°
20°
20°
Replication
2
3
4
5
1
2
3
4
5
Time
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
5
10
15
min.
min.
min.
min.
min.
min.
min .
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
Movement (cm)
12.25
14.5
15.0
10.5
14.5
16.0
7.5
NC
NC
8.0
NC
NC
17.5
20.0
22 +
20.5
22 +
NC
17.0
17.5
NC
22 +
NC
NC
22 +
NC
NC
NC No Change
-------
MOVEMENT AND COLLECTION OF "FREE LIQUID" FOR AIR POLLUTION
CONTROL EQUIPMENT SLUDGE ON THE INCLINED PLANE
Angle
5°
5°
5°
5°
5°
15°
15°
15°
15°
Replication Time
1 5
10
20
30
2 5
10
20
30
3 5
10
20
30
4 5
10
20
30
5 5
10
20
30
1 5
10
20
30
2 5
10
20
30
3 5
10
20
30
4 5
10
20
30
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
Movement
1.25
20.5
22 +
NC
5.0
22+
NC
NC
0.5
22+
NC
NC
10.5
22+
NC
NC
0.5
22+
NC
NC
7.5
22+
NC
NC
1.25
22+
NC
NC
0.5
19.0
22 +
NC
16.0
22+
NC
NC
1.1
1.95
1.85
1.7
0.9
1.5
0.0
0.0
2.6
-------
MOVEMENT AND COLLECTION OF "FREE LIQUID" FOR AIR POLLUTION
CONTROL EQUIPMENT SLUDGE ON THE INCLINED PLANE
(continued)
Angle
15°
25°
25°
25°
25°
25°
35°
35°
35°
Replication Time Movement (cm) F:
5 5 min.
10 min.
20 min.
30 min.
1 5 min.
10 min.
20 min.
30 min.
2 5 min.
10 min.
20 min.
30 min.
3 5 min.
10 min.
20 min.
30 min.
4 5 min.
10 min.
20 min.
30 min.
5 5 min.
10 min.
20 min.
30 min.
1 5 min.
10 min.
20 min.
30 min.
2 5 min.
10 min.
20 min.
30 min.
3 5 min.
10 min.
20 min.
30 min.
22+
NC
NC
NC
22+
NC
NC
NC
22 +
NC
NC
NC
22+
NC
NC
NC
22 +
NC
NC
NC
22 +
NC
NC
NC
22+
NC
NC
NC
22+ (solids)
NC
NC
NC
22+ (solids)
NC
NC
NC
2.0
3.4
1.0
1.8
1.5
0.9
0.0
0.0
0.0
-------
MOVEMENT AND COLLECTION OF "FREE LIQUID" FOR AIR POLLUTION
CONTROL EQUIPMENT SLUDGE ON THE INCLINED PLANE
(continued)
Replication
Time
35'
4
5
5
10
20
30
5
10
20
30
min.
min.
min.
min.
min.
min.
min.
min.
12.5
22 +
NC
NC
22+
NC
NC
NC
Movement (cm) Free Liquid(g)
0.0
0.0
NC No Change
-------
"FREE LIQUID" CONTENT OF PAINT SLUDGE AS
DETERMINED BY THE INCLINED PLANE
Angle Replication Time (min) Free Liquid (g)
5° 1 5 6.1
10 7.5
15 8.76
20 8.85
25 8.85
30 8.85
5° 2 5 5.5
10 8.0
15 8.8
20 9.4
25 9.5
30 9.5
5° 3 5 2.6
10 5.0
15 5.5
20 6.4
25 6.6
30 6.7
5° 4 5 8.60
10 8.67
15 10.02
20 10.57
25 10.57
30 10.57
5° 5 5 8.65
10 9.05
15 9.55
20 9.81
25 10.35
30 10.35
15° 1 5 26.50
10 29.35
15 30.00
20 30.32
25 30.38
30 30.38
-------
n
FREE LIQUID" CONTENT OF PAINT SLUDGE AS
DETERMINED BY THE INCLINED PLANE
(Continued)
Angle Replication Time (min) Free Liquid (g)
15° 2 5 20.75
10 26.58
15 28.35
20 29.32
25 29.85
30 30.15
15° 3 5 34.27
10 35.12
15 40.87
20 41.32
25 41.67
30 41.72
15° 4 5 21.02
10 24.37
15 24.77
20 24.77
25 24.77
30 24.87
15° 5 5 19.35
10 25.35
15 26.75
20 28.05
25 28.60
30 28.95
25° 1 5 19.97
10 21.87
15 22.97
20 23.37
25 23.57
30 23.87
25° 2 5 13.22
10 19.77
15 21.77
20 23.77
25 25.07
30 26.07
-------
"FREE LIQUID" CONTENT OF PAINT SLUDGE AS
DETERMINED BY THE INCLINED PLANE
(Continued)
Angle Replication Time (min) Free Liquid (g)
25° 3 5 17.49
10 17.82
15 20.72
20 21.72
25 22.67
30 22.97
25° 4 5 24.1
10 29.8
15 32.7
20 34.2
25 34.7
30 35.2
25° 5 5 19.47
10 23.77
15 27.87
20 28.57
25 29.52
30 29.97
NC No Change
-------
MOVEMENT OF "FREE LIQUID" AND SOLIDS
FOR SEPARATOR SLUDGE ON THE INCLINED PLANE
Angle Replication Time (rnin) Movement (cm)
5° 15 0.75 (solids)
10 NC
15 NC
20 NC
25 NC
30 NC
5* 25 1.5 (solids)
10 NC
15 NC
20 NC
25 NC
30 NC
5° 35 0.5 (solids)
10 NC
15 NC
20 NC
25 NC
30 NC
5° 45 1.0 (solids)
10 NC
15 NC
20 NC
25 NC
30 NC
5° 55 0.5 (solids)
10 NC
15 NC
20 NC
25 NC
30 NC
15° 1 5 2.0 (solids)
10 2.5 (solids)
15 NC
20 2.75
25 NC
30 NC
-------
MOVEMENT OF "FREE LIQUID" AND SOLIDS
FOR SEPARATOR SLUDGE ON THE INCLINED PLANE
(Continued)
Replication
2
15'
15'
15'
25'
25'
Time (min)
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
Movement (cm)
2.0 (solids)
NC
NC
NC
NC
NC
(solids)
1.5
NC
NC
NC
NC
NC
2.0 (solids)
