-------
-------
TECHNICAL REPORT DATA
(Pl\xtt tttd Inttnifixiit on tit rcttnr
. REPORT NO.
EPA/600/A-86/01S
a.
4. TITLE ANDSUBTITL6
EPA Method Study 33: Ignitabllity Characteristics
of Solids ,
». REPORT OATS
February 1986
1. PlflPORMINO ORGANIZATION CODE
7. AUTHOR1SI .
Handy, R.W.; Michael, L.C., Mclaughlin, C.E.
and Pellizzari. E.D.
I. PIRFORMINO ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Research Triangle Institute
P.O. Box 12194
Research Triangle Park, NC 27709
10. PROGRAM ELEMENT NO.
BSD1A
It. CONTRACT/GRANT NO.
68-03-3099
12. SPONSORING AGENCY NAME AND ADDRESS
Environmental Monitoring and Support Laboratory
Office of Research and Development
U.S..Environmental Protection Agency
Cincinnati, OH 45268
13. TYPE OF REPORT AND PERIOD COVERED
14. SPONSORING AGENCY CODE
EPA600/6
15. SUPPLEMENTARY NOTES
16. ABSTRACT
The objective of this research was to conduct an interlaboratory study to
estimate the precision of three 1gnitab1l1ty test methods for solid wastes:
radiant heat ignition, flame propagation and water extinguishabilfty. The study
consisted of two phases. The first phase involved the replicate measurements of
two well characterized test materials and a reference material by nine laboratories.
The second phase included similar replicate measurements of seven varied test
materials by up to five laboratories.
The study results indicated that not all sample types are amenable to
measurement by each test. Although all of the procedures showed some deficiency,
the test results indicated that, with some changes 1n test chamber design they are
potentially useful as routine methods.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS C. COSATI Field/Croup
18. DISTRIBUTION STATEMENT
Release to public
EPA Farm 2220-1 (R.». 4-77) *HC»IOU1 EDITION IS OBlOLtTC
19. SECURITY CLASS (This Report!
21. NO. OF PAGES
Unclassified
20. SECURITY
22. PRICE
-------
-------
FOREWORD
Environmental measurements are required to determine the quality of
ambient waters and the character of wastes and waste effluents. The
Environmental Monitoring and Support Laboratory - Cincinnati (EMSL-C1nc1nnat1)
conducts research to:
Develop and evaluate techniques to measure the presence and
concentration of physical, chemical, and radiological pollutants 1n
water, wastewater, bottom sediments, and solid wastes.
Investigate methods for the concentration, recovery, and
Identification of viruses, bacteria, and other microorganisms 1n
water.
Provide for an Agency-wide quality assurance program to assure
standardization and quality control of systems for monitoring water
and wastewater.
This publication of the EMSL-Clnclnnatl, entitled: "USEPA Method Study
33. Ign1tab1l1ty Characteristics of Solids" reports the results of a study of
three separate 1gn1tab111ty parameters; radiant heat Ignition, flame
propagation, and water ext1ngu1shab1!1ty. Federal agencies, states,
municipal Hies, universities, private laboratories, and Industry should find
this evaluative study helpful 1n their efforts to establish 1gn1tab111ty
criteria for solid and hazardous wastes.
Robert L. Booth
Director, EMSL-C1nc1nnat1
ill
-------
ABSTRACT ;;; ,,-v,.
The objective of this research was to'conduct an Inter!aboratory study to
estimate the precision of three 1gn1tab111ty test methods for solid wastes:
radiant heat Ignition, flame propagation and water ext1ngu1shab1Hty. The
study consisted of two phases. The first phase Involved the replicate
measurements of two well characterized test materials and a reference material
by nine laboratories. The second phase Included similar replicate
measurements of seven varied test materials by up to five laboratories.
