EPA/530-SW-91-079
91U/4816/012 - 01 September 18, 1991
BACKGROUND DOCUMENT FOR
THE LIQUID RELEASE TEST:
SINGLE LABORATORY EVALUATION AND
1988 COLLABORATIVE STUDY
Prepared by:
Research Triangle Institute
P.O. Box 12194
Research Triangle Park, NC 27709
Prepared for:
U.S. Environmental Protection Agency
EPA Contract Nos. 68-01-7075, Work Assignment 76, and 68-WO-0032,
Work Assignment 12
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TABLE OF CONTENTS
Section Page
ACKNOWLEDGMENTS v
1.0 INTRODUCTION 1
2.0 BACKGROUND 2
2.1 THE TEST DEVICE 3
2.2 SUMMARY OF METHOD 3
2.3 SORBENTS AND SORBATES 5
2.4 RELATED TESTS 5
2.4.1 The Pressurized Concentration Level 5
2.4.2 The Saturated Concentration Level 6
3.0 SINGLE-LABORATORY VALIDATION 7
3.1 SORBENTS AND SORBATES TESTED 7
3.1.1 Sorbent Processing and Splitting 7
3.1.2 Sorbent Moisture Content 10
3.2 EQUIPMENT CALIBRATION 12
3.3 FREE DRAIN AND SATURATED CONCENTRATION
DETERMINATIONS 12
3.4 LRT RESULTS AT DIFFERENT LIQUID LOADING LEVELS 13
3.5 RESULTS OF PAINT FILTER LIQUIDS TEST 17
3.6 RESULTS WHEN SAMPLE HEIGHT IS ALTERED 21
3.7 RESULTS WHEN TEMPERATURE IS ALTERED 21
3.8 DISCUSSION OF IMBIBER BEADS® 24
4.0 THE COLLABORATIVE STUDY DESIGN 25
4.1 SORBENT/SORBATE COMBINATIONS 25
4.2 LIQUID LOADING LEVELS IN TEST SAMPLES 26
4.3 DEVICE CALIBRATION 26
4.4 OPPORTUNITY TO DEMONSTRATE EQUIVALENCY 26
4.5 SAMPLE PREPARATION 27
4.5.1 Floor Dry 29
4.5.2 Safe-Step 29
4.6 DISCUSSION OF COLLABORATIVE STUDY DESIGN 29
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TABLE OF CONTENTS
Section page
5.0 DISCUSSION OF THE COLLABORATIVE STUDY RESULTS 33
5.1 RESULTS USING THE ADM DEVICE 33
5.2 RESULTS USING OTHER DEVICES 35
6.0 QUALITY ASSURANCE 37
7.0 CONCLUSIONS/RECOMMENDATIONS 38
8.0 REFERENCES 39
APPENDICES
A LIQUID RELEASE TEST (LRT) 1988 DRAFT PROTOCOL
B SATURATED CONCENTRATION (SC) AND PRESSURIZED CONCENTRATION (PC)
PROCEDURES AND RESULTS
B.I Saturated Concentration Procedure
B.2 Pressurized Concentration Procedure
B.3 Experimental Data
C LIQUID RELEASE TEST DEVICE CALIBRATION
C. 1 Procedure Used to Calibrate LRT Devices
C.2 Calibration Results for ADM LRT Devices
D LIQUID RELEASE TEST (LRT) RESULTS
D. 1 Results for Floor Dry/Water
D.2 Results for Safe-Step/Motor Oil
D.3 Results for Vermiculite/0.01 N Calcium Sulfate Solution
D.4 Results for Oil Dry/5% Acetone Solution
D.5 Results for Oil Dry/Diesel Fuel
E PAINT FILTER LIQUIDS TEST PROCEDURE
E. 1 Method 9095 Paint Filter Liquids Test
E.2 Results for Floor Dry/Water
E.3 Results for Safe-Step/Motor Oil
F 1988 LIQUID RELEASE TEST (LRT) COLLABORATIVE STUDY RESULTS
F. 1 Results From Seven Laboratories Testing ADM Devices
F.2 Results From Three Laboratories Testing Other Devices
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LIST OF FIGURES
Figure Page
1 Liquid Release Test device 4
2 The splitting scheme used to obtain individual samples of sorbent
for LRT testing 11
3 LRT results: Floor Dry/water 15
4 LRT results: Safe-Step/oil 15
5 LRT results: SND-M/diesel 16
6 LRT results: SND-M/acetone in water (5% solution) 18
7 LRT results for Vermiculite/calcium suifate (0.01 N solution) 19
8 LRT and PFLT results: Floor Dry/water 20
9 LRT and PFLT results: Safe-Step/motor oil 20
10 LRT results for 5-cm and 10-cm samples of Floor Dry/water 22
11 LRT results for 5-cm and 10-cm samples of Safe-Step/motor oil 22
12 LRT Results: SND-M/diesel fuel at 4°. 23°, and 40°C 23
13 Confidence intervals for probability of getting a wrong result
as a function of number of failures 31
14 Experimental design parameters 32
in
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LIST OF TABLES
Table Page
1 Sorbent Properties 8
2 Properties of Test Liquids 9
3 Saturated Concentration (SC) and Pressurized Concentration (PC) Levels For
Sorbent/Sorbate Combinations 14
4 Liquid Loading in Collaborative Study Samples 28
5 Results from the 1988 Collaborative Study Using ADM Devices 34
6 Results from the 1988 LRT Collaborative Study Equivalency Tests 36
IV
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ACKNOWLEDGMENTS
This report was prepared by Ms. Carrie L. Kingsbury, P.E., and Ms. Constance V.
Wall of Research Triangle Institute (RTI) under EPA Contract No. 68-WO-0032, WA 12.
The LRT developmental work, the Draft Protocol, and the 1987 and 1988 collaborative
studies were performed by RTI under EPA Contract No. 68-01-7075, WA 76. Ms. Paula
Hoffman was the Work Assignment Leader. Ms. Kingsbury served as Program Manager
from November 1987 through November 1988. Mr. Joseph Evans served as Quality
Assurance Coordinator for the project during the 1988 developmental work and collaborative
study. The RTI project team also included Ms. Pam Overby, Ms. Donna Smith (Womack),
Ms. Dana Greenwood, and Mr. Keith Leese. Professional geologist Mr. Robert Truesdale,
also of RTI, assisted with the sorbent processing scheme and the early developmental work.
Dr. Roy Borden, P.E., of North Carolina State University's Department of Civil Engineering
performed the equipment calibrations. Mr. Franklin Smith and Mr. Michael Messner of RTI
assisted with the collaborative study data evaluation.
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1.0 INTRODUCTION
The Liquid Release Test (LRT) is a laboratory test method designed to determine
whether or not liquid will be released from sorbents when they are subjected to a vertical
load, as would be experienced by materials buried in a landfill. The LRT is an attribute test
rather than a continuous variable measurement test. Thus, the result is either a release
detected (sample fails the test) or no release detected (sample passes the test). This report
describes the single-laboratory evaluation and the collaborative study conducted in 1988 to
evaluate performance of the LRT Draft Protocol, and provides an assessment of the method
based on the results of these tests. This test method was developed by the Research Triangle
Institute (RTI) for the U.S. Environmental Protection Agency's (EPA's) Office of Solid Waste
(OSW).
EPA developed the LRT to implement Section 3004 (c)(2) of the Resource
Conservation and Recovery Act (RCRA), as amended in 1984, which requires EPA to issue
regulations that "prohibit the disposal in landfills of liquids that have been absorbed in
materials that biodegrade or that release liquids when compressed as might occur during
routine landfill operations." Development of a method to determine releasable liquid began in
1985.
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2.0 BACKGROUND
In December 1986, EPA proposed a liquid release test method using the zero head-
space extractor (ZHE) to implement RCRA 3004 (c)(2) (FR, December 24, 1986).
Subsequent evaluation of the proposed test revealed problems in repeatability for some types
of sorbents. These problems were attributed to the ZHE's design. After an unsuccessful
attempt to modify the ZHE to make it better suited for this application, EPA decided that a
different test device was needed.
There are several reasons for abandoning the ZHE as the test device for determining
releasable liquid. Problems associated with the device included small sample capacity, rough
movement of the piston, and difficulty in cleaning. The sample size specification given in the
proposed rule proved to be problematic in that the ZHE did not have sufficient capacity to
hold 100 grams of certain low density sorbents. In addition, subsequent research determined
that for certain sorbent/sorbate combinations, sample length or height had a significant effect
on test results.
The ZHE requires a significantly longer test time (30 minutes) to match results
obtained in 10-minute tests with other devices. A major concern was that the longer time
requirement would prove disruptive and costly to off-site commercial landfills processing
large numbers of containers.
The proposed approach to applying a compressed load to the sample was the use of a
piston driven by compressed gases (e.g., air or nitrogen). Modifications made to the ZHE to
shorten the test time and eliminate clean-up and operational problems (such as piston
movement) precluded direct use of gas pressure to drive the ZHE piston.
A new test device to determine releasable liquids was developed, and, in 1987, RTI
began work on a Draft Protocol to be used with it This Draft Protocol was evaluated in a
collaborative study involving seven laboratories in the fall of 1987. Results of the study
showed an unacceptable number of false positives (releases observed due to direct contact
between the filter and sample). For additional information, see the fall 1987 collaborative
study report (RTI, 1988a).
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During 1988, RTI continued the test development. Several improvements were
implemented, including modification of the release detection filters and addition of a spacer
grid to prevent sorbent contact with the filter. Additional testing was performed to determine
the effect of temperature, sample height, and test duration, and to compare the method with
the Paint Filter Liquids Test (PFLT; Method 9095).
The PFLT is used to determine whether or not free liquid is present in a waste. Unlike
the LRT, the PFLT determination is made under only the force of gravity.
RTT completed the single-laboratory evaluation of the revised LRT method in the fall
of 1988. A new collaborative study, again involving seven laboratories, was then conducted
to enable further evaluation of the method.
2.1 THE TEST DEVICE
The test requires a device capable of applying a vertical load of 50 psi continuously to
the top of a confined cylindrical sample. RTI used a test device developed by Associated
Design and Manufacturing (ADM) of Alexandria, VA, in developing and evaluating the LRT
Draft Protocol. This device, illustrated in Figure 1, consists of a sample holder, the pressure
application device, blue papers to detect released liquid, supporting screens, and a spacing
grid to prevent wicking. Other test devices were also tested in the collaborative study (see
section 4.0 for discussion).
2.2 SUMMARY OF METHOD
A sample of the liquid-loaded sorbent is placed into the cylindrical sample holder to a
height of 10 cm. A stainless-steel screen is placed on top of the sample; a stainless-steel
grid and absorptive blue paper are placed over the screen. A similar screen, grid, and paper
assembly is also provided at the bottom of the sample. The stainless-steel screen placed
against the sample allows fluid to pass, but blocks the movement of solid panicles from the
sample. The stainless-steel grid provides a small air gap to prevent wicking of liquid from
the sample onto the paper. A compressive force of 50 psi is applied for 10 minutes to the top
of the sample. Release of liquid is indicated when a visible wet spot is observed on either
3
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Pressure
Application
Device
Sample
Holder
Blue Paper
Stainless-Steel Grid
Stainless-Steel Screen
Stainless-Steel Screen
Stainless-Steel Grid
Blue Paper
Figure 1. Test device for Liquid Release Test.
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the top or the bottom blue paper. If the papers show no indication of liquid, the result is
termed "no release."
The LRT is an attribute test rather than a continuous variable measurement test (i.e.,
the result is either a release detected or no release detected). The LRT Draft Protocol is
presented in Appendix A.
2.3 SORBENTS AND SORBATES
The term "sorbent" refers to any solid material that is used to sorb liquid. The
mechanism for sorption may be by liquid penetration into the inner structure of an absorbing
material (absorbent) or by liquid adherence to the surface of an adsorbing material
(adsorbent). Both absorption and adsorption are reversible processes, and many materials are
capable of holding liquids by both processes. Only those sorbents that are nonbiodegradable
were considered in developing the LRT.
The term "sorbate" refers to the liquid held by the solid sorbents. Properties of
sorbates that influence sorption include viscosity, specific gravity, surface tension, solubility
in water, and electrical properties.
2.4 RELATED TESTS
2.4.1 The Pressurized Concentration (PC) Level
The pressurized concentration (PC) is defined as the maximum liquid loading for a
given sorbent/liquid combination that will not release liquid under the conditions of the
landfill environment. The PC is expressed as the ratio of liquid to dry solids times 100
([mass liquid]/[mass solid] x 100). EPA selected a pressure of 50 psi to simulate landfill
overburden. For the LRT development and validation studies, the PC for each sorbent/liquid
combination must be determined so that the LRT results can be compared to a reference
point.
As part of the effort to develop the LRT, RTI also developed a procedure to establish
the PC level. This procedure involves subjecting a sample containing excess liquid to a static
load of 50 psi for an extended time period (usually several days). The weight loss of the
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sample is monitored as excess liquid is released. The blue papers used to detect liquid
releases are also monitored. The PC is the liquid loading in the sample when releases cease
and the rate of weight loss approaches a constant low level of 0.01 g per hr or less. The
procedure to determine the PC is given in Appendix B.
2.4.2 The Saturated Concentration (SO Level
The saturated concentration (SC) level is the liquid loading for a given sorbent/liquid
combination that will release free liquid at a rate of at least one drop (typically 0.1 mL) per
minute. The SC level is determined under gravitational forces only (i.e., no static load is
applied to the sample), and serves as a reference point for evaluating an upper bound for the
liquid loading in test samples. Samples with liquid loading above the SC cannot be evaluated
in the LRT because they would release liquid without applying a static load.
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3.0 SINGLE-LABORATORY VALIDATION
The objective established by EPA for the validation study was to determine the liquid
loading, if any, relative to the PC, at which the LRT gives consistent results. To validate the
improved LRT protocol. RTI tested several sorbent/sorbate combinations and examined the
effects of several possible variables on the test results. This work was carried out during the
spring and summer of 1988.
3.1 SORBENTS AND SORBATES TESTED
Most of the LRT method validation tests were carried out with two sorbent/sorbate
combinations: Floor Dry/water and Safe-Step/motor oil. These two combinations represent
properties likely to be encountered in the materials subject to the LRT. Additional sorbents
(Vermiculite, SND-M, and Imbiber Beads®) were also tested to demonstrate method
performance. Properties of these sorbents are given in Table 1.
The sorbent/sorbate combinations tested were Vermiculite/0.01 N calcium sulfate;
SND-M/water with 5% acetone; SND-M/diesel fuel; and Imbiber Beads®/diesel fuel.
Properties of the various liquids that were tested are given in Table 2. Water was selected as
a test liquid because it is present in so many liquid wastes. To simulate groundwater or
surface water, calcium sulfate was added to the water used in testing Vermiculite. Motor oil
and diesel fuel were selected to represent a broad spectrum of nonpolar organic solvents and
petroleum products.
Imbiber Beads® were selected to represent the organic polymer sorbents that are used
to sorb petroleum products and other organics. See section 3.8 for a discussion of the tests
using Imbiber Beads®.
3.1.1 Sorbent Processing and Splitting
The sorbent materials used in the method validation experiments are distributed in
relatively small quantities (typically 25-lb. bags or smaller). Because of the large number of
tests needed to validate the method for a given sorbent, it was necessary to use material from
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TABLE 1. SORBENT PROPERTIES*
CLASS OR PROPERTY
Material Class
Special Features
Bulk Density lb/ft3
Sorbenc Density
(no voids) (lb/ftj)
Sorplion Capacity
(grams liquid per gram sorbcul):
will) water
witli aliphatic Hydrocarbon
with aromatic Hydrocarbon
Source
Biodegradable
FLOOR DRY
diatomiie
Granular
24 to 25**
156
1.4
II
2.1
Eagle-Picher
Minerals.
Inc., Cincinnati, OH"
No
SAFE STEP
sorbent clay
fine particles
37
137.2
1.0
0.7
0.8
Andesile of
California, Inc.
No
SND-M
sorbent clay
fine particles
29-36
137.2
1.0
0.7
0.8
Oil Dry
Corporation
Chicago, IL
No
VERMICULITE
expanded
mineral
loose particles
(compressible)
5-10
149.7
5.5
3.5
4.5
No
IMBIBER BEADS®
cross-linked polymer
(poly t-butylstyrene
spheres)
38
59.9
2.5
16.3
18.3
EMCO
Little Rock, AR
Undetermined
' Dala arc from EPA/600/2 87/047 (Melvold and Gibson, 1987). unless olherwise indicated
Personal communication: Mr John K Craig, Eagle Picher, Inc., to Ms. Paula Hoffman, August 18, 1987.
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TABLE 2. PROPERTIES OF TEST LIQUIDS
DESCRIPTION OR
PROPERTY
Description of liquid used
in collaborative study
Specific Gravity
Surface Tension
Kinematic Viscosity
(Ccnlipoisc)
WATER
Dcionizcd Water
1.00
72 dynes/cm @
25°C
1 .0 (a) 20°C
-0.5 @ 55°C
MOTOR OIL
SAE 50 weight motor oil
(Valvoline)
0.89
325 @ 40°C
2l-23@ 1(X)°C
DIESEL FUEL
Qean liquid, yellow color,
faint odor of petroleum
hydrocarbon
0.86
3. 1 @ 40°C
ACETONE (5%)
IN WATER
Dcionized water with 5%
acetone, a polar organic solvent
0.99
55.5 dynes/cm 25°C
0.3 16 @ 25°C
(for pure acetone)
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several lots. RTI took special care in combining and blending the dry material from separate
lots to provide a uniform matrix for testing. The total volume of dry sorbent was processed
and then split into aliquots of the appropriate volume for testing. A riffle splitter was used
for all splitting operations.
The splitting scheme used to obtain the individual samples of sorbent is shown in
Figure 2. The first operation was to blend the material from different bags of sorbent.
Individual bags of sorbent (labeled No. 1, No. 2,...No. n) were each split into four equivalent
portions, labeled A, B, C, and D. After all bags were split in this way, all the portions
labeled "A" were combined, and likewise for all the "B", "C", and "D" portions. This
operation yielded four large equivalent portions of the subject sorbent.
The second operation was to split each portion repeatedly until samples of an
appropriate size for testing (i.e., approximately 200 g) were obtained. Each sample was
placed in a 1-L wide-mouth glass bottle, capped, and sealed with parafilm.
3.1.2 Sorbent Moisture Content
The moisture content of the various sorbents is not constant. It varies, depending on
the type of sorbent and the lot. In order to control the total liquid loading in the mixtures
tested, one must know the initial moisture content in the sorbent before addition of the test
liquid.