3.0 (solids)
NC
NC
NC
3.5
1.0 (solids)
1.5 (solids)
NC
NC
2.0
NC
(solids)
5.5
NC
9.0
22+
NC
NC
6.5 (solids)
NC
9.0
15.5
22 +
NC
-------
MOVEMENT OF "FREE LIQUID" AND SOLIDS
FOR SEPARATOR SLUDGE ON THE INCLINED PLANE
(Continued)
Angle
25°
Replication
3
25'
25'
35'
35'
35*
Time (min)
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
Movement (cm)
5.0 (solids)
NC
NC
NC
NC
5.5
4.0
NC
NC
NC
4.5
11.5
5.0
NC
NC
NC
NC
20.0
9.5
10.0
22 +
NC
NC
NC
12.0
18.0
NC
22+
NC
NC
9.5
NC
16.0
22+
NC
NC
(solids)
(solids)
(1 drop)
(solids)
(solids)
(solids)
-------
MOVEMENT OF "FREE LIQUID" AND SOLIDS
FOR SEPARATOR SLUDGE ON THE INCLINED PLANE
(Continued)
Angle
35°
Replication
4
35'
45'
45'
45'
45'
Time (min)
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
5
10
15
20
25
30
Movement (cm)
(solids)
8.0
NC
9.5
20.0
22+
NC
7.5 (solids)
NC
NC
8.0
18.0
22 +
(solids)
14.5
15.0
22 +
NC
NC
NC
14.0 (solids)
NC
19.5
22+
NC
22+ (solids)
22+ (solids)
NC
NC
NC
NC
NC
14.0 (solids)
NC
20.0
22+
NC
18.5 (solids)
-------
MOVEMENT OF "FREE LIQUID" AND SOLIDS
FOR SEPARATOR SLUDGE ON THE INCLINED PLANE
(Continued)
Angle Replication Time (min) Movement (cm)
45° 5 5 22+ (solids)
10 NC
15 NC
20 NC
25 NC
30 NC
NC No Change
-------
APPENDIX B
TEST PROTOCOL AND RESULTS FOR THE DETERMINATION
OF "FREE LIQUID" BY THE LAB PRESS
-------
THE DETERMINATION OF "FREE LIQUID"
BY THE LAB PRESS
Test Procedure
Summary and Method
A sample is placed in the test cylinder of the lab
press. Force is applied by a hydraulic piston which simulates
landfill pressures. The amount of liquid that is extracted
at the specified pressure is quantified.
Apparatus
1. Carver Laboratory Press, Model C 12-ton capacity:
Lab press capable of exerting enough pressure to simulate
the pressure present in landfills at depths of 20 to 100 feet.
2. Filter Plate Assembly: Includes a filter holding
ring and test cylinder capable of separating liquids from
solids when pressure is applied.,
3. Collection pan: used to collect the liquid extracted
during the test. It should be constructed of nonreactive
material.
General Procedure
1. Assemble the filter plate assembly with a 16-mesh
screen.
2. Assemble the test cylinder. Place the test cylinder
over the holding ring/ screen side up, until the bottom of
holding ring is flush with the bottom of the test cylinder.
-------
3. Weigh out a designated amount of test material
(enough to fill the cylinder to the recommended 3/4 in. from
the top) and place in the test cylinder. Smooth the surface
of the testing material.
4. Place a filter screen on the surface of the test
material. Cover this screen with a filter pad and place the
plunger on top of the filter pad.
5. Place the test cylinder and plunger in the collec-
tion pan on the platen of the press.
6. Apply the desired pressure to the sample for a
5-minute test duration.
7. Remove the test cylinder from the lab press.
Remove any "free liquid" that has collected in the collection
pan or on the test cylinder and discard.
8. Using the ejector provided with the lab press,
eject the solid material from the test cylinder and weigh.
9. Calculate the percent "free liquid" in the original
test sample:
a. weight of weight of weight of "free liquid"
original - sample after = removed from
test pressed sample
material
b. weight of "free liquid" x 100 « % "free liquid" of
weight of original test sample
test sample
-------
"FREE LIQUID" CONTENT (PERCENT) OF
DRILLING MUD AS DETERMINED BY THE LAB PRESS
AT VARIOUS PRESSURES*
43.33 psi
61.00
52.15
68.90
51.70
57.85
Ave rage
58.32
34.67 psi
49.01
39.10
39.94
51.93
21.13
40.22
26.00 psi
22.48
33.72
15.96
27.65
25.25
25.01
17.33 psi
20.23
41.21
14.01
16.94
25.81
18.06
8.67 psi
8.69
12.74
12.36
7.87
13.86
11.10
* All tests were conducted with a 16 mesh screen for a test
duration of 5 minutes.