The study results Indicated that not all sample,types are amenable to
measurement by each test. Although all of the procedures showed some
deficiency, the test results Indicated that, with some changes 1n test
chamber design they are potentially useful as routine methods.
iv
-------
Contents
Section ,ti; Page
u av. i aimer. .««,,««..,,«,..,,»»,,».,««»«»,,««,»««...,., 11
Foreword [[[ ill
Hus tract ««»«««»»,«,«,,,,.,,,,.,,,.,,,,,,,,«,,,,««.«««,«.... lv
I aU I cS ««««.«»«,,
1. INTRODUCTION .............................. '. ..................... 1
2. SUMMARY [[[ 2
3. RECOMMENDATIONS ................................................. 4
4. DESCRIPTION OF STUDY ....................................... ..... S
Test Design ...................... ....... ................... 5
Methodology ........... ................. ,... ...... . ........ S
Participating Laboratories ................................. S
Phase 1 [[[ 6
Selection and Preparation of Wastes ........................ 6
S. TREATMENT OF DATA ............................................... 8
6. DISCUSSION AND CONCLUSIONS ............................ . ......... 10
Phase I Results ........................ . ................... 10
Outliers [[[ 17
Phase II Results ........................................... 17
Statistical Summary and Precision Statement ................ 17
Evaluation of Methods ............... . ...................... 17
-------
TABLES
Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
!5
16
17
18
19
20
21
22
r. »««*«<
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
Phase
i i
Phase II - Statistical Summary
Physical Description of Test.Materials
Phase I Results - Radiant Heat Ignition Test.
I Results - Flame Propagation Test
I Results - Water Ext1ngu1shab1l1ty Test
II Results - Radiant Heat Ignition Test
Heat
Heat
»*««>«««>«
Test Material
Test Material
Test Material
Test Material
Test Material
No.
II Results - Radiant Heat Ignition Test
II Results - Radiant Heat Ignition Test
II Results - Radiant Heat Ignition Test
II Results - Radiant Heat Ignition Test
II Results Flame Propagation Test - Test Material
II Results - Flame Propagation Test - Test Material
II Results - Flame Propagation Test - Test
II Results - Flame Propagation Test
II Results - Flame Propagation Test
II Results - Water Ext1ngu1shab1l1ty Test
II Results - Water Ext1ngu1shab1Hty Test
II Results - Water Ext1ngu1shab1l1ty Test
II Results - Water Ext1ngu1shab1l1ty Test
II Results - Water Ext1ngu1shab1l1ty Test
II Results - Water Ext1ngu1shab1l1ty Test
II Results - Water Ext1ngu1shab1Hty Test
Material
- Test Material
- Test Material
Test
Test
Test
Test
Test
Test
Test
No.
No.
No.
No.
Material
Material
Material
Material
Material
Material
Material
No.
No.
No.
No.
No.
3..
4..
5.,
8..
9..
5,
6,
7,
8,
9,
No.
No.
No.
No.
No.
No.
No.
Page
3
7
11
13
15
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
vi
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SECTION 1
INTRODUCTION
The United States Environmental Protection Agency (USEPA) has specified 1n
the Federal Register (1) that a solid waste .exhibits the characteristic of
1gn1tablllty if "it 1s capable of causing'fire through friction, absorption of
moisture or spontaneous chemical changes and, when Ignited, burns so
vigorously and persistently that 1t creates a hafard." At the present time,
there are no suitable, validated procedures for determining the 1gn1tab1l1ty
characteristics of solid (non-11qu1d) wastes.
The objective of this Interlaboratory study was to assess precision and
potential of application of three 1gn1tab1l1ty tests; radiant heat Ignition,
flame propagation, and water extlngulshabHlty. This report contains a
description of this study, an assessment of the three tests of 1gn1tab1l1ty
characteristics and recommendations for further development of the methods.
-------
SECTION 2
SUMMARY
This evaluation, the first for evaluation of potential testing methods for
sol Ids, was performed at the Research Triangle Institute (RTI) (2).