In previous work using Floor Dry, the bulk material was air-dried prior to splitting so
that the moisture content was essentially zero prior to the addition of sorbate. Because of the
very large quantity of material needed for the 1988 method validation, it was not practical to
dry the bulk sorbent completely before the blending and splitting operations. In addition,
there was concern that if the sorbent were processed in a bone-dry condition, it would tend to
sorb moisture from the air, the extent depending on the length of time the various samples
were exposed to the ambient conditions. To take into account the inherent moisture, RTI
processed the bulk material without drying and then estimated the average moisture content
([grams of water/grams of solid] x 100) for the split samples.
10
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Combined all A's
B's
Cs
D's
A 3
A B C 3 A3
A B C D A3
Figure 2. The splitting scheme used to obtain individual samples of sorbent for LRT testing.
11
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To estimate the average moisture content, four of the sealed bottles of Floor Dry, each
containing 200 grams of sorbent. were selected at random and tested to determine moisture
content. These samples were weighed and then oven-dried at 93.3°C (200°F) for 24 hours.
The cooled samples were weighed again. Heating was repeated until constant weight was
attained (i.e., there was no further weight loss upon further heating). Moisture content for the
four Floor Dry samples ranged from 1.00% to 1.35% and averaged 1.10%. The average
moisture content of 1.10 was taken into account when the Floor Dry samples were prepared
to achieve a specific liquid loading for the LRT validation testing.
3.2 EQUIPMENT CALIBRATION
Four ADM devices were used in the test validation experiments. These devices were
calibrated prior to the test effort to ensure that the pressure application was correct. The
procedure for calibration and the calibration data are given in Appendix C. All device
calibrations were performed by Dr. Ray Borden of the Nonh Carolina State University's Civil
Engineering Laboratory.
3.3 SATURATED CONCENTRATION AND PRESSURIZED CONCENTRATION
DETERMINATIONS
Tests were conducted to establish the SC and PC for each sorbent/sorbate combination.
The procedures to determine the SC and PC are described below:
A pre-weighed, dry sorbent (e.g., 250 g Floor Dry; 450 g Safe-Step) is saturated for 24
hours in an excess amount of the sorbate. The sorbent is then placed in a pre-weighed
dry LRT sample holder and allowed to drain under force of gravity for 15 minutes.
The wet sorbent and sample holder are then weighed. The SC is the liquid loading in
the sample ([grams liquid/grams solid] x 100) immediately following the gravity drain.
The sample holder with drained sorbent is placed in the pressure device. A static load
of 50 psi is applied. After one hour, the compression on the sample holder is released.
The sample and holder are re-weighed to determine the liquid weight loss. Dry filters
are set in place, and the load is reapplied. The sample and holder are re-weighed at
regular intervals. This is continued until no visible release is detected on the blue
12
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papers. The test is concluded at this point The rate of liquid loss is calculated. The
PC level is the liquid loading in the sample when the rate of liquid loss reaches 0.01
g/hr or less.
In duplicate tests, good agreement was seen in the results obtained for Floor Dry/water.
Safe-Step/mo tor oil, and Oil Dry/acetone (5% in water). The PC results for Vermiculite are
questionable because small particles of sorbent were lost in one of the tests. The results of the
PC determinations are summarized in Table 3. The raw data are provided in Appendix B
along with the detailed procedure used for the determinations.
3.4 LRT RESULTS AT DIFFERENT LIQUID LOADING LEVELS
To validate the method, different sorbent/sorbate combinations were tested with liquid
loadings above and below the PC level. Multiple samples were tested at each liquid loading
level. Raw data for the LRTs performed for all sorbent/sorbate combinations are given in
Appendix D.
The test results for Floor Dry with water and for Safe-Step with motor oil are
presented in Figures 3 and 4, respectively. The LRT results for samples with liquid loadings
well above the PC level show consistent releases. The experimentally determined SC levels
and PC levels are also shown in these figures. For Floor Dry/water tests, all samples with
liquid loading at or above 137 (1.1 times the PC level) gave releases. For Safe-Step/oil, all
samples tested at liquid loadings at or above 32 (approximately 1.5 times the PC level) gave
releases.
The test results for SND-M with diesel fuel are presented in Figure 5. These data
show the pattern of releases versus no-releases spanning the range of liquid loading from 70
(0.7 g liquid per g solid) to 90 (0.9 g liquid per g solid). At a liquid loading of 70, none of
the eight samples tested gave a release, whereas all nine samples tested at a liquid loading of
85 gave releases. Some of the samples with liquid loadings between 75 and 87 gave releases,
and some did not. Only one anomalie was seen: in the six samples with liquid loading at 87.
all but one gave releases.
13
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TABLE 3. SATURATED CONCENTRATION (SC) AND
PRESSURIZED CONCENTRATION (PC)
FOR SORBENT/SORBATE COMBINATIONS*
SORBENT/SORBATE
Floor Dry/Water
Safe- Step/Motor Oil
SND-M/Acetone (5% in water)
SND-M/ Diesel Fuel
Vermiculite/0.01 N Calcium Sulfate
PC Level
125.0
124.6
22
22
102.7
100.6
ND**
150
(2ior
SC Level
(approximate)
140
30
118
ND**
160
* The SC and PC are expressed as the ratio of grams of liquid to grams of solid,
multiplied by 100. Refer to Appendix B for the raw data for each determination.
** Not determined.
Result is questionable due to loss of panicles with the liquid.
14
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u
K
ti
10
9
a
7
6
3
4
3
2
1
0
1
2
3
4
5
6
7
a
9
10
No Release
Release
PC
sc
120 123 130 133 133 137
Liquid Loading Ltv«l
Figure 3. LRT results: Floor Dry/water.
140 142
10
9
8
7
6
5
4
3
2
1
0
1
2
3
4
s
6
7
a
9
10
No Release
PC
Release
sc
20 22 25 28 30 32
Liquid Loading L«v«l
40
Figure 4. LRT results: Safe-Step/oil.
15
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70
75
77 80
Liquid Loading l«v«i
85
90
Figure 5. LRT results: SND-M/diesel.
16
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The test results for SND-M with acetone (5% in water) and Vermiculite with 0.01 N
calcium sulfate solution are presented in Figures 6 and 7, respectively. Even with the small
number of samples of the SND-iM/acetone combination tested, the pattern of results shows all
releases in samples close to the SC level and both release and no-release results as the liquid
loading approaches the PC level. The tests for the Vermiculite/calcium sulfate combination
span a wide range of liquid loadings. Two samples with liquid loading at 150 (1.5 g liquid
per g solid) both gave releases as did all samples tested with liquid loading above 200.
Results from nine samples with liquid loadings ranging from 110 to 130 included both
releases and no-releases.
3.5 RESULTS OF PAINT FILTER LIQUIDS TEST
All hazardous materials to be disposed in landfills are required to pass the Paint Filter
Liquids Test (PFLT), known as SW-846 Method 9095 (U.S. EPA, 1986). The complete
method for the PFLT is given in Appendix E.
The PFLT was performed on several sorbent/sorbate combinations to see how results
compared with those of the LRT. The PFLT differs from the LRT in that a smaller sample
(100 g) is used, and there is no compression of the sample other than gravity. The test
duration is also shorter (5 minutes compared to 10 minutes for the LRT).
Samples of Floor Dry/water and Safe-Step/oil were tested at several different liquid
loadings. The results are shown in Figures 8 and 9, respectively, along with the LRT results.
For the Floor Dry/water samples. Method 9095 showed releases at liquid loadings as low as
125 (i.e., 1.25 g water per 1.00 g dry sorbent), while the lowest LRT releases occurred at 135
(1.35 g liquid per g dry sorbent). This suggests that Method 9095 is, at least for some
sorbates, a more stringent test than the LRT. For oily liquids, however, the LRT appears to
be more stringent. This is demonstrated by the test results for the Safe-Step/motor oil
combination. No releases of motor oil were observed, even in samples with liquid loading of
50 (i.e., 0.50 g oil per 1.00 g dry sorbent) in the Method 9095 whereas the LRT showed
releases at oil loadings as low as 25 (0.25 g oil per 1.00 g dry sorbent). These results suggest
17
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s
•8
10
9
a
7
6
3
4
3
2
1
0
1
2
3
4
3
6
7
8
9
10
NO
PC
I
sc
102 103 110.7
Liquid Loading L«v«4
113
1 18
Figure 6. LRT results: SND-M/acetone in water (5% solution).
18
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10
9
8
7
6
3
4
3
2
1
0
1
2
No
4
5
6
7
8
9
10
Releas*
I
PC
I
I
SC
I
—i 1 1—
no I 130
120
I 160
150
Liquid loading L«v«l
213
231
Figure 7. LRT results: Vermiculite/calcium suifate.
19
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7
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1 20 125 1 30 1 33 1 35 1 37 1 40 1 42
Liquid Looding L«v«l
LRT Results RS^N PFLT
Figure 8. LRT and PFLT results: Floor Dry/water.
•I
K
IU
9
a
7
6
5
4
3
2
1
1
2
3
4
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6
7
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;
No Release
Release
20 I 22
29
28
32
Liquid Loading L«v«l
LRT Result* R^CSl PFLT
40
Figure 9. LRT and PFLT results: Safe-Step/motor oil.
2U
-------
that the two methods should be used in combination to determine whether an unknown
sample contains releasable liquid. The PFLT should be performed first since it is a simpler
test. If a sample gives releases in the PFLT, there is no need to perform the LRT.
3.6 RESULTS WHEN SAMPLE HEIGHT IS ALTERED
The ADM test cell holder is designed to be filled to a height of 10 cm. To test the
effect of sample size, 5-cm samples of Floor Dry/water and Safe-Step/oil, with four different
liquid loadings, were tested. The results of these tests along with the results from similar 10-
cm test samples are shown in Figures 10 and 11. These results indicate that the smaller
samples give less consistent results, evidence that the LRT is sensitive to sample size.
3.7 RESULTS WHEN TEMPERATURE IS ALTERED
The viscosity of most liquids decreases as temperature increases; thus, it is likely that
the temperature of sorbent/sorbate test samples will affect LRT results. To test the effects of
temperature on the LRT, samples of SND-M with diesel fuel were prepared with liquid
loadings ranging from 70 to 90 (0.7 to 0.9 g liquid per g dry sorbent). Samples at each
loading were tested at 4°C and 40°C. Results of these tests, along with test results for
samples at 23°C, are presented in Figure 12. As expected, releases occurred in the heated
samples at liquid loadings below the lowest liquid level giving releases in the colder samples.
At a liquid loading of 85 (0.85 g liquid per g sorbent), all samples tested at 23°C and 40°C
gave releases whereas three releases and three no-releases were seen for the samples tested at
4°C.
In some instances, materials that have been exposed to extreme outdoor temperatures
during transport will need to be tested. For example, sorbed waste in drums transported by
truck during hot weather may reach temperatures above 40°C. In cold weather, the
temperature may be well below 0°C. If samples are taken from drums on the truck and
brought directly to the laboratory, for consistent results, the samples should be brought to
room temperature before testing.
21
-------
I
i
1U
9
8
7
0
5
4
3
2
1
1
2
3
4
5
6
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9
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-
-
-
.
No RaleaM
a
ReleaM
I PC
1
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-
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120 125
130 133 135 137 140 142
Liquid Loo
BfiflJJH 10-cm sompfe*
E
10
9
8
7
S
4
S 2
* 0
* i
1 2
| 3
4
s
«
7
8
9
10
;igure 10. LRT results
.
-
-
-
I
1
1
1
1
1
1
1
1
1
1
-
-
-
1
1
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i
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: PC
20 1 22 1
' 128
din? L«v«<
ESS 3-cm sompta.
for 5-cm and 10-cm samples of Floor Dry/water
n
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i
»
sc
30 32
No R408M
R«lMM
1
. m.f+
29
Liquid Loodinq
10-cm Mmpl««
5-cm
Figure 11. LRT results for 5-cm samples and 10-cm samples of Safe-Step/motor oi
oil.
22
-------
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6
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2
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70
73 77
80 83 89 87
90
Liquid Looking
23 4«?r««i c*lciu« KSSSN 4 d«qr««« c«lciu» V/SSl 40
-------
3.8 DISCUSSION OF IMBIBER BEADS®
The sampling and testing of organic polymer sorbents pose problems that could not be
resolved in the LRT development and validation studies. RTI attempted to test a mixture
consisting of the sorbent Imbiber Beads® (IB) and diesel fuel in the ADM LRT device with
the following results.
At low liquid loading levels (0.1 to 0.2 g liquid per g sorbent), IB could be transferred
easily to the LRT sample holder. After compression at 50 psi for 10 minutes, however, the
sample was a solid mass. To remove the sample from the cell was extremely difficult
(eventually it had to be hammered out). At low liquid loading levels, no release of liquid was
observed.
At higher liquid loading levels (above 0.4 g liquid per g sorbent), the beads appeared
to polymerize, forming a solid rubber-like mass. The material appears to be altered
irreversibly. In this form, the material had to be cut into small pieces in order to transfer it to
the sample holder. The irreversible behavior of this material suggests that use of IB
constitutes a solidification technique rather than sorption.
24
-------
4.0 THE COLLABORATIVE STUDY DESIGN
The purpose of the collaborative study was to assess the interlaboratory variability of
the method and to demonstrate consistency of test results. In addition to evaluating the
method protocol developed for use with the ADM test device, the collaborative study also
provided an opportunity for other manufacturers to demonstrate equivalency of their devices
to detect liquid release.
Five laboratories that had participated in the previous study (in the fall of 1987) agreed
to assist again by testing samples using the 1988 Draft Protocol and the ADM test device.
One additional laboratory also agreed to participate. Thus, the collaborative study included
six participating laboratories plus RTI. Ultimately, a total of 36 tests were performed by each
of the six participating laboratories: six samples at each of three different liquid loadings for
two different sorbent/sorbate combinations. A total of 42 tests were performed for Floor
Dry/water at each of three different liquid loadings. For Safe-Step/oil, 42 tests were
performed at two liquid loadings, and 37 tests were performed at one liquid loading.
4.1 PARTICIPATING LABORATORIES
The laboratories listed below participated in the 1988 collaborative study:
• Chemical Waste Management. Inc., Riverdale, IL
GSX Services, Pinewood. SC
• Industrial and Environmental Analysts, Inc., RTP, NC
Microbac Laboratories, Inc., Erie. PA
• Western Research Institute, Laramie, WY
Wilson Laboratories. Salina. KS (WL)
Research Triangle Institute. RTP, NC (RTI)
Using the ADM LRT device, these laboratories tested the samples prepared by RTI.
25
-------
4.2 OPPORTUNITY TO DEMONSTRATE EQUIVALENCY
The collaborative study also provided an opportunity for companies to demonstrate
equivalency of other test devices. Three participating laboratories received sets of samples so
that they could perform tests in an alternate device. The laboratories and the devices they
tested are Chemical Waste Management, Inc., (their own device); Analytical Testing and
Consulting (their own device); and Western Research Institute (WRI) (Millipore device).
Prior to the study, drawings of these devices and the test protocol to be used were sent to RTI
for review.
Two of the alternate test devices use sample cells similar in size to the ADM cell. The
Millipore device requires a somewhat larger sample.
4.3 DEVICE CALIBRATION
All of the ADM test devices used in the collaborative study were previously calibrated
for the 1987 collaborative study to ensure that the pressure application by each device was
correct and consistent between devices. Immediately prior to the 1988 collaborative study,
each device was recalibrated to be certain that there would be a minimum variation in the
vertical pressure imposed on the samples tested in different devices at different laboratories.
The recalibrations also served to indicate how frequently recalibration of the ADM device is
needed to maintain consistency in the pressure readings. The device calibrations were
performed by Dr. Roy Borden, Department of Civil Engineering, North Carolina State
University. The calibration method is presented in Appendix C.
4.4 SORBENT/SORBATE COMBINATIONS
The sorbent/sorbate combinations selected for the collaborative study were Floor
Dry/water and Safe-Step/motor oil. These same sorbents/sorbate combinations were used in
the 1987 study. Using these same combinations again allowed verification that the problems
identified in 1987 had been effectively corrected. (See RTI, 1988a, for discussion of the 1987
study.) These two sorbent/sorbate combinations presented different types of problems from
the standpoint of handling and testing.
26
-------
Properties of Floor Dry and Safe-Step are given in Table 1, and the properties of
deionized water and Valvoline SAE 50 weight motor oil are listed in Table 2 (see section
3.0).
The PC levels for water in Floor Dry and for oil in Safe-Step were determined in long-
term tests as explained in section 3.3. The liquid loadings for samples to be tested in the
collaborative study were selected based on the experimentally determined PC level for each
combination.
In the method validation study, the Floor Dry/water combination showed a PC of
125%. For samples with known liquid loadings above the PC level, the LRT results showed
a very narrow range of liquid loadings, going from zero releases to all releases (i.e., six
samples tested at a liquid loading of 133 gave zero releases while eight samples tested at a
liquid loading of 137 all gave releases; see Figure 3). The Safe-Step/oil combination showed
a PC of 22%. LRT results for Safe-Step/oil showed a broad range of liquid loadings in the
transition region between zero releases to all release results (see Figure 4).
Each participating laboratory initially received two groups of Floor Dry/water samples
and two groups of Safe-Step/oil samples. Six separate replicate samples comprised each
group. The liquid loadings in the test samples and the relationship to the PC are given in
Table 4.
4.5 SAMPLE PREPARATION
As in the LRT development and validation testing, it is important that all collaborative
study samples prepared from a given sorbent be as uniform as possible. To minimize the
effects of sorbent variability on the replicate tests, samples of dry sorbent for the study were
prepared from a very large single batch of sorbent. Since the total quantity of sorbent needed
exceeded the amount in a single shipment or lot, separate lots of sorbent were combined (as
illustrated in Figure 2, section 3.0) to make an acceptably large batch. This large batch was
split repeatedly into two equivalent ponions (using a riffle sample splitter) until samples were
obtained of approximately the quantity necessary for a single test.
27
-------
TABLE 4. LIQUID LOADING IN COLLABORATIVE STUDY SAMPLES
SORBENT/SORBATE
COMBINATION
Floor Dry/Water
(group 1)
(group 2)
Safe-Step/Oil
(group 1)
(group 2)
LIQUID LOADING*
AT PC
121.3
125.4"
22
LIQUID LOADING*
IN TEST SAMPLES
(SIX REPLICATES)
110
135
138
19.8
33
28
RELATIONSHIP
TO PC
0.9 PC
1.1 PC
1.1 PC
0.9 PC
1.5 PC
1.27 PC
Liquid loading, expressed as percentage, is defined as g liquid per g dry sorbent times
100.
Recalculated based on revised data.