-------
"FREE LIQUID" CONTENT (PERCENT) OF PAINT SLUDGE
AS DETERMINED BY THE LAB PRESS
AT VARIOUS PRESSURES (psi)*
Replication
1
2
3
4
5
43.33
21.18
21.19
19.71
21.17
21.01
34.67
19.79
22.14
20.43
19.19
18.05
26.00
15.21
13.39
17.25
15.68
13.57
17.33
11.07
14.25
11.02
11.91
12.54
8,67
10.25
9.14
7.91
9.61
7.79
Average 20.85 19.95 15.02 12.16 8.94
* All tests were conducted with a 16 mesh screen for a test
duration of 5 minutes.
-------
"FREE LIQUID" CONTENT (PERCENT) OF AIR POLLUTION CONTROL
EQUIPMENT SLUDGE AS DETERMINED BY
THE LAB PRESS AT VARIOUS PRESSURES (psi)*
Replication
1
2
3
4
5
43.33
4.05
2.6
4.27
1.01
3.63
34.67
2.87
2.67
0.77
3.17
3.17
26.00
1.82
0.88
1.82
0.97
2.57
17.33
0.0
0.0
0.0
0.0
0.0
8.67
0.0
0.0
0.0
0.0
0.0
Average 3.11 2.53 1.61 0.0 0.0
* All tests were conducted with a 16 mesh screen for a test
duration of 5 minutes.
-------
"FREE LIQUID" CONTENT (PERCENT) OF SEPARATOR
SLUDGE AS DETERMINED BY THE LAB PRESS
AT VARIOUS PRESSURES (psi)*
Replication
1
2
3
4
5
43.33
9.36
7.5
11.9
9.07
8.5
34.67
8.6
8.6
7.1
7.9
7.8
26.00
8.1
6.2
7.5
7.7
6.2
17.33
7.3
5.8
6.5
6.5
8.0
8.67
3.98
4.94
3.66
4.01
4.86
Average 9.26 8.0 7.14 6.82 4.29
* All tests were conducted with a 16 mesh screen for a test
duration of 5 minutes.
-------
APPENDIX C
TEST PROTOCOL AND RESULTS FOR THE DETERMINATION
OF "FREE LIQUID" BY THE FILTRATION UNIT
-------
THE DETERMINATION OF "FREE LIQUID"
BY THE FILTRATION UNIT
Test Procedure
Summary and Method
A sample is placed in the test cylinder of the filtration
unit. Positive pressure, which simulates landfill pressures,
is applied by compressed nitrogen. The amount of "free
liquid" that is extracted is collected is quantified.
Apparatus
1. Millipore Hazardous Waste Filtration System:
Filtration unit commonly used in EP toxicity testing.
2. Compressed Nitrogen: Capable of exerting enough
pressure to simulate the pressure applied at landfills at
depths from 20 to 100 feet.
3. Filters: 0.45 micron membrane filter and a prefilter.
4. Distilled water: Used for wetting the filters
prior to testing.
General Procedure
1. Wet membrane with distilled water and place on the
base screen of the filtration unit.
2. Center the test cylinder onto the membrane.
3. Wet the prefilter and lower it through the top of
the test cylinder onto the membrane filter.
4. Weigh out a representative sample of material to
be tested (minimum size lOOg).
-------
5. Place test sample in test cylinder, making sure to
completely cover the bottom of the test cylinder.
6. Place the top plate of the filtration unit on the
test cylinder and tighten the hand wheel bolts.
7. Attach pressure tubing to the nitrogen tank and
hose adapter on top of the top plate.
8. Apply specified pressure to sample from the compressed
nitrogen tank.
9. Collect and weigh all the "free liquid" that is
extracted.
10. Subtract 8.67 g from the weight of the "free
liquid" extracted, which is the average amount of liquid
extracted from the filter and membrane.
11. Calcuate the "free liquid" in the original test
sample:
weight of "free liquid" x 100 = % "free liquid" of
weight of original test sample
test sample
-------
"FREE LIQUID" CONTENT (PERCENT) OF DRILLING MUD
AS DETERMINED BY THE FILTRATION UNIT
AT VARIOUS PRESSURES (psi)*
Replication
1
2
3
4
5
43.33
5.59
2.44
1.99
4.12
5.94
34.67
2.60
7.15
1.1
2.00
0.35
26.00
5.85
6.90
4.15
5.65
3.05
17.33
3.80
2.90
7.15
3.05
5.65
8.67
0.0
2.45
0.0
0.0
0.9
Average 4.02 2.58 5.12 4.51 0.67
* All tests conducted with an 0.65 urn membrane filter for
a test duration of 30 minutes.
-------
"FREE LIQUID" CONTENT (PERCENT) OF AIR POLLUTION
CONTROL EQUIPMENT SLUDGE AS DETERMINED BY THE
FILTRATION UNIT AT VARIOUS PRESSURES (psi)*
Replication
1
2
3
4
5
17.33
8.91
9.8
11.54
10.18
9.65
8.67
9.53
9.34
10.03
10.05
10.25
Average 10.02 9.84
* All tests were conducted with an 0.65 urn membrane filter
for a test duration of 30 minutes.
-------
"FREE LIQUID" CONTENT (PERCENT) OF PAINT SLUDGE AS
DETERMINED BY THE FILTRATION UNIT
AT VARIOUS PRESSURES (psi)*
Replication
1
2
3
4
5
Average 21.39 22.38
* All tests were conducted with an 0.65 urn membrane filter
for a test duration of 30 minutes.