Techniques for 1gn1tab1Hty measurements were developed and tested on a
variety of waste materials. Three 1gn1tab1l1ty characteristics, radiant heat
ignition time, flame propagation rate and water ext1ngu1shab1!1ty were tested
on seven waste materials by three to five laboratories. Measured values for
each test were statistically analyzed. The overall means, precisions and
percent relative standard deviations for all waste types are shown 1n Table 1.
Based on the data acquired, the following conclusions were made.
Major problems with equipment and procedural details were discovered
in this collaborative effort. These deficiencies must be corrected
before the methods can be collaboratlvely tested or recommended for
use as standard procedures.
Two of the largest sources of error arise from the recording methods
used and lack of precise, beginning and end points of the tests.
The three methods tested are potentially useful for evaluating the
ignitability hazards posed by solid wastes, however, considerable
standardization and automation of the test procedures will be
required.
Exposure of some waste types (cotton fiber, polyurethane foam) to a
radiant heat source Is not sufficient to Ignite the samples.
The flame propagation and water extlngulshablHty tests could not be
performed on petroleum-based wastes, as the wastes were not readily
ignitable by a flame as specified 1n the method.
-------
TABLE 1. Phase II Statistical Summary
CJ
Radiant Heat
Test Material
No.
No.
No.
No.
No.
No*
No.
3 Cotton Fiber
Day 1
Day 2
4 Polyurethane Foam
Day 1
Day 2
5 Paint Waste
Day 1
Day 2
6 Waste 011
Day 1
Day 2
7 Waste 011 /Sand
Day 1
Day 2
8 Waste Solvent
Day 1
Day 2
9 Sawdust/Kerosene
Day 1
Day 2
X (Sec)
ND
ND
ND
ND
98(n=5)
104(n=-4)
119(n=4)
151(n»4)
151(n»4)
127(n=4)
49(n-4)
16(n-5)
14(n=4)
Sr
52
25
17
23
39
6
,.>-;;
'*T6
6
3
Ignition
S
56
63
38
152
68
63
23
9
6
3
%RSD
58
60
32-
101
45
50
.
38
19
35
24
Flame Propagation
S (cm/sec) Sr S %RSD
4.3 (n=3) 1.4 2.3 53.8
2.6 (n»l) * * *
0.3 (n-3) 0.05 0.07 21.4
0.3 (n-1) * * *
0.04(n-4) 0.1 0.01 28.8
0.03(n»2) 0.005 0.004 13.6
ND
ND
ND
ND
0.1 (n-3) 0.1 0.1 100.0
0.1 (n-1) * * : *
OJl(n»4) 0.04 0.11 104.3
0.20(n»2) 0.03 0.02 12.3
Water Ext1ngu1shab1lity
2 (mL)
4.3(n=4)
2.4(n»3)
33.3(n-3)
4.0(n»2)
2.3(n»4)
2.8(n»3)
4.9(n-1)
2.8(n-l)
2.5(n-1)
2.9(n»l)
*
4.9(n-3)
5.2(n=2)
2.7(n-4)
2.9(n-3)
Sr
0.5
1.5
2.3
0.5
0.7
0.8
*
*
" *
*
0.8
0.6
1.1
0.8
S
3.0
1.3
2.6
2.4
1.1
1.3
*
*
*
*
2.5
2.2
1.4
1.3
%RSD
69.4
55.3
77.6
61.0
49.2
44.8
*
*
*
*
50.8
41.9
51.8
43.2
* a value cannot be calculated from existing data
n a number of laboratories reporting data
ND » No data reported
-------
SECTION 3 :
RECOMMENDATIONS! §v^ '
Based on the study results, observations regarding the methodology, and
comments from study participants, the following recommendations are presented
for future work:
For the radiant heat Ignition test, develop an automated system which
activates the radiant heat source when the chamber Interior reaches
the desired temperature.
Introduce an elapsed time device to accurately measure beginning and
end points of the radiant heat and flame propagation tests.
To avoid false starts, lengthen the sample trough used 1n the flame
propagation test so that sample may be Ignited without activating the
first thermocouple. A narrower trough would also minimize
misdirected propagation, giving more consistent results.