28
-------
4.5.1 Floor Dry
Because the test development and validation studies required such a large number of
samples, there was insufficient material from the initial sorbent batch to supply samples for
the 1988 collaborative study. A separate large batch of Floor Dry had to be obtained and
split. About 250 200-g samples were needed. The same splitting scheme described in section
3.1.1 was again used to prepare the samples. Each 200-g split was placed in a 1-L wide-
mouth glass bottle, capped, and sealed with parafilm. These sorbent samples were labeled
sequentially (Zl, Z2,...Z250) and stored until time for use.The average moisture content in the
new batch of samples was needed to prepare test samples to a prespecified liquid loading for
the collaborative study. To estimate the average moisture content of the new Floor Dry
samples, moisture determinations were performed (as described in section 3.1.2) on four of
the sealed 200-g samples, selected at random. The results of the four moisture determinations
ranged from 0.90% to 1.15% and averaged 1.06%.
4.5.2 Safe-Step
A sufficient quantity of material was processed and split at the beginning of the
method validation study to supply samples for the collaborative study. Thus, no new
processing steps were needed.
4.6 DISCUSSION OF COLLABORATIVE STUDY DESIGN
The collaborative study was designed to evaluate the method's capability to reproduce
results obtained previously by RTI for specific sorbent/sorbate combinations. In particular,
the study objectives were to:
evaluate the probability of passing a wet sample (i.e., a sample with liquid
loading above 1.1 PC for Floor Dry/water and above 1.5 PC for Safe-Step/motor
oil);
• evaluate the probability of failing a dry sample (i.e., a sample with liquid loading
below 0.9 PC); and
assess interlaboratory precision.
29
-------
Since the result from an individual test is either a release or a non-release, the results
of a large number of tests are expected to have a binomial probability distribution. Based on
this distribution, Figure 13 shows that a design having 36 analyses of any one mix will have a
somewhat limited power to correctly find that the test is unacceptable if, in fact, the error rate
for the test is too high.
The figure shows that having 0 wrong results out of 36 samples implies that the true
probability of getting a wrong result for that mixture is less than 8% based on the 90% upper
confidence level (UCL). If the study shows that 8 out of 36 results are wrong, then the true
probability of a wrong result is somewhere between 12% (90% lower confidence limit [LCL])
and 37% (90% upper confidence limit [UCL]).
Six samples at each liquid loading for each sorbent/sorbate combination were provided
to each laboratory. This gives a total of 42 samples for each liquid loading, providing a
design of slightly higher power than the sample size of 36 evaluated in Figure 13. Figure 14
shows the power of the experimental design used for the collaborative study. The design is
for a sample size of 42 (n = 42) (i.e., 7 laboratories X 6 replicates for each sample type).
The collaborative study was designed to test the null hypothesis (H0) that the true
probability of passing a wet sample or of failing a dry sample is p = 0.1 versus the alternative
(Ha) that the probability exceeds 0.1. With the 42 test design, the null hypothesis is rejected
if more than 8 wrong results are observed. In Figure 14, the box entitled "Tail Area
Probabilities" shows that the probability (area) of accepting the null hypothesis when it is true
is greater than 95%. This information is presented graphically with the tail area probabilities
as the ordinate and the numbers of failures as the abscissa.
Another item of concern is the power of the design to reject the null hypothesis if it is
false. The power is given by (1 - beta). As seen in the box in Figure 14, if the true
probability of passing a wet sample or of failing a dry sample is p = 0.2, then the probability
of rejecting the null hypothesis (power) is approximately 1 - 0.19 = 0.81.
30
-------
O.4
0.35
o:
c.
o
O.3
0.25
-------
Sample Size: n = 42
Tail Area Probabilities
Ho :
Hal :
Ha2 :
p = 0 . 1 Alpha = 0.1
p = 0.2 Beta 1 = 0.19
p = 0.3 Beta 2 = 0.0012
Critical Value = 6.69
2
6
7
8
9
Area
0 .88
0.95
0.98
0.99
(Area = probability of X cr
fewer failures in 42 trials,'
I
0.22
0.2
O.18
O.1 6
O.14.
O.I 2
O.I
O.O8
O.O6
O.O*
O.O2
O
Probability Mass Function
Binomial Random Variable
J
\
O1 23*56789 1O 11 12
Number of Failures in 42 Trials
Cumulative Distribution Function
Binomial Random Variable
'.a
E
O 1 2 3 4- 5 6 78 9101112
Number of Failures in 4-2 Trials
Figure 14. Experimental design parameters.
32
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5.0 DISCUSSION OF THE COLLABORATIVE STUDY RESULTS
5.1 RESULTS USING THE ADM DEVICE
The collaborative study results from all tests conducted using the ADM device are
shown in Table 5 (see Appendix F for a complete data set). The Floor Dry/water and Safe-
Step/oil results both show four releases for samples with liquid loading at 0.9 PC. Since this
is below the critical number of wrong results allowed by the design (see Figure 14), there is
no reason to reject the H0 that the true probability is 0.1 of failing a sample with a liquid
loading of 0.9 PC.
The Floor Dry/water results showed 24 releases (out of 42 tests) for the samples with a
liquid loading of 135 (1.1 PC). After the results were reported, a third group of Floor
Dry/water samples was tested at a slightly higher liquid loading (138). From these 42 tests,
26 releases were reported. This is not significantly different from the results for the samples
loaded at 135. Both groups of wet samples give sufficient evidence to reject the H0 that the
true probability is 0.1 of passing a sample with a liquid loading at 135 to 138.
These Floor Dry/water results indicate that a liquid loading of 138 is still within the
transition region where both releases and non-releases are observed. The transition region
may, in fact, extend beyond 1.1 times the PC for the Floor Dry/water combination. Another
explanation is that the error associated with the PC determination is such that the samples
with liquid loading at 138 are very close (say, within 5%) to the true PC. There is
insufficient information on the particular batch of sorbent used in the collaborative study to
draw a meaningful conclusion on this issue.
The Safe-Step/motor oil samples with a liquid loading of 33 (1.5 PC) all gave releases.
After these results were reported, a third group of Safe-Step/motor oil samples with a liquid
loading of 28 (1.27 PC) was tested. Out of 37 tests, all but two gave releases. Thus, the null
hypothesis is not rejected for either of the two wet samples. The results indicate that a liquid
loading of 1.5 PC is above the edge of the transition zone that gives both releases and non-
releases.
33
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TABLE 5. RESULTS FROM THE 1988 COLLABORATIVE STUDY USING ADM DEVICES
LIQUID LOADING LEVEL*
(relationship to PC)
Lab #1
Lab #2
Lab #3
Lab #4
Lab #5
Lab #6
RTI
TOTAL
NUMBER
OF
RELEASES
TOTAL
%
RELEASE
NUMBER OF RELEASES FOR FLOOR DRY AND WATER**
110
(0.9 PC)
135
(I.I PC)
138
(1.1 PC)+
0
4
3
1
3
1
0
4
3
1
2
3
0
3
5
2
2
5
0
6
6
4
24
26
9.5
57.1
b 1 .9
NUMBER OF RELEASES FOR SAFE STEP AND OIL**
19.8
(0.9 PC)
28
(1.27 PC)
33
(1.5 PC)
1
6
6
0
6
6
0
6
6
0
5
6
1
6
6
2
5
6
0
1±
6
4
35
42
9.5
94.6'
I(X).()
OJ
-b.
Liquid loading is expressed as (g of liquid per g dry sorbent) x (100).
Each laboratory tested six samples of each sample type, except as noted.
Based on a recalculation of the PC
Only one sample was tested.
35 releases out of 37 samples lested
-------
5.2 RESULTS USING OTHER DEVICES
Table 6 summarizes the data from three participating laboratories using devices other
than the ADM device. These tests were conducted to demonstrate equivalency to the ADM
device. Equivalency test results for Floor Dry/water samples showed 0 releases for samples
with liquid loadings of 110 (0.9 PC). For wet samples with a liquid loading at 135, half of
the 18 samples gave releases. All of the wet samples with a liquid loading at 138 gave
releases. These results indicate that the devices tested performed at least as well as the ADM
device for the Floor Dry/water samples.
In the tests of the Safe-Step/oil samples, the CWM device showed three releases out of
five tests for the samples with a liquid loading at 19.8 (0.9 PC); no releases were reported
from six tests conducted in each of the other devices. All samples with a liquid loading at 33
(1.5 PC) gave releases. The performance of these devices appears to be at least as consistent
as the ADM device. The Millipore device and the device by Analytical Testing and
Consulung performed parucularly well. The results obtained using the CWM device for the
dry sample suggest that it gives a more stringent test.
-------
TABLE 6. RESULTS FROM 1988 LRT COLLABORATIVE STUDY EQUIVALENCY TESTS
LIQUID LOADING
LEVEL*
NUMBER OF RELEASES
CWM
DEVICE
MILLIPORE
DEVICE
ANALYTICAL
TESTING
DEVICE
TOTAL
NUMBER
OF TESTS
TOTAL
NUMBER
OF
RELEASES
TOTAL
%
RELEASE
FLOOR DRY AND WATER
no
(0.9 PC)
135
(1.1 PC)
138
(1.1 PC)
0
0
6
0
5
6
0
4
6
18
18
18
0
9
18
0.0
50.0
100.0
SAFE-STEP AND OIL
19
(0.9 PC)
33
(1.5 PC)
3"
6
0
6
0
6
17
18
3
18
17.6
100.0
_
a*
Liquid loading is expressed as (g of liquid per g dry sorbent) x (100).
Only 5 samples were analyzed in the CWM device.
-------
6.0 QUALITY ASSURANCE
A Quality Assurance Project Plan (RTI. 1988b) for the LRT method development and
evaluation effort is provided as a companion document to this report.
37
-------
7.0 CONCLUSIONS/RECOMMENDATIONS
Based on the results of the method validation testing and the 1988 collaborative study.
the following conclusions were drawn:
• Overall, the LRT method, as tested, showed improvement over the Draft Protocol
evaluated previously.
• The LRT is, for some sorbent/sorbate combinations, a more stringent test than the
PFLT (Method 9095), and for some combinations, the PFLT is more stringent.
Based on this finding, use of the two tests in combination should be considered.
The PFLT should be performed first, since it requires only minimal equipment, a 5-
minute test time, and minimal cleanup time.
The LRT is sensitive to sample size. Therefore it is important to use a consistent
sample volume to determine liquid release. If devices other than the ADM device
are used in equivalency demonstrations, sample volume should be considered in
determining equivalency to results from the ADM device.
«
• The LRT results are affected by temperature. For consistent results,
samples should be brought to a reasonable room temperature (e.g., 23°C)
prior to testing.
• The LRT method has not been demonstrated for sorbents that polymerize in
the presence of certain sorbates (e.g.. Imbiber Beads® with petroleum
products).
• Comparing the single-laboratory results to the collaborative study results (i.e..
comparing Figures 3 and 4 to Table 5) shows the multilaboratory results to be
slightly more aberrant. In the collaborative study, the LRT method passed dry
samples more than 90% of the time for the two sorbent/sorbate mixtures; this is
acceptable. The method performed well on the Safe-Step/oil sorbate wet samples at
both 127% and 150% PC.
The collaborative study did not demonstrate acceptable performance of the LRT
method for the Floor Dry/water samples with liquid loadings at 135 and 138.
• In general, interlaboratory differences do not appear to be unreasonable.
The failure of certain wet samples to show releases is probably due to the
close proximity of the liquid loading to the PC level. When liquid loading is close
to the PC level, multiple tests show releases and no-releases.
• The equivalency results indicate that other devices perform as well as the
ADM device, albeit with less test data.
38
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8.0 REFERENCES
1. Craig, John R.. 1987. Personal communication from Mr. Craig, Eagle Picher Minerals,
Inc., Cincinatti, OH to Ms. Paula Hoffman, Research Triangle Institute, RTP, NC.
August 18, 1987.
2. Melvold, Robert W. and Steven C. Gibson. 1987. Guidance Manual for Selection and
Use of Sorbents for Liquid Hazardous Substance Releases. Prepared for U.S. EPA -
Cincinnati, OH, by Environmental Monitoring and Services, Inc. Newbury Park, CA.
EPA/600/2-87/047. July 1987.
3. U.S. EPA. 1986. Test Methods for Evaluating Solid Waste, Physical Chemical Methods
(SW-846).
4. RTL I988a. Fall 1987 Liquid Release Test Collaborative Study Report (Draft).
Prepared by Paula Hoffman, Research Triangle Institute, RTP, NC, under EPA Contract
68-01-7075, WA 76. Submitted to Project Manager Barry Lesnick, U.S. EPA, OSW.
January 1988.
5. RTI. I988b. Further Development of the Liquid Release Test, Quality Assurance
Project Plan. Prepared by Research Triangle Institute, RTP, NC, under EPA Contract
68-01-7075, WA 76. Submitted to Work Assignment Manager Barry Lesnick, U.S.
EPA, OSW. April 1988.
39
-------
APPENDIX A
LIQUID RELEASE TEST (LRT)
1988 DRAFT PROTOCOL
A-l
-------
LIQUID RELEASE TEST (LRT) PROCEDURE
1.0 Scope and ApplIcatlon
1.1 The Liquid Release Test (LRT) 1s a laboratory test designed to
determine whether or not liquids Will be released from sorbents when they are
subjected to overburden pressures 1n a landfill.
1.2 Any liquid-loaded sorbent that falls the EPA Paint Filter Free
Liquids Test (PFT) (SW-846 Method 9095), may be assumed to release liquids 1n
this test. Analysts should ensure that the material In question will pass the
PFT before performing the LRT.
2.0 Summary of Method
2.1 A representative sample of the liquid-loaded sorbent, standing 10 cm
high 1n the device, 1s placed between twin stainless steel screens and two
stainless-steel grids, 1n a device capable of simulating landfill overburden
pressures. An absorptive filter paper 1s placed on the side of each
stainless-steel grid opposite the sample (I.e., the stainless-steel screen
separates the sample and the filter paper, while the stainless-steel grid
provides a small air gap to prevent wlcklng of liquid from the sample onto the
filter paper). A compresslve force of 50 ps1 1s applied to the top of the
sample. Release of liquid 1s Indicated when a visible wet spot 1s observed on
either filter paper.
A-2
-------
3.0 Interferences
3.1 When testing sorbents loaded with volatile liquids (e.g., solvents),
any released liquid migrating to the filter paper may rapidly evaporate. For
this reason, filter papers should be examined Immediately after the test has
been conducted.
3.2 It 1s necessary to thoroughly clean and dry the stainless-steel
screens prior to testing to prevent false positive or false negative results.
Material caught 1n screen holes may Impede liquid transmission through the
screen causing false negative results. A stiff bristled brush, like those
used to clean testing sieves, may be used to dislodge material from holes 1n
the screens. The screens should be ultrasonlcally cleaned with a laboratory
detergent, rinsed with Delonlzed water, rinsed with acetone, and thoroughly
dried.
When sorbents containing oily substances are tested, 1t may be necessary
to use solvents (e.g., methanol or methylene chloride) to remove any oily
residue from the screens and from the sample holder surfaces.
3.3 When placing the 76 mm screen on top of the loaded sample It 1s
Important to ensure that no sorbent 1s present on top of the screen to contact
the filter paper and cause false positive results. In addition, some sorbent
residue may adhere to container sldewalls and contact the filter as the sample
compresses under load, causing wet spots on the edges of the filter. This
type of false positive may be avoided by carefully centering the 76 mm filter
paper 1n the device prior to Initiating the test. •
A-3
-------
3.4 Visual examination of the sample may Indicate that a release 1s
certain (e.g., free standing liquid or a sample that flows Hke a liquid),
raising concern over unnecessary clean-up of the LRT device. An optional 5
minute Pre-Test, described 1n Appendix A of this procedure, may be used to
determine whether or not an LRT must be performed.
4.0 Apparatus and Materials
4.1 LRT Device (LRTD): A device capable of applying 50 ps1 of pressure
continuously to the top of a confined, cylindrical sample (see Figure 1). The
pressure 1s applied by a piston on the top of the sample. All device
components contacting the sample (I.e., sample-holder, screens, and piston)
should be resistant to attack by substances being tested. The LRTD consists
of two basic components , described below.
4.1.1 Sample holder: A rigid-wall cylinder, with a bottom plate,
capable of holding a 10 cm high by 76 mm diameter sample.
4.1.2 Pressure Application Device: In the LRTD (Figure 1), pressure
1s applied to the sample by a pressure rod pushing against a piston
that lies directly over the sample. The rod may be pushed against the
piston at a set pressure using pneumatic, mechanical, or hydraulic
pressure. Pneumatic pressure application devices should be equipped
with a pressure gauge accurate to within * 1 ps1, to Indicate when the
desired pressure has been attained and whether or not 1t Is adequately
maintained during the test. Other types of pressure application
A-4
-------
FIGURE 1.
LRT Device
Pressure
Application
Device
50 psi
Piston
Sample
Sarr:3le-ho iaing Cylinder
Filter
Separator Plate
Separator Plate
Filter
Bottom Plate
A-5
-------
devices (e.g., mechanical or hydraulic) may be used 1f they can apply
the specified pressure continuously over the ten minute testing time.
The pressure application device must be calibrated by the manufacturer,
using a load cell or similar device placed under the piston, to ensure
that 50+1 ps1 1s applied to the top of the sample. The pressure
application device should be sufficiently rugged to deliver consistent
pressure to the sample with repeated use.
4.2 Stainless-Steel Screens: To separate the sample from the filter,
thereby preventing false positive results from particles falling on the filter
paper. The screens are made of stainless steel and have hole diameters of
0.012 Inches with 2025 holes per square Inch. Two diameters of screens are
used: a larger (90 mm) screen beneath the sample and a smaller (76 mm) screen
that 1s placed on top of the sample 1n the sample-holding cylinder.
4.3 Stainless-Steel Grids: To provide an air gap between the stainless-
steel screen and filter paper, preventing false positive results from
capillary action. The grids are made of 1/32' diameter, woven, stainless-
steel wire cut to two diameters, 90 mm and 76 mm.
4.4 Filter Papers: To detect released liquid. Two sizes, one 90 mm and
one 76 mm, are placed on the side of the screen opposite the sample. The 76
mm diameter filter paper has the outer 6 mm cut away except 3 conical points
used for centering the paper (see Figure 2). Blue, seed-germination filter
paper manufactured by Schlelcher and Schuell (Catalog Number 33900) 1s
suitable. Other colored, absorptive papers may be used as long as they
provide sufficient wet/dry contrast for the operator to clearly see a wet
spot.
A-6
-------
FIGURE 2. 76 mm diameter filter paper.
A-7
-------
4.5 Spatula: To assist 1n loading and removing the sample.
4.6 Rubber or wooden mallet: To tap the sides of the device to settle
and level the sample.
5.0 Reagents
5.1 Acetone.
6.0 Sample Collection, Preservation and Handling
6.1 All samples should be collected using a sampling plan that addresses
the considerations discussed 1n "Test Methods for Evaluating Solid Wastes (SW-
846)." The sampling plan should be designed to detect and sample any pockets
of liquids that may be present In a container (I.e., 1n the bottom or top of
the container).