17.33
23.47
20.17
2.1.60
20.54
21.16
8.67
23.12
20.73
19.69
23.30
25.10
-------
"FREE LIQUID" CONTENT (PERCENT) OF SEPARATOR SLUDGE
AS DETERMINED BY THE FILTRATION UNIT
AT VARIOUS PRESSURES (psi)*
Replication
1
2
3
4
5
43,33
22.87
23.31
21.28
21.41
22.53
34.67
21.6
23.9
20.3
22.7
20.71
26.00
20.07
20.55
19.39
19.46
20.36
17.33
17.07
20.7
18.1
19.91
17.91
8.67
12.1
12.6
12.23
11.1
12.07
Average 22.28 21.8 19.96 18.73 12.02
* All tests conducted with an 0.65 urn membrane filter for
a test duration of 20 minutes.
-------
APPENDIX D
TEST PTOTOCOL AND RESULTS FOR THE DETERMINATION OF
"FREE LIQUID" BY THE GRADUATED CYLINDER TEST
-------
THE DETERMINATION OF "FREE LIQUID"
BY THE GRADUATED CYLINDER TEST
Test Procedure
Summary of Method
100 ml of a representative sample of a waste is placed
in a 100-ml graduated cylinder. The cylinder is corked and
agitated until the waste is thoroughly mixed. Any liquid
which settles to the top of the cylinder is considered "free
liquid."
Apparatus
1. 100 ml graduated cylinder
2. Cork
General Procedure
1. Place 100 ml of a representative sample of a waste
in a 100-ml graduated cylinder.
2. Cork the graduated cylinder.
3. Agitate the waste until the sample is well mixed.
4. Allow the sample to set for 24 hours.
5. Record the amount of "free liquid" (ml) which has
settled to the top of the graduated cylinder.
-------
'FREE LIQUID" AS DETERMINED BY THE GRADUATED CYLINDER
Air Pollution
Time
5 rain.
10 rain.
15 min.
20 min.
25 min.
30 min.
35 min.
40 min.
45 min.
50 min.
1 Hour
1 Hr/15
1 Hr/30
1 Hr/45
2 Hours
Replication
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
min. 1
2
min. 1
2
min. 1
2
1
2
Paint
Sludge
0 ml
0
0
2.5
0
2.5
0
2.5
0
2.5
0
2.5
0
3
0
3
0
3
0
3
0
3
0
3
0
3
0
3
0
4
Control Equipment
Sludge
0 ml
0
0
0
0
1
0
2
1
2
2
2
2
2
2
2
2
2
2
2.5
2.5
3
3
3
3
3
3
3.5
4
4
Separator
Sludge
0 ml
0
0
0
0
0
0
0
0
0
1
0
2
1
3
2
3
2
3
2
3
2
3
2
3
2
3
2
3
2
Paper
Sludge
0 ml
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
-------
'FREE LIQUID" AS DETERMINED BY THE GRADUATED CYLINDER
(Page2)
Air Pollution
Time Re]
2 Hr/30 min.
3 Hours
4 Hours
5 Hours
24 Hours
.cation
1
2
1
2
1
2
1
2
1
2
Paint
Sludge
0 ml
4
0
4
0
4
0
4
0*
4
Control Equipment
Sludge
4 ml
4
4
4
4.5
4
4.5
5
4.5
5
Separator
Sludge
3 ml
2
3
2
3
2
3
2
4
3
Paper
Sludge
0 ml
0
_._
->
_-._
««. *_
__
* The paint sludge did not settle during the test, but when stamped
down after the test was completed, 5 ml of liquid settled out.
-------
TABLE 2
'FREE LIQUID" AS DETERMINED BY THE PAINT FILTER
Modification No. One
Air Pollution
Control
Time
15 min.
30 min.
Change
"free
liquid
45 min.
Change
"free
liquid
1 Hour
Change
"free
liquid
1 hr/
30 min
Change
"free
liquid
1 hr/
45 min
Replication
1
2
1
2
in
1
2
1
2
in
1
2
1
2
in
1
" 2
1
2
in
1
2
1
2
Equipment
Sludge
trace
0.0
trace
0.0
0
0
.-
Paint
Sludge
4.0
4.0
5.5
5.5
1.5
1.5
6.0
6.0
0.5
0.5
Separator
Sludge
1.0*
2.0*
4.0
3.5*
3.0
1.5
5.5
5.0
1.5
1.5
6.5
5.5
1.0
0.5
...
Paper
Sludge
3.0
3.0
4.0
5.0
1.0
2.0
5.0
6.0
1.0
1.0
6.0
7.0
1.0
1.0
8.0
9.0
1.0
1.0
8.5
9.5
-------
TABLE 2
"FREE LIQUID" AS DETERMINED BY THE PAINT FILTER
Modification No. One
(Page 2)
Time
Replication
Change in
"free 1
liquid" 2
Air Pollution
Control
Equipment Paint
Sludge Sludge
Separator
Sludge
Paper
Sludge
0.5
0.5
Total
"free
liquid"
1
2
trace
0.0
6.0
6.0
6.5
5.5
8.5
9.5
* Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
TABLE 3
"FREE LIQUID" AS DETERMINED BY THE PAINT FILTER
Modification No. Two
Air Pollution
C
Replication
1
2
* Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
Control Equipment
Sludge
0.0
0.0
Paint
S lud ge
3.0
3.0
Separator
Sludge
2.0*
1.0*
Paper
Sludge
1.0*
2.0*
-------
THE EFFECT OF "PERMASORB" ON THE
"FREE LIQUID" CONTENT OF SEPARATOR SLUDGE
Test
Number
5 min.
15 min.
5 min.
15 min.
30 min.
45 min.