Develop a mechanism for generating a uniform spray pattern for the
water ext1ngu1shab111ty test. Automate the spray pulsing system to
maximum extent possible. Incorporate a more accurate means of
measuring water delivery volume.
Define the exact endpolnt of the ext1ngu1shab1!1ty test.
-------
SECTION 4
DESCRIPTION OF STUDY
Test Design
The Interlaboratory study was conducted to measure the precision of three
measurements of 1gn1tab1l1ty characteristics of solids. The study was
composed of two phases: an Initial familiarization phase and a second phase 1n
which an Increased number of wastes was evaluated. For each waste type and
1gn1tab1l1ty characteristic, participants were required to perform six
replicate measurementsthree on each of two days. Analysis of the reference
material was required before and after each triplicate run.
Methodology
The test methods evaluated 1n this study, 1gn1tab1Hty, flame propagation
and water ext1ngu1shabH1ty, were developed as a means of judging the
combustion characteristics of waste materials. The details of these methods
are presented 1n Appendix A. The test chamber described 1n Appendix B was
used for'all evaluations. In the radiant heat Ignition test a radiant heat
source is placed 6 cm from the surface of a waste material. Ignition is
detected by a thermocouple sensor placed above the sample surface and the time
required for ignition is recorded on a strip chart recorder. The rate of
flame propagation 1s measured by recording the time required for a flame to
burn a premeasured distance between two thermocouple sensors placed a fixed
distance above the sample surface. Results are then expressed as cm/sec. The
axtinguishability characteristic is measured by Igniting the material and,
when the surface of the sample is completely aflame., extinguishing with a
calibrated spray of water, the volume of which is used as the measure of
extinguishability.
Participating Laboratories
Approximately 20 laboratories were contacted by Research Triangle
Institute (RTI) for an indication of interest. The initial list of contacts
was provided jointly by the Office of Solid Waste (OSW), the Environmental
Monitoring and Support Laboratory, Cincinnati (EMSL-C1ndnnati), and the
American Society for Testing and Materials (ASTM). Representatives of each
laboratory were informed of the nature and objective of the study and notified
that participation would be on an unpaid basis. Eight laboratories agreed to
participate, however, three laboratories of the eight that participated in
Phase I withdrew from Phase II of the study. The five remaining laboratories
submitted data from the radiant heat ignition test. Four of the five also
returned results from the flame propagation and water extinguishability
tests. The final study, therefore, Included the five laboratories which are
1isted below:
-------
Dow Chemical Company
Texas Division
Freeport, TX 77541
Gull ford Laboratories
827 Huffman Street
Greensboro, NC 27405
Research Tr1angle Institute
P.O. Box 12194
Research Triangle Park, NC 27709
Safety Consultants Engineering, Inc.
5240 Pearl Street . .
Rosemont, IL 60018
Twin City Testing and Engineering Laboratory, Inc.
662 Cromwell Avenue
St. Paul, MN 55114
Phase I
In this study, an Initial Phase I was Included to Increase the reliability
of Phase II measurements by 1) familiarizing the analysts with the ignita-
bility methodologies and 2) insuring accurate calibration and consistent
operation of the ignitability apparatus prior to Initiation of Phase II. Each
of nine laboratories war. provided an RTI-built.testing apparatus (Appendix B)
a reference material, and aliquots of two wastes, chosen because both had been
characterized previously in a single-laboratory evaluation (2). Wood wool
excelsior was chosen as the reference material because of its use by
Underwriters' Laboratories as a standard for class A fire extinguishers and
its consistent behavior in the single-laboratory evaluation. A summary of the
Phase I data 1s presented in Section 5, Discussion and Conclusions.
Selection and Preparation of Hastes .
The two materials used in Phase I were lignite-coal/xylene and red oak
sawdust/kerosene mixtures. The lignite coal was dried in a fume hood, ground,
and sieved to 40-60 mesh and placed 1n containers. The material was then
spiked with reagent grade xylene and mixed on a rotary blender for 20 minutes
to give a 25% (w/w) xylene concentration In the mixture. Red oak sawdust from
a sawmill was collected, air dried, placed In containers, spiked with reagent
grade kerosene, and mixed on a rotary blender for 20 minutes, yielding a 20%
kerosene concentration 1n the mixture.