6.2 Preservatives should not be added to samples.
6.3 Samples should be tested as soon as possible after collection, but 1n
no case after more than three days after collection. If samples must be
stored, they can be stored 1n sealed containers and maintained under dark,
cool conditions (temperature ranging between 35° and 72° F). Samples should
not be frozen.
A-8
-------
7.0 Test Procedure
The procedure below was developed for the original LRTD, manufactured by
Associated Design and Manufacturing Company (ADM). Procedures for other
LRTDs, along with evidence for equivalency to the ADM device, should be
supplied by the manufacturer.
7.1 Disassemble the LRTD and make sure that all parts are clean and dry.
7.2 Invert the sample-holding cylinder and place the large stainless-
steel screen, the large stainless-steel grid, then a 90 mm filter paper on the
cylinder base (bottom-plate side).
7.3 Secure the bottom plate (plate with a hole 1n the center and four
holes located on the outer circumference) to the flange on the bottom of the
sample-holding cylinder using four knob screws.
7.4 Turn the sample holder assembly to the rlght-slde-up position
(bottom-piate-s1de down). Fill the sample holder with a representative
sample until the sample height measures 10 cm (up to the etched line 1n the
cylinder).
7.5 Tap the sides of the sample holder with a rubber or wooden mallet to
remove air pockets and to settle and level the sample.
7.6 Repeat filling, and tapping until a sample height of 10 cm 1s
maintained after tapping.
A-9
-------
7.7 Smooth the top of the sarple with a spatula to create a horizontal
surface.
7.8 Place the small stainless-steel screen, then the small stainless-
steel grid on top of the sample.
NOTE: Prior to placing the stainless-steel grid on top of the screen, make
sure that no sorbent material Is on the grid side of the stainless-
steel screen.
7.9 Place the 76 mm filter paper on top of the small stainless-steel
grid, making sure the filter paper 1s centered 1n the device.
7.10 Using the piston handle (screwed Into the top of the piston) lower
the piston Into the sample holder until 1t sits on top of the filter paper.
Unscrew and remove the handle.
7.11 Place the loaded sample holder Into position on the baseplate and
lock Into place with two toggle clamps.
7.12 Place the pressure application device on top of the sample-holder.
Rotate the device to lock 1t Into place and Insert the safety key.
7.13 Connect air lines.
A-10
-------
7.14 Initiate rod movement and pressure application by pulling the air-
valve lever towards the operator and note time on data sheet. The pressure
gauge at the top of the pressure application device should read as specified
In the factory calibration record for the particular device. If not, adjust
regulator to attain the specified pressure.
NOTE: After pressure application the air lines can be disconnected, the
toggle clamps can be released, and the LRTD can be set aside for 10
minutes while other LRTDs are pressurized. LRTD pressures should be
checked every 3 minutes to ensure that the specified pressure 1s
being maintained. If the specified pressure 1s not being maintained
to within + 1 ps1, the LRTD must be reconnected to the air lines and
pressure applied throughout the 10 minute test.
7.15 After 10 minutes place the LRTD on the baseplate, reconnect air
lines and toggle clamps, and turn off pressure (retract the rod) by pushing
the air-valve lever away from the operator. Note time on data sheet.
7.16 When the air gauge reaches 0 ps1, disconnect the air lines and
remove the pressure-application device by removing the safety key, rotating
the device, and lifting 1t away from the sample holder.
7.17 Screw the piston handle Into the top of the piston.
7.18 Lift out the piston.
A-ll
-------
7.19 Remove the filter paper and Immediately examine It for wet spots
(wet area on the filter paper). The presence of a wet spot(s) Indicates a
positive test (I.e., liquid release). Note results on data sheet.
7.20 Release toggle clamps and remove sample holder from baseplate.
Invert sample holder onto suitable surface and remove the knob screws holding
the bottom plate.
7.21 Remove the bottom plate and Immediately examine the filter paper for
wet spots as described 1n step 7.19. Note results on data sheet. Wet spot(s)
on either filter Indicates a positive test.
APPENDIX A
1.0 Scope and Application
1.1 The LRT Pre-Test 1s an optional, 5 minute, laboratory test designed
to determine whether or not liquids will be definitely released from sorbents
before applying the LRT. This test 1s performed to prevent unnecessary clean-
up and possible damage to the LRT device.
1.2 This test 1s purely optional and totally up to the discretion of the
operator as to when 1t should be used.
A-12
-------
2.0 Summary of Method
A representative sample will be loaded Into a glass grid that 1s placed on
a glass plate already stained with 2 dyes (one water soluble and one oil
soluble). A second glass plate will be placed on top and a 2 Ib. weight
placed on top for 5 minutes. At the end of 5 minutes the base of the glass
grid 1s examined for any dye running along the edges, this would Indicate a
liquid release.
3.0 Interferences
A liquid release can be detected at lower Liquid Loading Levels with
extremely clean glassware. The glass plates and glass grid should be cleaned
with a laboratory detergent, rinsed with Oe1on1zed water, rinsed with acetone,
and thoroughly dried.
4.0 Apparatus and Materials
4.1 Glass Plate: 2 glass plates measuring 7.5 cm x 7.5 cm.
4.2 Glass Grid: See Figure 3.
4.3 Paint Brush: Two small paint brushes for applying dyes.
4.4 Spatula: To assist 1n loading the sample.
4.5 Weight: 2.7 Kg weight to apply pressure to the sample.
A-13
-------
FIGURE 3. Glass grid specifications.
A-14
-------
5.0 Reagents
5.1 Methylene Blue dye 1n methanol.
5.2 Anthraqulnone dye 1n toluene.
6.0 Sample Collection, Preservation and Handling
See LRT Procedure.
7.0 Test Procedure
7.1 Paint one strip, approximately 1 cm wide, of methylene blue dye
across the center of a clean and dry glass plate (see Figure 4). The dye 1s
allowed to dry.
7.2 Paint one strip, approximately 1 cm wide, of anthraqulnone dye across
the center of the same glass plate (see Figure 4). This strip should be
adjacent to and parallel with the methylene blue strip. The dye 1s allowed to
dry.
7.3 Place the glass grid 1n the center of the dye-painted glass plate.
7.4 Place a small amount of sample Into the glass-grid holes, pressing
down gently until the holes are filled to slightly above the grid top.
A-15
-------
Methylene Blue
Anthraquinone
v
FIGURE 4. Positioning of dye on glass plate,
A-16
-------
7.5 Place a second, clean and dry, glass plate on top of the sample and
grid.
7.6 Placed a 2.7 Kg weight on top of the glass for 5 minutes.
7.7 After 5 minutes remove the weight and examine the base of the grid
extending beyond the sample holes for any Indication of dyed liquid. The
entire assembly may be turned upside down for observation. Any Indication of
liquid constitutes a release and the LRT does not need to be performed.
A-17
-------
APPENDIX B
SATURATED CONCENTRATION (SC)
AND
PRESSURIZED CONCENTRATION (PC)
PROCEDURES AND RESULTS
B.1 Saturated Concentration Procedure
B.2 Pressurized Concentration Procudure
B.3 Experimental Data
B-l
-------
B.1 SATURATED CONCENTRATION PROCEDURE
Definition and General Description
The Saturated Concentration (SC) is defined as the Liquid-Loading Level (LLL) that results
when a sorbent is flooded with sorbate and excess liquid allowed to drain away. LLL is the ratio
of liquid weight to dry solid weight multiplied by 100. The SC for a specific sorbent/sorbate
combination is determined as part of the Pressurized Concentration (PC) determination and
provides an upper boundary for testing LLLs. The SC represents the LLL that should just start to
fail the Paint Filters Test.
A pre-weighed, dry sorbent (e.g., 200 g Floor Dry, 450 g Safe-Step) is saturated for 24 hours in
the sorbate. The sorbent is then allowed to drain using only gravitational forces until the flow
becomes negligible (less than a drop per minute). The wet sorbent is weighed and the SC value
determined by the ratio of the weight of the liquid to the weight of the dry sorbent.
Procedure
1. Weigh empty jar, and note weight to nearest tenth of gram.
2. Pour into empty jar an adequate dry, representative sample to fill 90-mm diameter, 10-cm-
high sample holder (e.g., 200 g Floor Dry, 450 g Safe-Step). Note weight to nearest tenth of
gram.
3. Determine dry sample weight by subtracting empty jar weight
4. Saturate the one-sample aliquot of sorbent for 24 hours by covering the sorbent in ajar with
the sorbate, such that all sorbent is wet and not exposed to the atmosphere.
5. Seal the jar with parafilm and shake the sample vigorously until the sorbent/sorbate are
homogenized. (NOTE: Safe-Step samples will have to be stirred rather than shaken.)
6. After 24 hours, shake the sample vigorously (NOTE: Do not re-stir Safe-Step; the sorbate
will have to be decanted due to the fine-grain size). Open the jar, place a single thickness of
ladies pantyhose over the mouth of the jar containing the saturated sorbent, turn the jar
upside down, and let the sorbate drain until the flow becomes negligible (less than one drop
per minute).
7. Weigh wet sorbent in jar, and calculate wet sorbent weight:
N
*
wet sorbent wt = wet sorbent in jar - empty jar wt
8. Calculate SC using the following equation:
SC = (wet sorbent wt - dry sorbent wt) x 100
dry sorbent wt
B-2
-------
B.2 PRESSURIZED CONCENTRATION PROCEDURE
Definition and General Description
The Pressurized Concentration (PC) is defined as the maximum Liquid-Loading Level (LLL)
which will not release liquids when subjected to 50 psi pressure over the life of the landfill. LLL
is the ratio of liquid weight to dry solid weight multiplied by 100.
Saturated sorbent is placed in a pre-weighed ADM-LRT-device sample holder. The saturated
sample is left to drain for 15 minutes and the device sample holder re-weighed. The sample
holder is placed in the device, and a pressure of 50 psi applied. After 1 hour, the pressure on the
sample holder is released and the cell is re-weighed to determine the liquid weight loss. Two dry
blue blotter papers (76-mm and 90-mm) are put into place. The pressure is immediately
reapplied and held constant (except for weighings) for hourly intervals until no visible release is
noted on the blotter papers, which are replaced at each weighing. The sample holder is then re-
weighed every 24 hours until, again, no visible release is noted on the blotter papers, which are
replaced at each weighing. The rate of liquid loss is calculated. When the rate of liquid loss
reaches 0.01 g/hr or less for three consecutive weighings, the PC LLL is calculated.
Procedure
1. Pre-weigh dry, empty ADM-LRT-device sample holder (consisting of sample holder
cylinder, flange, flange screws, piston, 2 stainless-steel screens, and 2 stainless-steel grids).
Note weight to nearest tenth of gram.
2. Attach sample holder flange to cylinder with the flange screws and with the 90-mm
stainless-steel screen and grid in place.
3. Place saturated sorbent in sample holder to the specified sample height (10 cm).
4. Place 76-mm stainless-steel screen and grid, then set the piston on top of the sample.
5. Weigh entire sample holder assembly with sorbent and piston inside. Note weight to nearest
tenth of gram.
6. Place a small pan under the drain-hole on the device to catch any sorbate that is squeezed
out.
7. Attach pressure-application device to sample holder and apply 50 psi pressure. Note time to
nearest minute.
8. After 1 hour, release the pressure, note the time to the nearest minute, remove the pressure
application device, and immediately weigh the entire sample holder assembly. Note weight
to nearest tenth of gram.
B-3
-------
9. Put in place one 76-mm and one 90-mm diameter blotter paper.
10. Immediately re-attach the pressure-application device to sample holder and apply 50 psi
pressure.
11. At the end of 1 hour, replace the blotter papers with dry blotter papers and weigh the entire
sample holder assembly, noting the weight to nearest tenth of gram. Immediately re-attach
the pressure-application device to sample holder and apply 50 psi pressure.
12. Repeat Step 11 at hourly intervals until no visible release is detected on the blotter papers.
13. Repeat Step 11 at 24-hour intervals until no visible release is detected on the blotter papers.
14. Calculate the Rate of Sorbate Lost (RSL) for each 1-hour and each 24-hour period:
RSL (g/hr) =rsample holder assembly wt - previous sample holder assembly wtl (g)
[time difference] (hours)
[Note: (g) weighed to nearest tenth of gram and hours measured to nearest tenth of an
hour.]
If this rate reaches a consistent value for three consecutive times, no further weighings are
necessary. If this rate does not reach a consistent value for two consecutive times, then
weighings should be continued until this criterion is met.
15. Calculate the SC:
SC = (wet sorbent wt at the first of (dry sorbent wt put
the two consistent RSL criteria) - in sample holder) x 100
dry sorbent wt put in sample holder
B-4
-------
PC DETERMINATIONS. FLOOR DRY & WATER
HTI-000 DEVICE DRY & CLEAN WT.: 3678 8 g
HTI000 DRY SAMPLE WT 167.7 g.
PRESSURE. SOpsi
B.3 Experimental Data
00
DATE
TIME delta TIME RTIOOO WEIGHT delta WEIGHT
(HRS) (HRS) WEIGHT (Q) CHANGE (g) CHANGE (g)
WT CHANGE/ delta WT CHANGE/
TIME CHANGE delta TIME CHANGE
COMMENTS
05/1 8/88
OS/18/88
OS/ 1 8/88
05/18/88
05/18/88
05/18/88
05/18/88
05/19/88
05/19/88
05/19/88
05/19/88
05/19/88
05/20/88
05/21/88
05/22/88
05/23/68
05/24/88
05/25/88
05/26/88
05/27/88
06/01/88
0.0
1.0
2.0
3.0
4.1
51
6 1
220
23 1
240
255
266
504
750
102.8
126.0
147.2
147.3
169.4
185.3
212.3
0
1
1
1
1
1
1
16
1
1
2
1
24
25
28
23
21
0
22
16
27
4289.8
4281.0
4276.4
42720
4267.9
42640
4263.2
4261.4
4261 0
42603
4259.5
42589
4256.2
4252.5
4252.9
4250.8
42493
4247.3
4245.4
4243.8
4239.8
0
88
4.6
4.4
41
39
08
1.8
04
0.7
08
0.6
2.7
3.7
-0.4
2.1
1.5
20
19
1.6
4.0
0
00
4.2
02
03
02
3.1
1.0
1.4
0.3
0.1
0.2
-2.1
1.0
4.1
-2.5
0.6
0.5
0.1
0.3
2.4
0
8.8
4.8
4.4
3.7
3.9
0.8
01
0.4
08
0.5
0.5
0.1
0.2
0.0
0.1
0.1
12.0
0.1
0.1
01
0
0.0
4.3
0.2
0.3
02
3.1
-0.1
1.4
-0.3
-0.1
02
-0.1
0.0
0.1
-0.1
0.0
-3.0
0.0
0.0
0.1
BF.SATURATED TF:1 SPOT ON EDGE
BF:SATURATED TF:1 SPOT ON EDGE
BF:SATURATED TF:1 SPOT ON EDGE
BF:SATURATED TF.DRY
BF:1 SPOT ON EDGE 4 2 CENTER TF:DAMP
BF:UNIFORM WETNESS TF:DAMP
BF:3 SPOTS TF.DAMP
BF2 SPOTS NEAR EDGE TF:1 SPOT ON EDGE
BF:DAMP TF:1 SPOT ON EDGE
BF4TF:NOSPOTS
BF.UNIFORM WETNESS TF:VEHY WET
BF.UNIFORM WETNESS TF:WET
BF:UNIFORM WETNESS TF:NO SPOTS
BF.UNIFORM WETNESS TF:WET
TF 4 BF: WET FROM EVAP
TF: VERY WET BF:SLIGHTLY WET
TF 4 BF: WET FROM EVAP
TF.LG SPOT NEAR EDGE BF:DAMP
TF 4 BF: WET FROM EVAP
-------
PC DETERMINATIONS. FLOOR DRY & WATER (5-18-88)
RTI-G DEVICE DRY & CLEAN WT.: 3856.5 fl.
RTIG DRY SAMPLE WT: 170.1 g.