1 hour
"Permasorb"(g)
1.0
Replication
0.7
0.6
"Free
Liquid"(ml)
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
1.0*
1.0*
3.0
3.0
3.0
3.0
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
APPENDIX E
TEST PTOTOCOL AND RESULTS FOR THE DETERMINATION
OF "FREE LIQUID" BY THE SIEVE TEST
-------
THE DETERMINATION OF "FREE LIQUID1
BY THE SIEVE SERIES
Test Procedure
Summary of Method
A representative sample of a waste is placed in a 10,
18, 35, and 60-mesh sieve series. The sieves are agitated
and any liquid which penetrates the bottom 60-mesh sieve is
considered "free liquid."
Apparatus
1. 10, 18, 35, and 60-mesh screen sieves.
General Procedure
1. Place 200 ml of a representative sample of a waste
in a 10, 18, 35, and 60-mesh sieve series.
2. Agitate the sieves for a 5-minute test duration.
3. Measure the amount of liquid (ml) which penetrated
the bottom 60-mesh screen.
-------
TABLE 1
'FREE LIQUID" AS DETERMINED BY SIEVE TEST
"Free Liquid1
Waste Replication (mlj
paint Sludge** 1 2.0*
2 1.0*
Air Pollution
Control Equipment
Sludge 1 2.0*
2 0.0
3 0.0
4 ' 0.5*
Separator Sludge 1 3.5*
2 0.0
3 7.0
4 2.0*
5 3.0*
Paper Sludge 1 0
2 0
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
** Liquid did not pass through the 60-mesh screen and
Readings were made using only the 10, 18, and 35 mesh
screens.
-------
APPENDIX F
TEST PROCEDURE AND RESULTS FOR THE DETERMINATION
OF "FREE LIQUID" BY THE PAINT FILTER TESTS
-------
THE DETERMINATION OF "FREE LIQUID"
BY THE PAINT FILTER TEST
Test Procedure
Summary of Method
100 ml of a waste is placed in a paint filter in.a
funnel. A watch glass is placed on top of the waste. Any
liquid which is generated by the waste is considered "free
liquid" and is measured in a 100 ml graduated cylinder.
Apparatus
1. Paint filter
2. Funnel
3. Watch glass
4. 100 ml graduated cylinder
General Procedure
1. Collect 100 ml of a representative sample of
waste.
2. Place the waste in the paint filter/ in a funnel,
and cover with a watch glass.
3. Collect all "free liquid" generated in a 100 ml
graduated cylinder.
4. Record the amount of "free liquid" (ml) generated
after a test duration of 5 and 15 minutes.
5. If the change in "free liquid" is greater than
10 percent, record the amount of "free liquid" at
15-minute intervals until the change is less than
10 percent.
-------
TABLE 1
"FREE LIQUID" AS DETERMINED BY THE PAINT FILTER
Air Pollution
Time
5 min.
10 min.
15 min.
20 min.
25 min.
30 min.
35 min.
40 min.
45 min.
Paint Control Equipment
.cation Sludge Sludge
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
4 ml
3.5*
___
5
3.5*
5
3.5*
___
_
5
3.5*
5
3.5*
___
_
5
3.5*
___
5
3.5*
_--
5
3.5*
5
3.5*
1.
0
1
1
2
0
2
2
3
0
3
3
4
0
3
4
4
0
3
4
4
0
3
4
4
0
3
4
4
0
3
4
4
0
3
4
5 ml*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
Separator
Sludge
1 ml*
1 *
___
1 *
1 *
2 *
2 *
2 *
2 *
3 *
3 *
-
4
3 *
4.5
3.5*
___
4.5
3.5*
___
4
5
_
Paper
Sludge
0
0
0
0
0
0
0
0
___
0
trace
trace
trace
___
trace
trace
trace
trace
_.__
2 *
3 *
___
-------
TABLE 1
'FREE LIQUID" AS DETERMINED BY THE PAINT FILTER
(Page 2)
Air Pollution
Time
50 min.
55 min.
1 Hour
1 Hr/15 min. 1
1 Hr/30 min. 1
1 Hr/45 min. 1
2 Hours
2 Hr/30 min. 1
3 Hours
Paint Control Equipment Separator
Lcation
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
Sludge
5
3.5*
___
5
3.5*
5
3.5*
5
3.5*
_
___
5
3.5*
__-
_
5
3.5*
-~
5
3.5*
___
_
5
3.5*
5
3.5*
Sludge
4 *
0
3 *
4 *
4 *
0
3 *
4 *
4 *
0
3 *
4 *
4 *
0
3 *
4 *
4 *
0
3 *
4 *
4 *
0
3 *
4 *
4 *
0
3 *
4 *
4 *
0
3 *
4 *
4 *
0
3 *
4 *
Sludge
5
5
___
5.5
5
5.5
5
___
__-
6
5.5
__
6.5
6
___.
7
6.5
__-
7.5
7
___
8
7.5
___
8.5
8
___
___
Paper
Sludge
2 *
3 *
_ _
_
2 *
3 *
_
2 *
3 *
---
3 *
3 *
_ _
3 *
3 *
_-_
_
3 *
3 *
_-_
_
3 *
3 *
_
3 *
3 *
_-_
3 *
4
___
-------
TABLE 1
'FREE LIQUID" AS DETERMINED BY THE PAINT FILTER
(Page t)
3
Time Replication
4 Hours 1
2
3
4
5 Hours 1
2
3
4
6 Hours 1
2
3
4
Air Pollution
Paint Control Equipment Separator
Sludge Sludge Sludge
5
3.5*
___
5
3.5*
___
5
3.5*
__
_
4 *
trace
3 *
4 *
4 *
trace
3 *
4 *
4 *
trace
3 *
4 *
9
9
10
9
___
10.5
9.5
Paper
Sludge
3.5*
4
-__
4
5.5
_
___
__.
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE DETERMINATION OF "FREE LIQUID"
BY THE PAINT FILTER TEST
Test Procedure
Summary of Method
100 ml of a waste is placed in a paint filter in a
funnel. A watch glass is placed on top of the waste. Any
liquid which is generated by the waste is considered "free
liquid" and is measured in a 100 ml graduated cylinder.