Test materials 3 through 9 were used 1n Phase II of the study. All wastes
are described 1n Table 2.
-------
Table 2. Physical Description of Jest Materials
Phase I Materials
1. Coal/Xylene. Lignite coal was ground to approximately 10 mesh and
combined with reagent grade xylenes to yield a 25% (w/w) mixture of
xylenes and coal.
2. Sawdust/Kerosene. Red oak sawdust was dried for 24 hours at ambient
temperature. A mixture of 20X (w/w) reagent grade kerosene and dried
red oak sawdust was prepared.
Phase II Materials
3. Cotton Fiber. Commercially available.
4. Polyurethane Foam. A one-Inch thick foam of the type used for padding
on furniture or in pillows. Submitted as a single piece. Commercially
available.
5. Paint Waste. A yellow-colored composite paint waste obtained from a
hazardous waste disposal facility. This material had the consistency of
putty and a strong acetate odor. There was.no apparent separated
solvent on surface. Characteristic of paint manufacturing residual.
6. Waste Oil. A composite of used oil collections from local service
stations. This material had the consistency of molasses.
7. Waste Oil/Sand. A mixture of a light waste oil, the same as used in
Waste No. 6, (60%) and builder's sand (40%). Some stirring needed to
maintain sample homogeneity.
8. Waste Solvent. A viscous orange-colored composite of waste materials
obtained at Triangle Resources Industries, Reidsville, NC 27320.
9. Same as No. 2.
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Section 5
TREATMENT OF DATA
The purpose of the data generated 1n this collaborative study was to
estimate the single and overall precision of measurements of the 1gn1tab111ty
characteristics of solid wastes. Because there are no true values-associated
with the measurements for each material tested, statistical analyses are
necessarily limited to estimates of precision. Prior to statistical analyses,
all data were -tested for outliers using an Iterative Cochran's test for
homogeneity of variances at the 95* confidence leve.1. 'According to Cochran,
If a standard deviation of one set of replicates Is significantly different
from the other standard deviations 1n the group, then that set belongs to a
separate population and can be rejected subject to the significance level
criteria below. The criteria for the rejection was 0.05 significance level
for Cochran's "C" given by the formula shown below:
largest
"1
Si = standard deviation of the 1th pair of duplicates
Data rejected using Cochran's test are denoted by "**" following the results
in Phase II data tables (Appendix C). No further attempts were made to
identify outlying data. With the unusually small amount of data returned by
study participants 1t was feared that elimination of erratic but valid data
points would occur, biasing the final results.
For each laboratory and waste material, ,the traditional mean and standard
deviation of daily triplicate measurements were calculated. Single-laboratory
precision estimates (Sr) were calculated from these,data as follows:
Single-Laboratory/Analyst Standard Deviation:
c2 . n c2 . 4. c2
"LI \1 nL2 \2 * * * nL1 b1
nLl + nL2 * * njj
where: nL-f = number of replicate determinations performed by laboratory 1
2
= variance of replicate measurements by laboratory 1
8
-------
To characterize the multllaboratory performance of the methods, the overall
meanX, the overall precision (S) and the percent relative standard deviation
XRSDV were computed as follows:
Overall Mean: X 1 " v
ST * «« 11
" 1-1 i
where: n number of laboratories
T » mean of measurements reported by laboratory 1
Overall Precision:
(V
where S- » standard deviation of means of n laboratories
p
For this study, So has been estimated from means of 3 replicate observations in
each laboratory, thus 1t Includes all the variability common between
p
laboratories (Sg)» but only one third of the variability common within each
laboratory (S /3). Since we want S to Include all variability for a single
analysis in any laboratory, therefore for this study;
99??? ? ??
r£ _ r*- t <£ _ et . ^C . jfC. _ rC. . y^C.