PRESSURE: SOpsi
B.3 Experimental Data
DATE
05/18/88
05/18/88
05/18/88
05/18/88
05/18/88
05/18/88
05/18/88
00
i
O> 05/19/88
05/19/88
05/19/88
05/19/88
05/20/88
05/21/88
05/22/88
05/23/88
05/24/88
05/25/88
05/26/68
05/27/88
06/01/88
TIME delta TIME
(MRS) (MRS)
00
1.0
2.0
3.0
4.1
5.1
6.1
22.0
23.0
23.9
25.5
50.7
74.6
102.7
125.8
147.2
147.3
169.5
185.4
212.4
0
1
1
1
1
1
1
16
1
1
2
25
24
28
23
21
0
22
16
27
RTI-G WEIGHT delta WEIGHT WT CHANGE/ dafta WT CHANGE/
WEIGHT (g) CHANGE (g) CHANGE (g) TIME CHANGE delta TIME CHANGE
4269.4
4256.9
4252.6
4251 .7
4251 .3
42448
4244.1
4242.6
4241 .8
4241.3
4240.6
4238.7
4236.7
4234.6
4232.6
4231.0
4229.3
4227.1
4225.7
4221.9
0
12.5
4.3
09
0.4
6.5
0.7
1.5
0.8
0.5
0.7
1.9
2.0
2.1
2.0
1.6
1.7
2.2
1.4
3.8
0
0.0
8.2
3.4
0.5
-6.1
5.8
-0.8
0.7
0.3
-0.2
-1.2
-0.1
-0.1
0.1
0.4
-0.1
-0.5
0.8
2.4
0
12.5
4.5
0.9
0.4
6.5
0.6
0.1
0.8
0.6
0.5
0.1
0.1
0.1
0.1
0.1
10.2
0.1
01
0.1
0
0.0
8.6
3.4
0.5
-6.1
5.4
-0.1
0.7
0.3
-0.1
0.0
0.0
0.0
0.0
0.0
-0.6
0.0
0.1
0.1
COMMENTS
BF:SATURATED TF:DRY
BF.1 LG SPOT TF.1 SPOT ON EDGE
BF:1 LG SPOT TF:1 SPOT ON EDGE
BF:SATURATED TF:MISSING
BF .SEVERAL SPOTS TF .VISIBLE WETNESS
ON EDGE
BF:UNIFORM WETNESS TFiDAMP
TF:1 SPOTS BF:DAMP
BF:1 SPOT TF:DAMP TO TOUCH
BF & TFDAMP TO TOUCH
BFATF:VERYWET
BF .UNIFORM WETNESS TF: WET
BF:UNIFORM WETNESS TF: WET
BF:SLIGHTLY WET TFVERY WET
TF: WET FROM EVAP. BF: MOIST &
PARTICLES ON FILTER
TF:WET BF:SLIGHTLY WET
TF: LG SPOT ON EDGE BF: MOIST FROM EVAP
TF:MOIST TO TOUCH BF:SLIGHTLY WET
TF & BF: WET FROM EVAP
-------
B.3 Experimental Data
SC AND PC DETERMINATIONS: SND-M & 5% ACETONE SOLUTIONS
DEVICE: WRI-1 (CELL, GRIDS, SCREENS. AND PISTON) WT: 3783.8 g
DRY SAMPLE WT: 217.4 g WET SAMPLE WT: 748.7 g
WATER REMOVED AFTER SATURATION CONCENTRATION: 254.6 g
WATER REMOVED AFTER SO MINUTES OF PRESSURE: 30.6 g
PRESSURE: 50 PSI
CO
DATE
06/27/88
06/27/88
06/27/88
06/27/88
06/27/88
06/27/88
06/27/88
06/27/88
06/27/88
06/28/88
06/28/88
06/28/88
06/29/88
06/29/88
06/30/88
06/30/88
07/01/88
07/01/88
07/05/88
07/05/88
TIME
(HRS)
0.0
1.0
1.2
2.2
2.3
3.3
3.4
4.4
4.6
23.4
24.6
49.5
49.6
73.6
73.8
97.8
98.0
193.9
194.1
delta TIME
(HRS)
0.0
1.0
0.2
1.0
0.2
0.9
0.2
1.0
0.2
18.8
1.3
24.8
0.2
24.0
0.2
24.0
0.2
95.9
0.2
-194.1
WRI-1 WEIGHT delta WEIGHT WT CHANGE/ delta WT CHANGE/
WEIGHT (g) CHANGE (g) CHANGE (g) TIME CHANGE delta TIME CHANGE
4251.1
4245.9
4241 .2
42367
4233.1
42302
4230.0
4227.5
4225.6
4223.4
4223.2
4222.7
4220.6
4220.4
4218.3
4218.1
4216.1
4215.8
4211.8
4211.5
0
5.2
4.7
4.5
3.6
2.9
0.2
2.5
1.9
2.2
0.2
0.5
2.1
0.2
2.1
0.2
2.0
0.3
4.0
0.3
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
0.0
0.0
0.0
0.0
0
5.2
28.2
4.5
21.6
3.1
1.2
2.5
11.4
0.1
0.2
0.0
12.6
0.0
12.6
0.0
12.0
0.0
24.0
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
0.0
0.0
0.0
0.0
0.0
COMMENTS
TF WET ON EDGE; BF SATURATED
BF SATURATED; TF WET ON EDGE
BF SATURATED; TF WET ON EDGE
BF SATURATED; TF DRY
BF WET; TF DRY
TF DRY; BF DRY
TF EDGE WET; BF UNIFORM WETNESS
BF 3/4 WET ; TF DRY
TF WET; BF DAMP FROM ENVIRONMENT
TF 4 BF NO RELEASE
TF WET AROUND EDGE
TF SPOTS ON EDGE
TF WET AROUND EDGE
TF4BF MOIST FROM ENVIRONMENT
TF4BF NO RELEASE
TF4BF MOIST FROM ENVIRONMENT
TF4BF NO RELEASE
TF4BF MOIST FROM ENVIRONMENT
TF4BF NO RELEASE
-------
B.3 Experimental Data
PC DETERMINATIONS. SAFE STEP & OIL (38 p«rcent liquid loading)
DEVICE: RTI-G (CELL, GRIDS, SCREENS, AND PISTON) WT: 3858.7 g
DRY SAMPLE WT: 444.4 g WET SAMPLE WT: 613.3 g
PRESSURE: 50 PS!
00
DATE
06/27/88
06/27/88
06/27/88
06/27/88
06/27/88
06/27/88
06/27/88
06/27/88
06/28/88
06/28/88
06/28/88
06/28/88
06/28/88
06/28/88
06/28/88
06/28/88
06/28/88
06/28788
06/29/88
06/29/88
06/29/88
06/29/88
06/29/88
06/29/88
06/29/88
TIME delta TIME
(HRS) (HRS)
0.0
1.0
2.0
2.2
3.2
3.3
4.3
4.5
23.2
23.4
24.5
24.6
25.7
25.8
26.8
27.0
28.0
28.2
44.1
44.2
45.2
45.4
46.4
466
47.9
0.0
1.0
1.0
0.2
1.0
0.2
1.0
0.2
18.7
0.2
1.1
0.2
1.0
0.2
1.0
0.2
1.0
0.2
15.9
0.2
1.0
0.2
1.0
0.2
1.4
RTIG WEIGHT delta WEIGHT WT CHANGE/ delta WT CHANGE/
WEIGHT (g) CHANGE (g) CHANGE (g) TIME CHANGE delta TIME CHANGE
4422.9
4415.2
4411.6
4410.1
4407.6
4406.9
4405.4
4404.7
4402.0
4401.7
4401.5
4401.2
4400.6
4400.4
4399.7
4399.2
4398.6
4398.3
4397.0
4396.8
4396.5
4396.4
4396.1
4395.9
4395.5
0
7.7
3.6
1.5
2.5
0.7
1.5
0.7
2.7
0.3
0.2
0.3
0.6
0.2
0.7
0.5
0.6
0.3
1.3
0.2
0.3
0.1
0.3
0.2
0.4
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
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0
7.7
3.6
9.0
2.5
4.2
1.5
4.2
0.1
1.8
0.2
1.8
0.6
1.2
0.7
2.5
0.6
1.8
0.1
1.2
0.3
0.6
0.3
1.2
0.3
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
0.0
0.0
0.0
0.0
0.0
0.0
0.0
00
0.0
COMMENTS
TF & BF SATURATED
TF & BF WET
TF & BF 1/2 WET
TF: HALF WET BF: EDGE WET & FEW
SPOTS IN CENTER
TF HALF WET & BF LESS WET THAN TF
TF 3/4 WET ; BF VERY WET
BF WET ON EDGE; TF DRY
BF: SPOTS ON EDGE AND 1 IN CENTER
TF: WET ON EDGE
TF 1 SPOT ON EDGE; BF 5 SPOTS
TF WET ON EDGE; BF EDGE & CENTER SPOTS
TF 2 SPOTS CENTER; BF SPOTS
TF & BF SPOTS OF WETNESS
TF & BF FEW SPOTS CENTER AND EDGE
TF A BF FEW SPOTS CENTER AND EDGE
TF WET ON EDGE; BF WET EXCEPT CENTER
TF NH; BF 5 SPOTS ON EDGE
TF & BF SLIGHT WETNESS ON EDGE
TF & BF NR
TF NR; BF 3 SPOTS NEAR EDGE
TF NR; BF SLIGHTLY WET AROUND EDGE
TF 1 SPOT; BF SMALL AERA ON EDGE
TF NR; BF SPOT ON EDGE
PC DETERMINATIONS. SAFE STEP & OIL (38 percent liquid loading)
-------
B.3 Experimental Data
PC DETERMINATIONS: SAFE STEP & OIL (38 percent liquid loading)
(continued)
DATE
06/29/88
06/29/88
06/29/88
06/29/88
06/29/88
06/30/88
06/30/88
06/30/88
ni
i 06/30/88
40 06/30/88
06/30/88
06/30/88
06/30/88
06/30/88
06/30/88
06/30/88
07/01/88
07/01/88
07/01/88
07/01/88
07/01/88
07/01/88
07/01/86
07/05/88
TIME (Mia TIME
(HRS) (HRS)
48.1
49.1
49.3
50.1
50.3
67.2
67.3
68.7
68.8
69.8
70.0
71.3
72.9
73.1
89.9
90.1
91.1
91.3
92.3
92.4
93.9
94.0
190.4
190.6
0.2
1.0
0.2
0.9
0.2
16.9
0.2
1.4
0.2
1.0
0.2
1.3
1.7
0.2
16.8
0.2
1.0
0.2
1.0
0.2
1.4
0.2
96.4
0.2
RTI-G WEIGHT delta WEIGHT WT CHANGE/ delta WT CHANGE/
WEIGHT (g) CHANGE (g) CHANGE (g) TIME CHANGE delta TIME CHANGE
4395.4
4395.0
4394.7
4394.4
4394.1
4393.1
4393.0
4392.8
4392.7
4392.3
4392.2
4392.0
4391.8
4391.6
4391.6
4391.0
4390.8
4390.7
4390.6
4390.6
4390.6
4390.4
4390.4
4388.9
0.1
0.4
0.3
0.3
0.3
1.0
0.1
0.2
0.1
0.4
0.1
0.2
0.2
0.2
0.0
0.6
0.2
0.1
0.1
0.0
0.0
0.2
0.0
1.5
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
0.0
0.0
0.0
0.0
0.0
0.0
0.0
00
0.6
0.4
1.8
0.3
1.8
0.1
0.6
0.1
0.6
0.4
0.6
0.2
0.1
1.2
0.0
3.6
0.2
0.6
0.1
0.0
0.0
1.2
0.0
9.0
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
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
COMMENTS
TF 1 SPOT NEAR CENTER; BF SPOT
TF STRIPS IN CENTER & EDGE SPOTS;
BF SPOT ON EDGE
TF SPOTS ON GRID MARKS; BF SPOTS ON ED
TF EDGE & SPOT ON GRIDS & BF EDGE WET
TF THREE SPOTS ON GRID; BF EDGE &
SPOTS ON GRIDS
TF NR; BF EDGES
TF NR; BF EDGES
TF NR; BF EDGES
BF1 SPOT ON EDGE
BF 4 SPOTS ON EDGE
BF FEW SPOTS ON GRID NEAR EDGE
BF FEW SPOTS ON EDGE
BF 1 SMALL SPOT ON EDGE
TF FEW SMALL SPECS; BF 1/8 WET FROM EDG
BF SPOTS ON EDGE
BF 1 SMALL SPOT
TF & BF NR
BF 1 SPOT NEAR EDGE
TF & BF NR
TF & BF NR
TF NR; BF DAMP ON EDGE
TF & BF NR
-------
B.3 Experimental Data
PC DETERMINATIONS: SND-M & 5% ACETONE SOLUTION
DEVICE: WRI-E (CELL, GRIDS, SCREENS. AND PISTON) WT. 3842.7 g
DRY SAMPLE WT: 228.6 g WET SAMPLE WT: 700.8 g
PRESSURE: SO PSI
DATE
07/18/88
07/18/88
07/18/88
07/18/88
07/18/88
07/18/88
07/18/88
07/18/88
07/18/88
• 07/10/88
O 07/10/88
07/18/88
07/10/88
07/20/88
07/20/88
07/21/88
07/21/88
07/22788
07/22/88
07/25/88
07/25/88
07/26/88
TIME dahaTIME
(MRS) (MRS)
0.0
1.0
1.2
2.2
2.4
3.8
40
5.2
5.4
21.2
21.4
22.4
22.5
46.3
46.5
71.2
71.4
04.1
04.2
164.4
164.6
180.0
0.0
1.0
0.2
1.0
0.2
1.5
0.2
1.2
0.2
15.8
0.2
1.0
0.2
23.8
0.2
24.7
0.2
22.7
0.2
70.2
0.2
24.4
WRI-E WEIGHT dalta WEIGHT WT CHANGE/ delta WT CHANGE/
WEIGHT (g) CHANGE (g) CHANGE (g) TIME CHANGE (Mta TIME CHANGE
4340.5
4334.8
4330.0
4325.1
4321.7
4317.8
4315.3
4313.2
4313.1
4310.1
4310.0
4309.4
4300.2
4306.1
4305.8
4303.2
4302.9
4300.8
4300.6
4206.0
4295.8
4203.3
0
5.7
4.8
49
3.4
3.9
2.5
2.1
0.1
3.0
0.1
0.6
0.2
3.1
0.3
2.6
0.3
2.1
0.2
4.6
0.2
2.5
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
0.0
0.0
0.0
0.0
0.0
0.0
0
5.7
28.8
4.7
20.4
2.7
15.0
1.7
0.6
0.2
0.6
0.6
1.2
0.1
1.8
0.1
1.8
0.1
1.2
0.1
1.2
0.1
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
0.0
0.0
0.0
0.0
0.0
0.0
COMMENTS
TF 1/4 WET; BF SATURATED
TF 1/4 WET; BF SATURATED
TF 1/4 WET; BF SATURATED
TF 1/8 WET; BF SATURATED
TF NR; BF SATURATED
BF 3/4 WET
BF 3/4 WET
TF & BF NR
TF MOIST FROM ENVIRONMENT; BF WET
TF & BF NR
TF & BF NR
TF & BF NR
TF & BF WET FROM ENVIRONMENT
TF & BF NR
TF & BF DAMP FROM ENVIRONMENT
TF 8. BF NR
TF ft BF DAMP FROM ENVIRONMENT
TF « BF NR
TF & BF DAMP FROM ENVIRONMENT
TF ft BF NR
TF ft BF DAMP FROM ENVIRONMENT
-------
B.3 Experimental Data
PC DETERMINATIONS: SAFE STEP & OIL (32 percent liquid loading)
DEVICE: RTI-000 (CELL, GRIDS. SCREENS. AND PISTON) WT: 3882.2 g
DRY SAMPLE WT: 439.2 g WET SAMPLE WT: 579.8 g
PRESSURE: 50 PSI
DATE
07/25/88
07/25/88
07/25/88
07/25/88
07/25/88
07/26/88
07/26/88
07/26/88
07/26/88
07/26/88
07/26/88
07/26/88
07/26/88
07/26/88
07/26/88
07/26/88
07/27/88
07/27/88
07/27/88
07/27/88
07/27/88
07/27/88
07/27/88
07/27/88
07/27/88
07/27/88
07/27/88
TIME delta TIME
(HRS) (HRS)
0.0
0.2
1.2
1.4
2.3
2.5
18.2
18.3
19.4
19.5
20.6
20.7
22.4
23.4
23.6
24.5
24.7
41.7
41.9
43.0
43.1
44.6
44.8
45.8
45.9
47.0
472
0.0
0.2
1.1
0.2
0.9
0.2
15.7
0.2
1.0
0.2
1.1
0.2
1.6
1.0
0.2
1.0
0.2
17.0
0.2
1.1
0.2
1.5
0.2
1.0
0.2
1.1
0.2
RTI-000 WEIGHT delta WEIGHT WT CHANGE/ delta WT CHANGE/
WEIGHT (g) CHANGE (g) CHANGE (g) TIME CHANGE delta TIME CHANGE
4459.5
4452.0
4448.2
4442.4
4438.8
4436.5
4432.6
4432.3
4431.0
4430.5
4429.3
4428.7
4427.0
4426.4
4426.1
4425.3
4425.2
4423.6
4423.3
4423.4
4423.3
4423.1
4422.9
4422.6
4422.3
4421.9
4421.8
0
7.5
3.8
5.8
3.6
2.3
3.9
0.3
1.3
0.5
1.2
0.6
1.7
0.6
0.3
0.8
0.1
1.6
0.3
-0.1
0.1
0.2
0.2
0.3
0.3
0.4
0.1
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
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0
45.0
3.6
34.8
4.0
13.8
0.2
1.8
1.3
3.0
1.1
3.6
1.0
0.6
1.8
0.8
0.5
0.1
1.8
-0.1
0.6
0.1
1.2
0.3
1.8
0.4
0.6
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
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
COMMENTS
TF ft BF SATURATED
TF ft BF SATURATED
TF ft BF WET
TF ft BF WET
TF ft BF WET
TF ft BF WET
TF ft BF WET ON GRIDS
TF ft BF WET ON GRIDS ft EDGES
TF ft BF WET ON GRIDS
TF ft BF WET ON GRIDS
TF ft BF WET ON GRIDS
TF ft BF WET ON GRIDS
TF ft BF WET ON GRIDS
TF ft BF WET ON EDGES AND GRIDS
TF ft BF WET ON EDGES AND GRIDS
TF ft BF WET ON EDGES AND GRIDS
TF ft BF 1/2 WET
TF SPOTS; BF SPOTS AND EDGES WET
BF ft TF FEW SPOTS
TF SPOT ; BF WET ON EDGE
TF NR; BF EDGE WET AND SPOTS ON GRIDS
TF ft BF SPOTS
BF & TF EDGES WET
BF SPOTS ON EDGE
-------
B.3 Experimental Data
PC DETERMINATIONS: SAFE STEP & OIL (32 parcant liquid loading)
(continued)
CO
1
K- >
to
DATE
07/28/86
07/28/88
07/28/88
07/28/88
07/28/88
07/28/88
07/28/88
07/28/88
07/28/88
07/28/88
07/29/88
07/29/88
07/29/88
07/29/88
08/01/88
08/01/88
TIME (MtaTIME
(MRS) (HRS)
48.2
63.7
63.9
65.8
66.0
68.0
682
69.6
69.8