Apparatus
1. Paint filter
2. Funnel
3. Watch glass
4. 100 ml graduated cylinder
General Procedure
1. Collect 100 ml of a representative sample of
waste.
2. Place the waste in the paint filter in a funnel
and cover with a watch glass.
3. Collect the "free liquid" generated in a 100 ml
graduated cylinder.
4. Record the amount of "free liquid" generated in ml
every 5 minutes for the first hour, every 15 minutes
for the second hour, every half hour for the third
hour, and every hour for the next three hours.
-------
Modification No. 1;
General Procedure
1. Collect 100 ml of a representative sample of
waste.
2. Place the waste in the paint filter, in a funnel,
and cover with a watch glass.
3. Collect the "free liquid" generated in a 100 ml
graduated cylinder.
4. Record the amount of "free liquid" (ml) generated
after a test duration of 15 minutes.
5. Stir the test sample and allow it to drain for
15 minutes.
6. Record the amount of "free liquid" generated.
7. Calculate the change in "free liquid" that has
drained from the test sample after 15 minutes and after
one-half hour.
8. If the change in "free liquid" is greater than
10 percent, record the amount of "free liquid" at
15-minute intervals until the change is less than
10 percent.
Modification No. 2;
General Procedure
1. Collect 100 ml of a representative sample of
waste.
2. Place the waste in the paint filter in the funnel
and cover with a watch glass.
3. Note any "free liquid"1 which is generated.
-------
APPENDIX G
ABSORBENT MATERIALS
TEST RESULTS: "PERMASORB"
THE EFFECT OF "PERMASORB" ON THE
"FREE LIQUID" CONTENT OF SEPARATOR SLUDGE
Test
Number Time
1 5
15
2 5
15
3 5
15
30
45
1
min.
min.
min.
min.
min.
min.
min.
min.
hour
"Permasorb" (g) Replication
1.0 1
2
1
2
0.7 1
2
1
2
0.6 1
2
1
2
1
2
1
2
1
2
"Free
Liquid" (ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
1.0*
1.0*
3.0
3.0
3.0
3.0
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF "PERMASORB" ON THE
"FREE LIQUID" CONTENT OF PAPER SLUDGE
Test
Number
5 min.
15 min.
5 min.
15 min.
30 min.
45 min.
1 hour
"Permasorb"(g)
1.0
Replication
0.6
0.5
"Free
Liquid"(ml)
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
1.0*
trace
2.0*
1.0*
3.0*
2.0*
4.0*
2.0*
4.0
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF "PERMASORB" ON THE
"FREE LIQUID" CONTENT OF PAINT SLUDGE
"Free
Replication Liquid"(ml)
1 0.0
2 0.0
1 0.0
2 0.0
1 0.0
2 0.0
1 0.0
2 0.0
1 0.0
2 0.0
1 1.0
2 0.0
1 1.0*
2 1.0*
1 2.0*
2 1.0*
1 2.0*
2 1.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
Test
Number
1
2
3
4
Time
5
15
5
15
5
15
5
15
min.
min.
min.
min.
min.
min.
min.
min.
Permasorb" (g)
0.5
0.3
0.2
0.1
-------
THE EFFECT OF "PERMASORB" ON THE
"FREE LIQUID" CONTENT OF AIR POLLUTION
CONTROL EQUIPMENT SLUDGE
Test
Number Time "Permasorb" (g)
1 5 min. 1. 0
15 min.
2 5 min. 0.9
15 min.
3 5 min. 0.8
15 min.
4 5 min. 0.7
15 min.
Replication
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
4. 4. ^.*_»
Liquid" (ml)
0.0
0. 0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
trace
trace
-------
APPENDIX H
ABSORBENT MATERIALS
TEST RESULTS: TRIPAK SOLIDIFCATION MEDIUM
-------
THE EFFECT OF TRIPAK SOLIDIFICATION MEDIUM
ON THE "FREE LIQUID" CONTENT OF PAPER SLUDGE
TriPak
Test
Number
1
2
Time
5 min.
15 min.
5 min.
15 min.
Solidification
Medium (g)
8
7
Replication
1
2
1
2
1
2
1
2
"Free
Liquid" (ml)
0.0
0.0
0.0
0.0
trace
0.0
trace
0.0
-------
THE EFFECT OF TRIPAK SOLIDIFICATION MEDIUM
ON THE "FREE LIQUID" CONTENT OF PAINT SLUDGE
TriPak
Test
Number
1
2
Time
5 min.
15 min.
5 min.
15 min.
30 min.
Solidification
Medium (g)
4
3
Replication
1
2
1
2
1
2
1
2
1
2
"Free
Liquid" (ml)
0.0
0.0
0.0
0.0
0.0
trace
trace
1.0*
trace
1.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF TRIPAK SOLIDIFICATION MEDIUM
ON THE "FREE LIQUID" CONTENT OF AIR
POLLUTION CONTROL EQUIPMENT SLUDGE
Test
Number
5 min.
15 min.
30 min.