70.7
86.6
86.8
88.2
88.4
112.1
112.2
1.0
15.5
0.2
1.9
0.2
2.0
0.2
1.4
0.2
0.9
15.9
0.2
1.5
0.2
23.6
0.2
RTI-000 WEIGHT delta WEIGHT WT CHANGE/ delta WT CHANGE/
WEIGHT (g) CHANGE (g) CHANGE (g) TIME CHANGE delta TIME CHANGE
4421.4
4420.4
4420.2
4420.0
4420.0
4419.7
4419.6
4419.2
4419.1
4419.0
4418.3
4418.1
4418.0
4418.0
4416.4
4416.4
0.4
1.0
0.2
0.2
0.0
0.3
0.1
0.4
0.1
0.1
0.7
0.2
0.1
0.0
1.6
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
0.0
0.4
0.1
1.2
0.1
0.0
0.1
0.6
0.3
0.6
0.1
0.0
1.2
0.1
0.0
0.1
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
0.0
COMMENTS
BF SPOTS ON EDGE
TF & BF WET ON EDGE AND
TF&BF 1-2 SPOTS
BF WET ON EDGE (1 SPOT)
BF WET ON EDGE (1 SPOT)
BF WET AROUND EDGE
BF WET AROUND EDGE
BF WET AROUND EDGE
TF A BF NR
TF 4 BF NR
TF & BF NR
GRIDS
TF & BF WET FROM ENVIRONMENT
TF & BF NR
-------
B.3 Experimental Data
DO
PC DETERMINATIONS: VERMICUUTE & CaSO4 SOLUTIONS (160 percent liquid loading)
DEVICE: WRI-1 (CELL, GRIDS. SCREENS. AND PISTON) WT: 3780.6 g
DRY SAMPLE WT: 64 3g WET SAMPLE WT: 167.3 g
PRESSURE: SO PSI
DATE
TIME delta TIME WRI-1 WEIGHT detta WEIGHT
WEIGHT (9) CHANGE (g) CHANGE (g)
WT CHANGE/ delta WT CHANGE/
TIME CHANGE delta TIME CHANGE
COMMENTS
07/26/88
07/26/88
07/26/86
07/26/88
07/27/88
07/27/88
07/28/88
07/28/88
07/29/88
07/29/88
0.0
1.1
1.3
2.3
26.4
26.6
52.2
52.4
77.0
77.1
0.0
1.1
0.2
1.0
24.2
0.2
25.6
0.2
24.6
0.2
3947.4
3944.0
3943.6
3942.8
3941.1
3941.0
3939.5
3938.7
3937.6
3937.3
0
3.4
0.4
0.8
1.7
0.1
1.5
0.8
1.1
0.3
0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0
3.1
2.4
0.8
0.1
0.6
0.1
4.8
0.0
1.8
0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
TF
&BF
SATURATED
TF WET AROUND EDGE; BF NR
TF
SPOTS ON EDGE
TF & BF WET FROM ENVIRONMENT
TF
TF
TF
TF
TF
&BF
&BF
&BF
4BF
&BF
NR
WET FROM ENVIRONMENT
NR
WET FROM ENVIRONMENT
NR
PC DETERMINATIONS: VERMICUUTE * CaS04 SOLUTION (160 percent liquid loading)
DEVICE: WRI-E (CELL. GRIDS. SCREENS, AND PISTON) WT:
DRY SAMPLE WT: 67.8 g WET SAMPLE WT:
PRESSURE:
DATE
06/01/88
08/01/88
08/01/88
08/01/88
08/01/88
06/01/68
08/02/88
08/03/88
08/04/88
08/06/88
08/08/88
SO PSI
TIME
(HRS)
0.0
1.0
1.2
2.7
3.7
3.9
27.9
51.9
77.0
100.7
113.5
(MtaTIME
(HRS)
0.0
1.0
0.2
1.5
1.1
0.2
24.0
24.0
25.1
23.7
12.8
176.4g
WRI-E
WEIGHT (g)
4020.1
4018.4
4018.2
4017.3
4016.7
4016.3
4014.8
4013.3
4010.9
4009.1
4007.2
3842.7 g
WEIGHT
CHANGE (g)
0
1.7
0.2
0.9
0.6
0.4
1.5
1.5
2.4
1.8
1.9
drta WEIGHT
CHANGE (g)
0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
WT CHANGE/
TIME CHANGE
0
1.7
1.2
0.6
0.6
2.4
0.1
0.1
0.1
0.1
0.1
data WT CHANGE/
delta TIME CHANGE
0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
COMMENTS
TFWET
BF
; BF DRY
&TFNR
BF4TF
TF4BF
TF
TF
TF
TF
TF
&BF
&BF
4BF
&BF
&BF
NR
NR
NR
DAMP FROM
DAMP FROM
DAMP FROM
DAMP FROM
ENVIRONMENT
ENVIRONMENT
ENVIRONMENT
ENVIRONMENT
-------
B.3 Experimental Data
PC DETERMINATIONS: SAFE STEP & OIL (32 p«c«nl liquid loading)
DEVICE: RTI-G (CELL, GRIDS, SCREENS. AND PISTON) WT: 38612 g
DRY SAMPLE WT. 439.5 g WET SAMPLE WT: 580.1 g
PRESSURE: 50 psi
DATE
07/26/88
07/26/88
07/26/88
07/26/88
07/26/88
07/26/88
07/27/88
OJ 07/27/88
J- 07/27/88
•* 07/27/88
07/27/88
07/27/88
07/27/88
07/27/88
07/27/88
07/27/88
07/27/88
07/28/88
07/28/88
07/28/88
07/28/86
07/28/88
07/28/88
07/28/88
07/28/88
07/28/88
07/28/88
TIME delta TIME
(HRS) (MRS)
0.0
0.2
1.2
1.3
2.1
2.3
18.1
18.3
10.3
19.5
20.5
20.7
22.4
23.4
23.5
24.9
25.1
42.1
42.3
43.3
43.4
44.9
45.0
46.0
46.2
47.2
47.4
0.0
0.2
1.0
0.2
0.8
0.2
15.8
0.2
1.0
0.2
1.1
0.2
1.7
1.0
0.2
1.4
0.2
17.0
0.2
1.0
0.2
1.5
0.2
1.0
0.2
1.0
0.2
RTI-G WEIGHT dalta WEIGHT WT CHANGE/ delta WT CHANGE/
WEIGHT (g) CHANGE (g) CHANGE (g) TIME CHANGE delta TIME CHANGE
4428.5
4423.2
4418.0
4415.4
4412.7
4411.7
4408.4
4408.3
4407.9
4407.6
4406.6
4406.4
4405.1
4404.3
4404.1
4403.3
4403.2
4401.5
4401.3
4401.3
4401.2
4400.7
4400.7
4400.4
4400.3
4399.8
4399.5
0
5.3
5.2
26
2.7
10
3.3
0.1
0.4
0.3
1.0
0.2
1.3
0.8
0.2
0.8
0.1
1.7
0.2
0.0
0.1
0.5
0.0
0.3
0.1
0.5
0.3
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
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
00
0.0
0.0
0
31.8
5.2
15.6
3.4
6.0
0.2
0.6
0.4
1.8
1.0
1.2
0.8
0.8
1.2
0.6
0.6
0.1
1.2
0.0
0.6
0.3
0.0
0.3
0.6
0.5
1.8
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
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
COMMENTS
TF ft BF SATURATED
TF ft BF SATURATED
TF & BF WET
TF ft BF WET
TF & BF WET
TF ft BF WET
TF ft BF WET ON GRIDS
TF & BF SPOTS ON GRIDS
TF ft BF WET ON GRIDS
TF A BF WET ON GRIDS
TF ft BF WET ON GRIDS
TF & BF WET ON GRIDS
TF 4 BF WET ON GRIDS
ft EDGES
TF ft BF WET ON EDGES AND GRIDS
TF & BF WET ON EDGES AND GRIDS
TF ft BF WET ON EDGES AND GRIDS
TF ft BF 1/2 WET
TF ft BF FEW SPOTS
TF NR; BF FEW SPOTS
BF FEW SPOTS
TF SPOT ; BF FEW SPOTS
TF NR; BF EDGE WET AND
BF WET ON EDGE
TF ft BF SPOTS
BF ft TF EDGES WET
BF SPOTS ON EDGE
SPOTS ON GRIDS
-------
B.3 Experimental Data
PC DETERMINATIONS. SAFE STEP & OIL (32 petceot liquid loading)
(continued)
DATE
07/28/88
07/28/88
07/29/88
07/29/88
07/29/88
07/29/88
08/01/88
08/01/88
CD
TIME data TIME
(MRS) (MRS)
48.4
63.9
64.1
66.0
66.1
90.1
113.8
114.0
1.0
15.5
0.2
1.9
0.2
24.0
23.7
0.2
RTI-G WEIGHT delta WEIGHT WT CHANGE/ delta WT CHANGE/
WEIGHT (g) CHANGE (g) CHANGE (g) TIME CHANGE delta TIME CHANGE
4399.1
4398.4
4398.3
4398.3
4398.1
4396.8
4395.4
4395.5
0.4
0.7
0.1
0.0
0.2
1.3
1.4
-0.1
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.4
0.0
0.6
0.0
1.2
0.1
0.1
-0.6
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
COMMENTS
BF SPOTS ON EDGE
TF & BF WET ON EDGE AND GRIDS
TF A BF NR
TF & BF NR
TF & BF NR
BF WET AROUND EDGE
TF AND BF WET FROM ENVIRONMENT
TF & BF NR
Ul
-------
PC DETERMINATIONS: FLOOR DRY 4 WATER
RTI-000 DEVICE DRY & CLEAN WT.: 3884.B g.
RTI-000 DRY SAMPLE WT: 174.8 j.
PRESSURE: 50 psi
B.3 Experimental Data
CD
•
i— «
0)
DATE
09/08/86
09/08/88
09/08/88
09/08/88
09/08/88
09/08/88
09/08/88
09/08/88
09/09/88
09/09/88
09/09/88
09/10/88
09/11/88
09/12/88
09/13/88
09/14/88
09/15/88
TIME delta TIME
(MRS) (MRS)
0.0
1.0
2.0
22
3.2
33
4.7
4.8
21.4
22.8
23.0
52.2
76.7
99.6
123.4
143.0
169.9
0
1
1
0
1
0
1
0
17
1
0
29
25
23
24
20
27
RTI-OOO WEIGHT delta WEIGHT WT CHANGE/ delta WT CHANGE/
WEIGHT (g) CHANGE (g) CHANGE (g) TIME CHANGE delta TIME CHANGE
4305.9
4296.3
4291.6
4290.3
42870
4286.7
4286.0
4285.7
4279.9
4278.9
4278.5
4276.1
4274.0
4271.3
4269.7
4267.7
4264.6
0
9.6
4.7
1.3
3.3
0.3
0.7
0.3
5.8
1.0
0.4
2.4
2.1
2.7
1.6
2.0
3.1
0
0.0
4.9
3.4
-2.0
3.0
0.4
0.4
5.5
4.8
0.6
-2.0
0.3
-0.6
1.1
-0.4
-1.1
0
9.6
4.7
7.8
3.3
1.8
0.5
1.8
0.4
0.7
2.4
0.1
0.1
0.1
0.1
0.1
0.1
0
0.0
4.9
20.4
-2.0
18.0
-0.3
2.4
-0.3
3.3
3.6
-0.1
0.0
0.0
0.0
0.0
0.0
COMMENTS
BF:SATURATED TF:1SPOT ON EDGE
BF:SATURATED TF: NR
BF:NR TF:NR
BF 1 SPOT
BF4TF:VERY WET
TF & BF NR
TF & BF NR
WET FROM ENVIRONMENT
DAMP FROM ENVIRON.
SLIGHTLY DAMP FROM ENVIRON.
DAMP FROM ENVIRON.
DAMP FROM ENVIRON.
DAMP FROM ENVIRON.
-------
PC DETERMINATIONS: FLOOR DRY AND WATER
RTI-G DEVICE DRY & CLEAN WT.: 3859.4 g.
RTI-G DRY SAMPLE WT: 182.7 g.
PRESSURE: 50 psi
B.3 Experimental Data
to
DATE
09/06/88
09/08/88
09/08/88
09/08/88
09/08/88
09/08/88
09/08/88
09/08/88
09/09/88
09/09/88
09/09/88
09/09/88
09/09/88
09/09/88
09/10/88
09/11/88
09/12/88
09/13/88
09/14/88
09/15/88
TIME delta TIME
(HRS) (HRS)
0.0
1.0
2.0
2.2
3.2
3.3
4.7
4.9
21.0
22.6
22.8
23.8
24.0
25.0
53.8
78.4
101.2
124.8
144.8
171.6
0
1
1
0
1
0
1
0
16
2
0
1
0
1
29
25
23
24
20
27
RTI-G WEIGHT delta WEIGHT WT CHANGE/ delta WT CHANGE/
WEIGHT (g) CHANGE (g) CHANGE (g) TIME CHANGE delta TIME CHANGE
4303.6
4286.6
4281.5
4279.8
4277.2
4276.9
4276.2
4275.4
4269.0
4268.3
4268.0
4267.5
4267.3
4266.8
4263.7
4259.0
4256.2
4254.4
4252.7
4249.9
0
17.0
5.1
1.7
2.6
0.3
0.7
0.8
6.4
0.7
0.3
0.5
0.2
0.5
3.1
4.7
2.8
1.8
1.7
2.8
0
0.0
11.9
3.4
-0.9
2.3
-0.4
-0.1
-5.6
5.7
0.4
-0.2
0.3
-0.3
-2.6
-1.6
1.9
1.0
0.1
-1.1
0
17.0
5.1
10.2
2.6
1.8
0.5
4.8
0.4
0.4
1.8
0.5
1.2
0.5
0.1
0.2
0.1
0.1
0.1
0.1
0
0.0
11.9
20.4
-0.9
13.8
-0.3
-0.6
-0.3
3.6
2.4
-0.2
1.8
-0.3
-0.1
-0.1
0.1
0.0
0.0
0.0
COMMENTS
TF:NR BF:SATURAATED
BF:3/4 WET. TF:SPOTS ON EDGE
BF: 1/2 WET
BF : WET ON EDGE
BF:WET ON EDGE
TF4BFVERYWET
BF WET AROUND EDGE. 1 SPOT
TF & BF NR
BF 1 SPOT
TF & BF NR
TF & BF NR
TF & BF WET FROM ENVIRONMENT
TF & BF DAMP FROM ENVIRONMENT
TF & BF DAMP FROM ENVIRONMENT
TF & BF DAMP FROM ENVIRONMENT
TF & BF DAMP FROM ENVIRONMENT
-------
APPENDIX C
LIQUID RELEASE TEST DEVICE CALIBRATION
C.1 Procedure Used To Calibrate LRT Devices
C.2 Calibration Results For ADM LRT Devices
C-l
-------
C.1 Procedure Used To Calibrate LRT Devices
Note: This procedure was developed by Dr. Roy Borden, North Carolina
State University, Department of Civil Engineering, who served as a
consultant to RTI on this project. The procedure was used to calibrate
the devices built by Associated Design and Manufacturing Company
(ADM), Alexandria, VA.
General Description
Each LRT device should be calibrated to apply 50 * 1 psl to the top of a
sample. The calibration should be performed using all of the Individual pieces
of the device (I.e., pressure application device, sample cell body, baseplate,
and piston), spacers set at the location where the top of the sample would be,
and a load cell placed directly under the spacers. Placement of the load cell
requires a test frame to hold the LRT device, providing a hole underneath such
that the spacers can be set Inside the sample cell at the appropriate height and
the load cell placed directly below the spacers (See Figure ).
Procedure
1. Connect the LRT sample cell to the test frame as shown In Figure 3.
2. Place a calibrated load cell directly beneath the spacers which are set
at the appropriate height within the sample cell, representative of the
sample thickness (e.g., 10 cm).
3. Place a 76 mm stainless-steel screen, then a 76 mm filter paper on top
of the spacers
4. Place the piston on top of the spacers, stainless-steel screen, and
filter paper In the LRT sample cell.
5. Attach the pressure application device to the sample cell and apply 50
psl pressure to the piston via the baseplate regulator and monitor the
load cell. The load cell calibration Is used to determine the load per
unit area actually being applied by the system. The pressure Is then
released, the baseplate regulator adjusted, and the pressure again
applied to the piston. This procedure should be repeated until the
desire pressure of 50 * 1 psl 1s obtained.
6. After the desired setting 1s obtained, release the pressure and reapply
the pressure three times to ensure consistent results. Record the
pressure gauge (located on top of the pressure application device and
denoted by 'A' 1n Figure 3) and load cell readings for each trial.
C-2
-------
Pressure Gauge
Pressure
Application
Device
IT. -ra-
Calibration
Test Frame
/Tiston \
Spacer I
Spacer
Sample Cell
tf^ ...J. Spacer
r
i H ' ••
Spacer
~K
M f ! 1
Load Cell
1!
I
Spacer
Electric
Leads
Equipment Set-up for LRT Device Calibration
C-3
-------
C.2 Calibration Results For ADM LRT Devices
Piston Gauge Settings (psi)
Device
A
B
c
D
E
F
G
RTI-000
September 1987
56
53
53
49
58
51
...
43
April/August 1988
51
...
56.5
...
53.2
...
51
46
March 1991
42.5
...
...
49.3
48.7
...
...