TriPak
Solidification
Medium (g)
17
16
Replication
1
2
1
2
1
2
1
2
1
2
"Free
Liquid "(ml)
0.0
0.0
0.0
0.0
0.0
0.0
trace
1.0*
trace
1.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF TRIPAK SOLIDIFICATION MEDIUM
ON THE "FREE LIQUID" CONTENT OF SEPARATOR SLUDGE
Test
Number
1
2
TriPak
Solidification
Time Medium (g)
5
15
5
15
30
min.
min.
min.
min.
min.
7
6
Replication
1
2
1
2
1
2
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
1 drop
trace
1.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
APPENDIX I
ABSORBENT MATERIALS
TEST RESULTS: DRILLING MUD
-------
THE EFFECT OF DRILLING MUD ON THE
"FREE LIQUID" CONTENT OF PAINT SLUDGE
Test
Number
Time
5 min.
15 min.
5 min.
15 min.
5 min.
15 min.
5 min.
15 min.
5 min.
15 min.
Drilling
Mud (g)
10
Replication
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
2.0*
2.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF DRILLING MUD ON THE
"FREE LIQUID" CONTENT OF PAPER SLUDGE
Test
Number
5 min.
15 min.
5 min.
15 min.
30 min.
45 min.
Drilling
Mud (g)
10
Replication
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
1.0*
2.0*
1.0*
2.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF DRILLING MUD ON THE
'FREE LIQUID" CONTENT OF SEPARATOR SLUDGE
Test
Number
1
2
3
4
5
Time
5
15
5
15
5
15
5
15
5
15
min.
min.
min.
min.
min.
min.
min.
min.
min.
min.
Drilling
Mud (g )
10
5
3
2
1
Replication
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
r.c
o. o
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF DRILLING MUD ON THE
"FREE LIQUID" CONTENT OF AIR POLLUTION
CONTROL EQUIPMENT SLUDGE
Test Drilling "Free
Number Time Mud (g) Replication Liquid"(ml)
1 5 min. 2 1 0.0
2 0.0
15 min. 1 0.0
2 0.0
2 5 min. 1 1 trace
2 0.0
3 0.0
15 min. 1 trace
2 trace
3 0.0
-------
APPENDIX J
ABSORBENT MATERIALS
TEST RESULTS: "SAFE-N-DRI"
-------
THE EFFECT OF "SAFE-N-DRI" ON THE
"FREE LIQUID" CONTENT OF SEPARATOR SLUDGE
Test
Number Time "Safe-N-Dri" (g)
1 5 min. 7
15 min.
2 5 min. 6
15 min.
3 5 min. 5
15 min.
30 min.
45 min.
1 hour
Replication
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
"Free
Liquid" (ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
1.0*
1.0*
2.0*
1.0*
2.0*
1.0
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF "SAFE-N-DRI" ON THE
"FREE LIQUID" CONTENT OF PAINT SLUDGE
Test
Number
Time "Safe-N-Dri"(g)
5 min. 5
15 min.
5 min. 3
15 min.
30 min.
5 min. 2
15 min.
5 min. 1
15 min.
Replication
1
2
1
2
1
2
3
1
2
3
1
1
2
1
2
1
2
3
1
2
3
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
0.0
0.0
trace
0.0
0.0
0.0
0.0
trace
0.0
0.0
trace
0.0
0.0
-------
THE EFFECT OF "SAFE-N-DRI" ON THE
"FREE LIQUID" CONTENT OF AIR POLLUTION
CONTROL EQUIPMENT SLUDGE
Test
Number
Time "Safe-N-Dri"(g)
5 min. 15
15 min.
5 min.
15 min.
5 min.
15 min.
30 min.
13
12
Replication
1
2
1
2
1
2
1
2
1
2
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0. 0
0.0
0.0
0.0
0.0
trace
0.0
trace
trace
2.0*
2.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF "SAFE-N-DRI" ON THE
"FREE LIQUID" CONTENT OF PAPER SLUDGE
Test
Number
Time "Safe-N-Dri"(g)
5 min. 15
15 min.
5 min.
15 min.
5 min.
15 min.
30 min.
45 min.
1 hour
14
13
Replication
1
2
1
2
1
2
1
2
1
2
3
1
2
3
1
2
3
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
trace
1.0
trace
1.0*
2.0*
1.0*
2.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
APPENDIX K
ABSORBENT MATERIALS
TEST RESULTS: VERMICULITE
-------
THE EFFECT OF VERMICULITE ON THE
"FREE LIQUID" CONTENT OF PAINT SLUDGE
Test
Number
Time
5 min.
15 min.
5 min.
15 min.
5 min.
15 min.
Vermiculite(g) Replication
0.6
0.5
'Free
Liquid"(ml)
1
2
1
2
1
2
1
2
1
2
1
2
0.0
0.0
0.0
0.0
o.c
0.0
0.0
0.0
trace
trace
trace
1.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF VERMICULITE ON THE
"FREE LIQUID" CONTENT OF PAPER SLUDGE
Test
Number
1
2
Time
5 min.
15 min.
5 min.
15 min.
30 min.
45 min.
Vermiculite(g) Replication
3 1
2
1
2
2 1
2
1
2
1
2
1
2
"Free
Liquid" (ml)
0.0
0.0
0.0
0.0
0.0
0.0
trace
0.0
1.0*
trace
1.0*
trace
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF VERMICULITE ON THE
"FREE LIQUID" CONTENT OF SEPARATOR SLUDGE
Test
Number
Time Vermiculite(g) Replication
5 min. 5 1
2
15 min. 1
2
5 min. 3 1
2
15 min. 1
2
5 min. 2 1
2
15 min. 1
2
30 min. 1
2
45 min. 1
2
1 hour 1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
2.0*
2.0*
3.0
3.0
3.0
3.0
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF VERMICULITE ON THE
"FREE LIQUID" CONTENT OF AIR POLLUTION
CONTROL EQUIPMENT SLUDGE
Test
Number
1
2
3
Time
5 min.