42.4
C-4
-------
APPENDIX D
LIQUID RELEASE TEST (LRT) RESULTS
D. 1 Results for Floor Dry/Water
D.2 Results for Safe-Step/Motor Oil
D.3 Results for Vermiculite/0.01 N Calcium Sulfate Solution
D.4 Results for SND-M/5% Acetone Solution
D.5 Results for SND-M/Diesel Fuel
D-l
-------
D. 1 Results For Floor Dry/Water
LRT TESTS :FLOOR DRY i WATER
PRESSURE: 50 PSI
DATE SAMPLE SORBENT/ % LLL TIME HEIGHT DEVICE TOP BOTTOM
NUMBER SORBATE (MIN) (CM) FILTER FILTER
COMMENTS
05/25/88
06/10/88
06/10/88
06/10/88
06/10/88
06/10/88
06/10/88
06/10/88
06/10/88
06/10/88
06/10/88
06/10/88
06/1 0/88
05/31/88
06/02/88
05/31/88
05/25/88
06/02/88
06/02/88
06/02/88
06/02/88
05/31/88
06/02/88
05/31/88
06/03/88
06/02/88
05/31/88
06/03/88
06/03/88
05/31/88
06/03/88
05/31/88
06/03/88
06/03/88
06/03/88
06/03/88
05/31/88
05/31/88
06/03/88
06/03/88
05/31/88
06/03/88
05/31/88
06/03/88
05/31/88
06/03/88
U2
U249
U237
U252
U219
U250
U248
U14
U27
U26
U28
U10
U15
U100
U163
U104
U1
U178
U176
U164
U168
U95
U179
U103
U152
U165
U241
U161
U158
U36
U159
U240
U154
U155
U162
U239
U245
U251
U147
U151
U243
U149
U99
U148
U244
U146
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
125
130
130
130
130
130
130
133
133
133
133
133
133
135
135
135
135
135
135
135
135
135
137
137
137
137
137
137
137
137
140
140
140
140
140
140
140
140
142
142
142
142
142
142
142
142
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
WRI-E
WRI-E
WRI-E
WRI-1
WRI-E
WRI-1
WRI-1
WRI-E
WRI-E
WRI-1
WRI-1
WRI-E
WRI-1
WRI-E
WRI-1
WRI-1
WRI-1
WRI-E
WRI-1
WRI-1
WRI-1
WRI-E
WRI-E
WRI-1
WRI-1
WRI-1
WRI-1
WRI-E
WRI-1
WRI-E
WRI-E
WRI-1
WRI-1
WRI-E
WRI-1
WRI-E
WRI-E
WRI-E
WRI-E
WRI-1
WRI-1
WRI-E
WRI-E
WRI-1
WRI-1
WRI-1
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR TF: RELEASE ON EDGE
NR
NR
NR
R BF: 1 DOT ON GRID MARK
NR
R
R BF: 2 DOTS
R
R
R BF: SATURATED
R
R
R BF: 1/2 SATURATED
R
R
R
R
R
R
R
R
R
R
R
R
R
R
R
R
D-2
-------
D. 1 Results For Floor Dry/Water
LRT TESTS: FLOOR DRY & WATER (continued)
PRESSURE: 50 PSI •
DATE
05/26/88
05/12/88
05/12/88
06/08/88
06/03/88
06/08/88
06/03/88
06/03/88
06/03/88
06/03/88
06/03/88
06/03/88
06/03/88
06/03/88
06/03/88
06/08/88
06/08/88
SAMPLE
NUMBER
U3
*U23
*U24
•U236
*U174
*U236
*U174
*U157
*U180
*U157
*U180
•U156
*U160
*U160
*U156
*U150
*U150
SORBENT/
SORBATE
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
% LLL TIME HEIGHT
(MIN) (CM)
145
105
105
135
135
135
135
137
137
137
137
140
140
140
140
142
142
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
DEVICE TOP
FILTER
WRI-1
RTI-000
RTI-G
WRI-1
WRI-E
WRI-E
WRI-1
WRI-1
WRI-1
WRI-E
WRI-E
WRI-1
WRI-E
WRI-1
WRI-E
WRI-E
WRI-1
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
BOTTOM
FILTER
R
NR
NR
NR
R
NR
R
R
NR
R
NR
NR
NR
NR
R
R
R
STANDING WATER
RELEASE ON GRID
RELEASE ON GRID
RELEASE ON GRID
FILLED FIRST
RELEASE ON GRID
FILLED FIRST
FILLED FIRST
COMMENTS
IN BOTTOM OF JAR
MARK
MARK; FILLED FIRST
MARK
MARK; FILLED FIRST
LOADED IN ONE BOTTLE AND SPLIT INTO TWO SAMPLES
D-3
-------
D.2 Results For Safe-Step/Motor Oil
LRT TESTS: SAFE STEP & OIL
PRESSURE: 50 PSI
DATE SAMPLE
NUMBER
05/31/88
05/16/88
05/31/88
06/03/88
06/03/88
06/03/88
06/03/88
05/31/88
06/03/88
06/03/88
05/31/88
05/31/88
06/03/88
06/03/88
06/03/88
06/03/88
06/06/88
06/06/88
06/06/88
05/31/88
06/06/88
05/31/88
06/06/88
05/31/88
05/31/88
06/06/88
06/06/88
06/06/88
05/31/88
06/06/88
06/06/88
05/31/88
05/26/88
05/26/88
05/26/88
05/1 7/88
05/26/88
05/26/88
06/13/88
06/13/88
05/25/88
06/13/88
06/13/88
06/13/88
V147
V10
V198
V193
V199
V115
V111
V141
V114
V195
V139
V134
V194
V110
V200
V112
V203
V113
V109
V146
V119
V140
V201
V133
V197
V160
V157
V162
V196
V161
V116
V135
V191
V14
V189
V13
V126
V15
V132
V129
V55
V187
V155
V10
SORBENT/ % LLL TIME HEIGHT
SORBATE (MIN) (CM)
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
20
20
20
20
20
20
20
20
20
22
22
22
22
22
22
22
25
25
25
25
25
25
25
25
28
28
28
28
28
28
28
28
30
30
30
30
30
30
32
32
32
32
32
32
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
DEVICE TOP BOTTOM COMMENTS
FILTER FILTER
WRI-E
RTI-000
WRI-1
WRI-1
WRI-E
WRI-E
WRI-1
WRI-1
WRI-1
WRI-E
WRI-E
WRI-1
WRI-E
WRI-1
WRI-E
WRI-1
WRI-E
WRI-1
WRI-1
WRI-E
WRI-E
WRI-1
WRI-1
WRI-1
WRI-E
WRI-1
WRI-E
WRI-E
WRI-E
WRI-1
WRI-E
WRI-1
WRI-E
WRI-1
WRI-1
RTI-G
WRI-E
WRI-E
WRI-E
WRI-1
WRI-E
WRI-1
WRI-1
WRI-E
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
NR
NR
NR
R
NR
NR
R
R
R
NR
R
R
R
R
R
NR
R
R
R
R
R
H
R
R
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
NR
R
R
R
R
R
R
TF:RELEASE DUE CONTACT WITH EDGE
MAINTAINENCE WORKING ON ROOM TEMP
TF:RELEASE DUE CONTACT WITH EDGE
TF:RELEASE DUE CONTACT WITH EDGE
TF:RELEASE DUE CONTACT WITH EDGE
TF:RELEASE DUE CONTACT WITH EDGE
TF: CONTACT WITH EDGE; RELEASE ON GRID
TF:RELEASE DUE CONTACT WITH EDGE
TF: CONTACT WITH EDGE; RELEASE ON GRID
TF:RELEASE DUE CONTACT WITH EDGE BF:2
TF: WET SPOT ON GRID MARK
TF: SLIGHTLY WET ON GRID MARK
TF: CONTACT WITH EDGE; RELEASE ON GRID
TF: WET SPOT ON GRID MARK
TF: CONTACT WITH EDGE; RELEASE ON GRID
SAMPLE ONLY SAT FOR 24 HRS (NOT 72 HRS)
OOZES AROUND PISTON
OOZES AROUND PISTON
OOZES AROUND PISTON
OOZES AROUND PISTON
OOZES AROUND PISTON
MARK
MARK
DOTS
MARK
MARK
D-4
-------
D.2 Results For Safe-Step/Motor Oil
LRT TESTS: SAFE STEP & OIL (continued)
PRESSURE: 50 PSI
DATE
06/13/88
05/25/88
06/13/88
06/13/88
05/16/88
06/13/88
06/07/88
06/07/88
06/07/88
06/07/88
06/13/88
06/13/88
06/08/88
06/08/88
06/08/88
06/08/88
06/13/88
06/06/88
06/13/88
06/06/88
06/06/88
06/06/88
06/09/88
06/1 0/88
06/09/88
06/09/88
06/10/88
06/09/88
06/09/88
06/09/88
05/26/88
05/26/88
05/26/88
05/27/88
05/26/88
05/27/88
06/13/88
06/13/88
06/13/88
06/13/88
SAMPLE
NUMBER
V4
V182
V185
V183
V11
V124
V118
V120
V120
V118
V177
V177
V117
V117
V138
V138
V180
V204
V180
V202
V202
V204
V154
V153
V154
V152
V153
V143
V152
V143
V125
V125
V53
V52
V53
V52
V156
V176
V156
V176
SORBENT/ % LLL TIME HEIGHT
SORBATE (MIN) (CM)
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
40
40
40
40
40
40
20
20
20
20
22
22
22
22
22
22
25
25
25
25
25
25
28
28
28
28
28
28
28
28
30
30
30
30
30
30
32
32
32
32
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
DEVICE TOP
FILTER
WRI-1
WRI-E
WRI-E
WRI-E
RTI-G
WRI-1
WRI-E
WRI-1
WRI-E
WRI-1
WRI-E
WRI-1
WRI-1
WRI-E
WRI-1
WRI-E
WRI-E
WRI-E
WRI-1
WRI-1
WRI-E
WRI-1
WRI-1
WRI-E
WRI-E
WRI-1
WRI-1
WRI-E
WRI-E
WRI-1
WRI-E
WRI-1
WRI-1
WRI-E
WRI-E
WRI-1
WRI-1
WRI-E
WRI-E
WRI-1
R
R
R
R
R
R
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
R
R
R
NR
R
R
NR
R
R
R
R
R
R
R
R
R
BOTTOM COMMENTS
FILTER
R
R
R
R
R
R
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
NR
R
R
NR
R
R
NR
R
R
R
R
R
R
R
R
R
OOZES AROUND PISTON; LIQUID
OOZES AROUND PISTON; LIQUID
OOZES AROUND PISTON; LIQUID
OUT BOTTOM
OUT BOTTOM
OUT BOTTOM
MAINTAINENCE WORKING ON ROOM TEMP
OOZES AROUND PISTON; LIQUID
SLIGHT POOLING ON BOTTOM
SLIGHT POOLING ON TOP
SLIGHT POOLING ON TOP
SLIGHT POOLING
SLIGHT POOLING ON TOP
NO POOLING;! SPOT ON EDGE
SLIGHT POOLING
OUT BOTTOM
POOLING ON TOP AND BOTTOM OF SAMPLE
OOZES AROUND PISTON
OOZES AROUND PISTON
OOZES AROUND PISTON
OOZES AROUND PISTON
D-5
-------
D.3 Results For Vermiculite/0.01 N Calcium Sulfate Solution
LHT TESTS: VEHMICUUTE & CaS04 SOLUTION
PRESSURE: 50 PSI
DATE
07/29/88
08/01/88
08/01/88
07/21/88
07/21/88
07/21/88
07/20/88
07/20/88
07/20/88
07/19/88
07/19/88
07/18/88
07/18/88
07/20/88
07/15/88
07/15/88
07/15/88
SAMPLE
NUMBER
W19
W20
W36
W25
W24
W32
W27
W26
W31
W30
W29
W74
W28
W73
EXTRA-10
EXTRA-12
EXTRA-11
SORBEN77 % ILL TIME HEIGHT
SORBATE (MIN) (CM)
VER/CaSO4
VER/CaS04
VER/CaSO4
VER/CaSO4
VER/CaS04
VER/CaS04
VER/CaS04
VER/CaSO4
VER/CaSO4
VER/CaSO4
VER/CaSO4
VER/CaSO4
VER/CaSO4
VER/CaSO4
VER/CaSO4
VER/CaSO4
VER/CaSO4
110
110
110
120
120
120
130
130
130
150
150
215
215
215
231
231
231
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
DEVICE
WRI-E
WRI-1
WRI-1
RTI-G
RTI-G
WRI-1
RTI-G
WRI-1
WRI-1
WRI-1
WRI-1
RTI-G
RTI-G
RTI-G
WRI-1
WRI-1
WRI-E
TOP
FILTER
NR
NR
NR
NR
NR
R
NR
R
R
R
R
R
R
R
R
R
R
BOTTOM
FILTER
NR
R
R
NR
R
R
NR
R
R
R
R
R
R
R
R
R
R
BF
BF
BF
BF
TF
TF
COMMENTS
SATURATED
SATURATED
SMALL SPOTS ON
&TF1/2WET
4 BF 1/2 WET
& BF 1/2 WET
EDGE
TF 3/4 SATURATED; BF SATURATED
TF
TF
TF
TF
TF
TF
TF
4 BF SATURATED
& BF SATURATED;
4 BF SATURATED;
& BF SATURATED
4 BF SATURATED
4 BF SATURATED
4 BF SATURATED
H2O ON PISTON
H2O ON PISTON
D-6
-------
D.4 Results For SND-M/5% Acetone Solution
LflT TESTS: SND-WACETONE SOLUTION
PRESSURE: 50 PSI
DATE
08/01/88
08/01/88
08/01/88
07/18/88
07/18/88
07/18/88
07/25/88
07/25/88
07/25/88
SAMPLE SORBENT/ % LLL TIME HEIGHT
NUMBER SORBATE (MIN) (CM)
Y17
Y18
Y14
Y6
Y7
Y8
Y13
Y12
Y5
OD/ACE
OD/ACE
OD/ACE
OD/ACE
OD/ACE
OD/ACE
OD/ACE
OD/ACE
OD/ACE
105
105
105
110.7
110.7
110.7
115
115
115
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
DEVICE
WRI-1
WRI-1
WRI-1
RTI-G
RTI-G
RTI-G
WRI-1
WRI-1
WRI-1
TOP
FILTER
NR
NR
NR
NR
NR
NR
NR
NR
NR
BOTTOM COMMENTS
FILTER
R
NR
NR
R
NR
NR
R
R
R
BF 1/8 WET
BF SATURATED
D-7
-------
D.5 Results For SND-M/Diesel Fuel
TEMPERATURE RUGGEDNESSTEST
S/S = SND-M/DIESEL FUEL
TEMPERATURE = 23 degrees cetoius
TEST DURATION = 10 minutes
PRESSURE= 50 psig
SAMPLE HEIGHT= 10 cm
SAMPLE
DATE
DEVICE
%LLL
TF
BF
Y67
Y64
Y69
Y65
Y132
Y133
Y62
Y61
Y126
Y121
Y119
Y131
Y138
Y130
Y118
Y122
Y120
Y137
Y136
Y140
Y135
Y142
Y134
Y123
Y124
Y125
Y129
Y147
Y127
Y144
Y9
Y141
11/4/88
11/4/88
11/4/88
11/4/88
10/25/88
10/25/88
11/4/88
11/4/88
10/28/88
1 0/28/88
10/28/88
1 0/25/88
1 0/27/88
1 0/25/88
10/31/88
10/31/88
1 0/28/88
10/27/88
10/27/88
10/27/88
10/25/88
10/27/88
10/25/88
10/31/88
1 0/28/88
1 0/28/88
10/28/88
10/27/88
10/28/88
1 0/27/88
1 0/28/88
1 0/27/88
RTI-000
RTI-G
RTI-G
RTI-000
RTI-000
RTIG
RTI-000
RTI-G
RTI-000
RTI-G
RTI-000
RTI-G
RTI-000
RTI-000
RTI-000
RTI-000
RTI-G
RTI-000
RTI-G
RTI-G
RTI-G
RTI-000
RTI-000
RTI-G
RTI-G
RTI-000
RT-G
RTI-000
RTI-G
RTI-G
RTI-000
RTI-G
70
70
70
70
70
70
70
70
75
75
75
75
75
75
77
77
77
77
77
77
80
80
80
80
80
80
83
83
83
83
83
83
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
NR
NR
NR
NR
R
NR
R
NR
NR
NR
NR
NR
R
R
R
R
NR
R
NR
R
NR
NR
D-8
-------
D.5 Results For SND-M/Diesel Fuel
TEMPERATURE RUGGEDNESS TEST
S/S » SND-M/DIESEL FUEL
TEMPERATURE = 23 degrees celcius (continued)
SAMPLE
DATE
DEVICE
%LLL
TF
BF
Y145
Y16
Y146
Y143
Y10
Y88
Y93
Y92
Y128
Y15
Y11
Y3
Y4
Y2
Y1
Y150
Y83
Y84
Y79
Y80
Y38
1 0/27/88
1 0/28/88
10/27/88
10/27/88
10/28/88
11/8/88
11/8/88
11/8/88
10/28/88
10/31/88
1 0/31/88
10/31/88
10/31/88
10/31/88
10/31/88
10/24/88
11/7/88
1 1/7/88
11/7/88
11/7/88
1 0/24/88
RTI-G
RTI-000
RTI-000
RTI-000
RT1-G
RTI-000
RTI-G
RTI-000
RTI-000
RTI-G
RTI-000
RTI-000
RTI-000
RTI-G
RTI-G
RTI-000
RTI-000
RTI-000
RTI-G
RTI-G
RTI-G
85
85
85
85
85
85
85
85
85
87
87
87
87
87
87
90
90
90
90
90
90
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
R
R
R
R
NR
R
R
R
R
R
R
R
R
R
R
D-9
-------
D.5 Results For SND-M/Diesel Fuel
TEMPERATURE RUGGEDNESS TEST
S/S = SND-M/DIESELFUEL
TEMPERATURE = 4 degrees celcius (COLD)
TEST DURATION. 10 minutes
PRESSURE= 50 psig
SAMPLE HEIGHT= 10 cm
SAMPLE
DATE
DEVICE
%LLL
TF
BF
Y36
Y108
Y34
Y35
Y107
Y29
Y106
Y25
Y30
Y23
Y24
Y105
Y101
Y100
Y33
Y52
Y98
Y53
Y99
Y54
Y94
Y45
Y46
Y113
Y117
Y112
Y48
Y42
Y90
Y89
Y47
Y85
Y41
Y115
Y114
Y116
10/31/88
1 1/7/88
10/31/88
10/31/88
11/7/88
10/31/88
11/7/88
10/31/88
10/31/88
10/31/88
10/31/88
11/7/88
11/7/88
11/7/88
10/31/88
' 10/31/88
11/7/88
10/31/88
11/7/88
10/31/88
1 1/7/88
10/31/88
10/31/88
1 0/27/88
10/31/88
10/31/88
10/31/88
10/31/88
11/7/88
11/7/88
10/31/88
11/7/88
10/31/88
1 1/7/88
11/7/88
1 0/27/88
RTI-G
RTI-OOO
RTI-000
RTI-G
RTI-000
RTI-G
RTI-000
RTI-G
RTI-000
RTI-000
RTI-G
RTI-G
RTI-G
RTI-000
RTI-000
RTI-000
RTI-000
RTI-G
RTI-G
RTI-000
RTI-G
RTI-000
RTI-000
RTI-G
RTI-000
RTI-G
RTI-G
RTI-G
RTI-G
RTI-OOO
RTI-G
RTI-OOO
RTI-OOO
RTI-G
RTI-OOO
RTI-OOO
75
75
75
75
77
77
77
77
77
80
80
80
80
80
80
83
83
83
83
33
83
85
85
85
85
85
85
87
87
87
87
87
87
90
90
90
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
NR
NR
NR
R
NR
R
NR
NR
NR
R
R
NR
R
R
R
R
R
R
R
R
R
R
D-10
-------
D-5 Results For SND-M/Diesel Fuel
TEMPERATURE RUGGEDNESS TEST
S/S-SND-WDIESELFUEL
TEMPERATURE = 40 degrees ceteius (HOT)
TEST DURATION = 10 minutes
PRESSURE=50psig
SAMPLE HEIGHT- 10 cm
SAMPLE
DATE
DEVICE
%LLL
TF
BF
Y55
Y59
Y56
Y63
Y58
Y60
Y28
Y72
Y68
Y71
Y31
Y32
Y111
Y27
Y22
Y109
Y57
Y26
Y19
Y103
Y110
Y21
Y104
Y20
Y51
Y50
Y97
Y102
Y66
Y49
Y40
Y44
Y91
11/4/88
11/4/88
11/4/88
11/4/88
11/4/88
11/4/88
11/1/88
11/4/88
11/4/88
11/4/88
11/1/88
11/1/88
11/4/88
11/1/88
11/1/88
11/4/88
11/4/88
11/1/88
11/1/88
11/4/88
1 1/7/88
1 1/1/88
11/7/88
11/1/88
1 1/1/88
11/2/88
11/7/88
11/7/88
1 1/7/88
11/2/88
11/2/88
11/2/88
11/7/88
RTI-G
RTI-G
RTI-000
RTI-000
RTI-000
RTI-G
RTI-G
RTI-G
RTI-G
RTI-000
RTI-000
RTI-000
RTI-000
RTI-G
RTI-G
RTI-G
RTI-000
RTI-000
RTI-000
RTI-000
RTI-000
RTI-000
RTI-G
RTI-G
RTI-G
RTI-000
RTI-000
RTI-000
RTI-G
RTI-000
RTI-G
RTI-G
RTI-G
70
70
70
70
70
70
75
75
75
75
75
75
77
77
77
77
77
77
80
80
80
80
80
80
83
83
83
83
83
83
85
85
85
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
NR
R
NR
R
NR
R
R
NR
R
NR
R
NR
R
R
R
R
R
R
R
R
R
D-ll
-------
D.5 Results For SND-M/Diesel Fuel
TEMPERATURE RUGGEDNESS TEST
S/S - SND-M/DIESEL FUEL
TEMPERATURE » 40 degrees celcius (continued)
SAMPLE DATE DEVICE %LLL TF BF
Y96
Y43
Y95
Y37
Y70
Y39
11/7/88
11/2/88
11/7/88
11/2/88
11/2/88
11/2/88
RTI-G
RTI-G
RTI-000
RTI-G
RTWOO
RTI-000
85
85
85
87
87
87
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
D-12
-------
METHOD 9095
PAINT FILTER LIQUIDS TEST
1.0 SCOPE AND APPLICATION
1.1 This method 1s used to determine the presence of free liquids 1n a
representative sample of waste.
1.2 The method 1s used to determine compliance with 40 CFR 264.314 and
265.314.
2.0 SUMMARY OF METHOD
2.1 A predetermined amount of material Is placed 1n a paint filter. If
any portion of the material passes through and drops from the filter within
the 5-m1n test period, the material Is deemed to contain free liquids.
3.0 INTERFERENCES
3.1 Filter media were observed to separate from the filter cone on
exposure to alkaline materials. This development causes no problem If the
sample 1s not disturbed.
4.0 APPARATUS AND MATERIALS
4.1 Conical paint filter; Mesh number 60 (fine meshed size). Available
at local paint stores such as Sherwin-Williams and GUdden for an approximate
cost of $0.07 each.
4.2 Glass funnel; If the paint filter, with the waste, cannot sustain
Us weight on the ring stand, then a fluted glass funnel or glass funnel with
a mouth large enough to allow at least 1 1n. of the filter mesh to protrude
should be used to support the filter. The funnel 1s to be fluted or have a
large open mouth 1n order to support the paint filter yet not Interfere with
the movement, to the graduated cylinder, of the liquid that passes through the
filter mesh.
4.3 Ring stand and ring, or tripod.
4.4 Graduated cylinder or beaker; 100-mL.
5.0 REAGENTS
5.1 None.
9095 - 1
Revision
Date September 1986
E-2
-------
oO
RING STAND
Figure 1. Paint filter test apparatus.
9095 - 3
E-4
Revision 0
Date September 1986
-------
METHOD 9O9S
PAINT FILTER LIQUIDS TEST
7. 1
Aeaemble te«t
apparatus
7.9
Place
f 1
•»«ple In
Iter
Allow
• •inple to drain
Into ar«du*ted
cylinder
Did *ny te»t
n«ter}«l collect
In graduated
cylinder?
Material
7.4
to contain free
llquldc; «e« <4O
CFR 264.314 or
263.314
f Stop J
E-5
Revision 0
Date September 1986
-------
APPENDIX F
1988 LIQUID RELEASE TEST (LRT)
COLLABORATIVE STUDY RESULTS
F.1 Results from Seven Laboratories Testing ADM Devices
F.2 Results from Three Laboratories Testing Other Devices
F-l
-------
F. 1 Results From Seven Laboratories Testing ADM Devices
LIQUID RELEASE TEST RESULTS
1988 COLLABORATIVE STUDY
LAB: CWM
LRT DEVICE: ADM
SORBENT/LIQUID
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
* FD: FLOOR DRY
H20: WATER
SS: SAFE-STEP
SAMPLE
NUMBER
Z115
Z127
Z138
Z225
Z233
Z247
Z38
Z44
Z50
Z210
Z213
Z223
Z163
Z169
Z176
277
Z83
Z76
V223
V228
V222
V218
V221
V219
V3
V287
V288
V237
V286
V240
V40
V46
V44
V42
V45
V48
DRY
SAMPLE
WEIGHT
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
WEIGHT
LIQUID ADDED
(grams)
215.4
215.4
215.4
215.4
215.4
215.4
264.8
264.8
264.8
264.8
264.8
264.8
270.8
270.8
270.8
270.8
270.8
270.8
89.1
89.1
89.1
89.1
89.1
89.1
126.0
126.0
126.0
126.0
126.0
126.0
148.5
148.5
148.5
148.5
148.5
148.5
LIQUID
LOADING
LEVEL
(%)
110
110
110
110
110
110
135
135
135
135
135
135
138
138
138
138
138
138
19.8
19.8
19.8
19.8
19.8
19.8
28
28
28
28
28
28
33
33
33
33
33
33
LIQUID
RELEASE
RESULTS
T
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
R
R
R
R
R
R
B
NR
NR
NR
NR
NR
NR
R
R
NR
R
NR
R
R
NR
NR
R
NR
R
NR
NR
NR
R
NR
NR
R
R
R
R
R
R
R
R
R
R
R
R
F-2
-------
F. 1 Results From Seven Laboratories Testing ADM Devices
LIQUID RELEASE TEST RESULTS
1988 COLLABORATIVE STUDY
LAB: GSX
LRT DEVICE: ADM
SORBENT/LIQUID
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
* FD: FLOOR DRY
H20: WATER
SS: SAFE-STEP
SAMPLE
NUMBER
Z135
Z129
Z246
Z130
Z229
Z140
Z202
Z212
Z45
Z48
Z46
Z41
Z152
Z146
Z157
Z145
Z180
Z174
V69
V254
V261
V255
V238
V236
V104
V215
V209
V242
V106
V97
V22
V24
V267
V19
V274
V270
DRY
SAMPLE
WEIGHT
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
WEIGHT
LIQUID ADDED
(grams)
215.4
215.4
215.4
215.4
215.4
215.4
264.8
264.8
264.8
264.8
264.8
264.8
270.8
270.8
270.8
270.8
270.8
270.8
89.1
89.1
89.1
89.1
89.1
89.1
126.0
126.0
126.0
126.0
126.0
126.0
148.5
148.5
148.5
148.5
148.5
148.5
LIQUID
LOADING
LEVEL
(%)
110
110
110
110
110
110
135
135
135
135
135
135
138
138
138
138
138
138
19.8
19.8
19.8
19.8
19.8
19.8
28
28
28
28
28
28
33
33
33
33
33
33
LIQUID
RELEASE
RESULTS
T
R
NR
NR
NR
NR
R
NR
NR
NR
NR
R
NR
NR
NR
NR
NR
NR
NR
R
R
NR
NR
NR
NR
R
R
NR
R
R
R
R
R
R
R
R
R
B
NR
NR
NR
NR
NR
NR
NR
NR
R
NR
NR
NR
R
R
NR
R
R
R
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
NR
R
R
R
R
R
R
F-3
-------
F. 1 Results From Seven Laboratories Testing ADM Devices
LIQUID RELEASE TEST RESULTS
1988 COLLABORATIVE STUDY
LAB:IEA
LRT DEVICE: ADM
SORBENT/LIQUID
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H20
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
* FD: FLOOR DRY
H20: WATER
SS: SAFE-STEP
SAMPLE
NUMBER
Z133
Z122
Z110
Z116
Z224
Z120
Z131
Z124
Z119
Z183
Z193
Z197
U288
U289
U285
U286
U278
U282
V28
V37
V256
V63
V39
V67
V169
V175
V60
V216
V179
V170
V248
V25
V244
V247
V271
V245
DRY
SAMPLE
WEIGHT
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
WEIGHT
LIQUID ADDED
(grams)
215.4
215.4
215.4
215.4
215.4
215.4
264.8
264.8
264.8
264.8
264.8
264.8
270.8
270.8
270.8
270.8
270.8
270.8
89.1
89.1
89.1
89.1
89.1
89.1
126.0
126.0
126.0
126.0
126.0
126.0
148.5
148.5
148.5
148.5
148.5
148.5
LIQUID
LOADING
LEVEL
(%)
110
110
110
110
110
110
135
135
135
135
135
135
138
138
138
138
138
138
19.8
19.8
19.8
19.8
19.8
19.8
28
28
28
28
28
28
33
33
33
33
33
33
LIQUID
RELEASE
RESULTS
T
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
R
R
R
R
R
R
B
NR
NR
NR
NR
NR
NR
NR
R
NR
R
R
R
NR
R
NR
R
NR
R
NR
NR
NR
NR
NR
NR
NR
R
NR
NR
NR
NR
R
R
R
R
R
R
F-4
-------
F. 1 Results From Seven Laboratories Testing ADM Devices
LIQUID RELEASE TEST RESULTS
1988 COLLABORATIVE STUDY
LAB: MICROBAC
LRT DEVICE: ADM
SORBEISTT/LIQUID
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
* FD: FLOOR DRY
H20: WATER
SS: SAFE-STEP
SAMPLE
NUMBER
Z121
Z144
Z243
Z237
Z123
Z125
Z209
Z204
Z40
Z42
Z47
Z198
Z154
Z148
Z159
. Z153
Z147
Z158
V62
V29
V72
V262
V253
V258
V284
V108
V282
V207
V213
V241
V100
V250
V99
V243
V25
V27
DRY
SAMPLE
WEIGHT
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
. 450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
WEIGHT
LIQUID ADDED
(grams)
215.4
215.4
215.4
215.4
215.4
215.4
264.8
264.8
264.8
264.8
264.8
264.8
270.8
270.8
270.8
270.8
270.8
270.8
89.1
89.1
89.1
89.1
89.1
89.1
126.0
126.0
126.0
126.0
126.0
126.0
148.5
148.5
148.5
148.5
148.5
148.5
LIQUID
LOADING
LEVEL
(%)
110
110
110
110
110
110
135
135
135
135
135
135
138
138
138
138
138
138
19.8
19.8
19.8
19.8
19.8
19.8
28
28
28
28
28
28
33
33
33
33
33
33
LIQUID
RELEASE
RESULTS
T
R
NR
NR
NR
NR
NR
NR
NR
R
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
NR
NR
R
R
R
R
R
R
R
B
NR
NR
NR
NR
NR
NR
R
NR
R
NR
NR
NR
R
NR
R
NR
NR
R
NR
NR
NR
NR
NR
NR
R
R
R
R
NR
R
R
R
R
R
R
R
F-5
-------
F. 1 Results From Seven Laboratories Testing ADM Devices
LIQUID RELEASE TEST RESULTS
1988 COLLABORATIVE STUDY
LAB: WILSON
LRT DEVICE: ADM
SORBENT/LIQUID
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H20
FD/H2O
FD/H20
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
* FD: FLOOR DRY
H20: WATER
SS: SAFE-STEP
SAMPLE
NUMBER
Z128
Z111
Z238
Z118
2230
Z231
Z203
Z208
Z200
Z196
Z51
Z54
Z156
Z150
Z161
Z155
Z149
Z160
V34
V264
V35
V66
V259
V64
V214
V211
V281
V103
V206
V210
V17
V21
V23
V275
V265
V272
DRY
SAMPLE
WEIGHT
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
WEIGHT
LIQUID ADDED
(grams)
215.4
215.4
215.4
215.4
215.4
215.4
264.8
264.8
264.8
264.8
264.8
264.8
270.8
270.8
270.8
270.8
270.8
270.8
89.1
89.1
89.1
89.1
89.1
89.1
126.0
126.0
126.0
126.0
126.0
126.0
148.5
148.5
148.5
148.5
148.5
148.5
LIQUID
LOADING
LEVEL
(%)
110
110
110
110
110
110
135
135
135
135
135
135
138
138
138
138
138
138
19.8
19.8
19.8
19.8
19.8
19.8
28
28
28
28
28
28
33
33
33
33
33
33
LIQUID
RELEASE
RESULTS
T
NR
NR
R
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
R
R
R
R
R
R
B
NR
NR
R
NR
NR
NR
NR
R
R
NR
NR
R
NR
NR
R
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
F-6
-------
F. 1 Results From Seven Laboratories Testing ADM Devices
LIQUID RELEASE TEST RESULTS
1988 COLLABORATIVE STUDY
LAB: WRI
LRT DEVICE: ADM
SORBENT/LIQUID
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H20
FD/H2O
FD/H20
FD/H20
FD/H20
FD/H20
FD/H20
FD/H20
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
* FD: FLOOR DRY
H20: WATER
SS: SAFE-STEP
SAMPLE
NUMBER
Z219
Z218
Z227
Z234
Z248
Z242
2244
Z105
Z102
Z108
Z101
Z194
Z85
Z86
Z79
Z73
Z88
Z186
V75
V81
V74
V79
V77
V83
V59
V172
V58
V178
V174
V171
V85
V86
V88
V92
V93
V95
DRY
SAMPLE
WEIGHT
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
WEIGHT
LIQUID ADDED
(grams)
215.4
215.4
215.4
215.4
215.4
215.4
264.8
264.8
264.8
264.8
264.8
264.8
270.8
270.8
270.8
270.8
270.8
270.8
89.1
89.1
89.1
89.1
89.1
89.1
126.0
126.0
126.0
126.0
126.0
126.0
148.5
148.5
148.5
148.5
148.5
148.5
LIQUID
LOADING
LEVEL
(%)
110
110
110
110
110
110
135
135
135
135
135
135
138
138
138
138
138
138
19.8
19.8
19.8
19.8
19.8
19.8
28
28
28
28
28
28
33
33
33
33
33
33
LIQUID
RELEASE
RESULTS
T
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
NR
NR
NR
NR
NR
R
R
R
R
R
R
R
R
R
R
R
R
B
NR
NR
NR
NR
NR
NR
R
NR
NR
NR
R
R
R
R
R
NR
R
R
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
F-7
-------
F. 1 Results From Seven Laboratories Testing ADM Devices
LIQUID RELEASE TEST RESULTS
1988 COLLABORATIVE STUDY
LAB: RTI
LRT DEVICE: ADM
SORBENT/LIQUID
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
* FD: FLOOR DRY
H20: WATER
SS: SAFE-STEP
SAMPLE
NUMBER
Z136
Z250
Z249
Z236
Z235
Z232
Z109
Z259
Z188
Z43
Z192
Z53
U268
U279
U274
U275
U265
U270
V38
V33
V36
V30
V32
V31
V173
V
V
V
V
V
V251
V269
V18
V249
V252
V246
DRY
SAMPLE
WEIGHT
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
WEIGHT
LIQUID ADDED
(grams)
215.4
215.4
215.4
215.4
215.4
215.4
264.8
264.8
264.8
264.8
264.8
264.8
270.8
270.8
270.8
270.8
270.8
270.8
89.1
89.1
89.1
89.1
89.1
89.1
126.0
148.5
148.5
148.5
148.5
148.5
148.5
LIQUID
LOADING
LEVEL
(%)
110
110
110
110
110
110
135
135
135
135
135
135
138
138
138
138
138
138
19.8
19.8
19.8
19.8
19.8
19.8
28.0
33.0
33.0
33.0
33.0
33.0
33.0
LIQUID
RELEASE
RESULTS
T
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
R
B
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
R
R
R
R
R
R
NR
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
F-8
-------
F.2 Results From Three Laboratories Testing Other Devices
LIQUID RELEASE TEST RESULTS
1988 COLLABORATIVE STUDY
LAB: CWM
LRT DEVICE: THEIR OWN DEVICE
SORBENT/LIQUID
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H20
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H20
FD/H2O
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
' FD: FLOOR DRY
H20: WATER
SS: SAFE-STEP
SAMPLE
NUMBER
Z142
Z143
Z226
Z228
Z239
2240
Z217
Z221
Z199
Z95
Z96
Z107
Z166
Z177
Z171
Z165
Z175
Z164
V220
V224
V217
V226
V227
V225
V43
V41
V47
V49
V50
V51
DRY
SAMPLE
WEIGHT
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
WEIGHT
LIQUID ADDED
(grams)
215.4
215.4
215.4
215.4
215.4
215.4
264.8
264.8
264.8
264.8
264.8
264.8
270.8
270.8
270.8
270.8
270.8
270.8
89.1
89.1
89.1
89.1
89.1
89.1
148.5
148.5
148.5
148.5
148.5
148.5
LIQUID
LOADING
LEVEL
(%)
110
110
110
110
110
110
135
135
135
135
135
135
138
138
138
138
138
138
19.8
19.8
19.8
19.8
19.8
19.8
33
33
33
33
33
33
LIQUID
RELEASE
RESULTS
T
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
R
R
R
NR
NR
NR
R
R
R
R
R
B
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
R
R
R
NR
NR
R
R
R
R
R
R
F-9
-------
F.2 Results From Three Laboratories Testing Other Devices
LIQUID RELEASE TEST RESULTS
1988 COLLABORATIVE STUDY
LAB: WRI
LRT DEVICE MILUPORE
SORBENT/LIQUID
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
' FD: FLOOR DRY
H20: WATER
SS: SAFE-STEP
SAMPLE
NUMBER
Z134
Z141
Z132
Z137
Z223
Z126
Z205
Z89
Z78
Z84
Z37
Z190
Z82
Z75
Z81
Z87
Z74
Z80
V73
V78
V76
V82
V84
V80
V71
V87
V90
V91
V94
V96
DRY
SAMPLE
WEIGHT
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
WEIGHT
LIQUID ADDED
(grams)
215.4
215.4
215.4
215.4
215.4
215.4
264.8
264.8
264.8
264.8
264.8
264.8
270.8
270.8
270.8
270.8
270.8
270.8
89.1
89.1
89.1
89.1
89.1
89.1
148.5
148.5
148.5
148.5
148.5
143.5
LIQUID
LOADING
LEVEL
(%)
110
110
110
110
110
110
135
135
135
135
135
135
138
138
138
138
138
138
19.8
19.8
19.8
19.8
19.8
19.8
33
33
33
33
33
33
LIQUID
RELEASE
RESULTS
T
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
B
NR
NR
NR
NR
NR
NR
R
R
R
R
NR
R
R
R
R
R
R
R
NR
NR
NR
NR
NR
NR
R
R
R
R
R
R
F-10
-------
F.2 Results From Three Laboratories Testing Other Devices
LIQUID RELEASE TEST RESULTS
1988 COLLABORATIVE STUDY
LAB: ANALYTICAL TESTING & CONSULTING
LRT DEVICE: THEIR OWN DEVICE
SORBENT/LIQUID
FD/H2O
FD/H20
FD/H20
FD/H2O
FD/H20
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H20
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
FD/H2O
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
SS/OIL
* FD: FLOOR DRY
H20: WATER
SS: SAFE-STEP
SAMPLE
NUMBER
Z139
Z117
Z241
Z245
Z112
Z114
Z220
Z112
Z216
Z52
Z185
Z191
Z103
Z93
Z97
Z90
Z91
Z104
Z98
Z92
Z106
Z99
Z100
Z94
Z168
Z179
Z173
Z167
Z178
Z172
V263
V257
V260
V68
V61
V65
V268
V266
V276
V16
V20
V273
DRY
SAMPLE
WEIGHT
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
200.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
450.0
WEIGHT
LIQUID ADDED
(grams)
215.4
215.4
215.4
215.4
215.4
215.4
264.8
264.8
264.8
264.8
264.8
264.8
215.4
215.4
215.4
215.4
215.4
215.4
215.4
264.8
264.8
264.8
264.8
264.8
270.8
270.8
270.8
270.8
270.8
270.8
89.1
89.1
89.1
89.1
89.1
89.1
89.1
148.5
148.5
148.5
148.5
148.5
LIQUID
LOADING
LEVEL
110
110
110
110
110
110
135
135
135
135
135
135
110
110
110
110
110
110
135
135
135
135
135
135
138
138
138
138
138
138
19.8
19.8
19.8
19.8
19.8
19.8
33
33
33
33
33
33
LIQUID
RELEASE
RESULTS
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
R R
R R
LEAKED
CRACKED
R R
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR R
NR R
NR R
NR R
R R
NR R
R R
NR R
NR R
R R
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
R R
R R
R R
R R
R R
R R
F-ll
------- |