15 min.
5 min.
15 min.
5 min.
15 min.
Vermiculite (g) Replication
5 1
2
1
2
4 1
2
1
2
3 1
2
1
2
"Free
Liquid "(ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
trace
trace
-------
APPENDIX L
ABSORBENT MATERIALS
TEST RESULTS: CEMENT KILN DUST
-------
THE EFFECT OF CEMENT KILN DUST ON THE
"FREE LIQUID" CONTENT OF PAINT SLUDGE
"Free
Replication Liquid"(ml)
1 0.0
2 0.0
1 0.0
2 0.0
1 0.0
2 0.0
1 0.0
2 0.0
1 0.0
2 0.0
1 1.0*
2 1.0*
1 1.0*
2 1.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
Test
Number
1
2
3
Cement
Time Kiln Dust(g)
5
15
5
15
5
15
30
min.
min.
min.
min.
min.
min.
min.
20
15
14
-------
THE EFFECT OF CEMENT KILN DUST ON THE
"FREE LIQUID" CONTENT OF PAPER SLUDGE
Test
Number
1
Time
5 min.
15 min.
Cement
Kiln Dust(g)
25
5 min.
15 min.
30 min.
24
Replication
1
2
1
2
1
2
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
trace
trace
-------
THE EFFECT OF CEMENT KILN DUST ON THE
"FREE LIQUID" CONTENT OF AIR POLLUTION
CONTROL EQUIPMENT SLUDGE
Test
Number
5 min.
15 min.
5 min.
15 min.
5 min.
15 min.
Cement
Kiln Dust(g)
30
27
26
25
Replication
1
2
1
2
1
2
1
2
1
2
3
1
2
3
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
0.0
0.0
trace
trace
trace
trace
-------
THE EFFECT OF CEMENT KILN DUST ON THE
"FREE LIQUID" CONTENT OF SEPARATOR SLUDGE
Test
Number
1
2
3
4
Cement
Time Kiln Dust(g)
5
15
5
15
5
15
30
45
1
5
15
30
min.
min.
min.
min.
min.
min.
min.
min.
hour
min.
min.
min.
5
4
3
2
Replication
1
2
1
2
1
2
1
2
1
2
3
1
2
3
2
2
2
1
2
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
0,0
1.0*
2.0*
2.0*
0.0
0.0
1.0*
1.0*
1.0*
1.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
APPENDIX M
ABSORBENT MATERIALS
TEST RESULTS: "HAZORB"
-------
THE EFFECT OF "HAZORB" ON THE
"FREE LIQUID" CONTENT OF PAINT SLUDGE
Test
Number
5 min.
15 min.
5 min.
15 min.
Time "Hazorb"(g)
5 min. 1
15 min.
0.8
0.7
Replication
1
2
1
2
1
2
1
2
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
trace
trace
-------
THE EFFECT OF "HAZORB" ON THE
"FREE LIQUID" CONTENT OF PAPER SLUDGE
Test
Number
5 min.
15 min.
30 min
45 min.
1 hour
"Hazorb" (g)
2
Replication
1
2
1
2
1
2
1
2
1
2
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
2.0*
2.0*
3.0
3.0
3.0
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
THE EFFECT OF "HAZORB" ON THE
"FREE LIQUID" CONTENT OF AIR POLLUTION
CONTROL EQUIPMENT SLUDGE
Test
Number
Time "Hazorb"(g)
5 min. 4
15 min.
5 min. 3
15 min.
30 min
45 min.
5 min. 2
15 min.
Replication
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
"Free
Liquid"(ml)
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
trace
3.0
trace
3.0
1.0*
2.0*
1.0*
2.0*
Reading is less than the minimum marking on the graduated
cylinder and is an approximation.
-------
APPENDIX N
ABSORBENT MATERIALS
TEST RESULTS: FLY ASH
-------
THE EFFECT OF "HAZORB" ON THE
"FREE LIQUID" CONTENT OF SEPARATOR SLUDGE
Test
Number
Time "Hazorb"(g)
5 min. 2
15 min.
5 min. 1
15 min.
30 min.
Replication
1
2
1
2
1
2
1
2
1
2
"Free
Liquid" (ml)
0.0
0.0
0.0
0.0
0.0
o.c
trace
trace
trace
trace
-------
THE EFFECT OF FLY ASH ON THE
"FREE LIQUID" CONTENT OF PAINT SLUDGE
Test
Number
1
2
3
Time Fly Ash(g)
5 min. 40
15 min.
5 min. 36
15 min.
5 min. 35
15 min.
30 min.
Replication
1
2
1
2
1
2
1
2
1
2
1
2
1
2
"Free
Liquid" (ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
trace
trace
trace
-------
THE EFFECT OF FLY ASH ON THE
"FREE LIQUID" CONTENT OF PAPER SLUDGE
Test
Number Time Fly Ash(g)
1 5 min. 51
15 min.
2 5 min. 50
15 min.
30 min.
3 5 min. 49
15 min.
30 min.
Replication
1
2
1
2
1
2
3
1
2
3
1
2
3
1
2
1
2
1
2
rree
Liquid" (ml)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
trace
0.0
0.0
trace
0.0
0.0
0,0
0.0
trace
trace
trace
trace
Protection Agency
'- -> Saut-i DvM..b:;,'n Street
Chicago, Illinois 606Q4
-------
APPENDIX G
ABSORBENT MATERIALS
TEST RESULTS: "PERMASORB"
------- |