S - SB + Sr - SB + Sr + 25r - 5X + 25r
~r
Percent Relative Overall Standard Deviation:
%RSD = 4 x 100
-------
Section 6
DISCUSSION AND CONCLUSIONS
Phase I Results
The Importance of requiring participants to analyze preliminary samples
prior to the formal study has been shown 1n previous method validation
studies. Such analyses help provide more realistic data by: 1) familiarizing
analysts with analytical methods; 2) allowing resolution of equipment or
procedural problems; and 3) screening laboratories that are either unwilling
or unable to solve analytical difficulties. For this collaborative effort, no
attempt was made to disqualify laboratories, but only to familiarize them with
the test chambers and samples. Each laboratory received sufficient amounts of
each of two test materials for measurement of the three 1gn1tab1l1ty
characteristics. The results of Phase I measurements are shown 1n Tables 3-5.
The mean Ignition times reported by six laboratories for test material 1
(coal/xylene) was 24.0 seconds on day 1 and 24.5 on day 2. Overall precision
S of those measurements was 11.1 and 7.8 seconds, respectively, representing
relative standard deviations (XRSD) of 46.3 and 32.0 percent. Ignition time
measurements on test material 2 (sawdustAerosene) were times of 16.0 and 23.5
seconds for day 1 and day 2 measurements, respectively, with relative standard
deviations of 27.2 and 47.4 percent. The reference material, wood wool
excelsior, measured before and after each set of three samples, performed
consistently on both days, giving means of 49.5 and 51.4 seconds and relative
standard deviations of 14.1 and 5.7 percent. The results obtained from test
materials 1 and 2 do not appear to have been influenced significantly,
therefore, by fluctuations 1n the operating characteristics of the test
chambers. ' "
Results of flame propagation tests reported by seven laboratories for test
material 1 yielded a mean propagation rate of 0.49 and 0.57 cm/sec for day 1
and day 2 measurements, respectively, with relative standard deviations of
43.3 and 25.45L Precision for test material 2 was slightly poorer, as
indicated by day 1 and day 2 relative standard deviations of 40.9 and 50.0*,
respectively. Only four laboratories reported flame propagation data for test
material 2. All of the remaining laboratories reported that a flame would not
propagate over the entire surface of the samples. Since this problem did not
occur in the single laboratory evaluation of these methods (2) or in the
analysis of the reference material (Table 4), a probable cause of non-
propagation was non-homogeneity of the test material. At least one laboratory
reported that the contents of separate containers of the same test material
differed in appearance.
In the water extingu1shabH1ty test, the volume of water needed to
extinguish a flame on test material 1 was 17.8 mL for both days 1 and 2, with
overall precision (S) of 14.5 ml (XRSD 81.3X) and 17.6 ml (98.8*),
respectively. Test material 2 fires required an average of 5.9 ml of water in
day 1 measurements and 3.0 ml 1n day 2 measurements. Percent relative
standard deviations were 79.1 and 55.IX on day 1 and day 2, respectively,
while those for the reference material were 102.9 and 53.3X.
10
-------
Table 3. Phase I Results - Radiant Heat Ignition Test
Test Material 1: Coal/Xylene
Laboratory No.
Summary Statistics
Day 1
Day 2
Day 1
Sample Mean (Sec) 7
Std. Deviation S
Variance S?
Sample Mean (Sec) 7
Std. Deviation S
Variance S2
Sample Mean (Sec) 7
Std. Deviation S
Variance S2
Day 2 Sample Mean (Sec) 7
Std. Deviation S
Variance $2
101
19.0
1.6
2.3
22.2
1.2
1.4
. Test
.
101
13.2
2.9
8.4
'16.7
3.8
14.8
102 105 106
22.7 23.0 16.5
1.3 1.0 1.7
1.6 1.0 3.0
28.0 25.3 18.8
0.6 5.7 1.2
0.4 32.3 1.6
107 111
45.8 17.3
3.8 1.7
14.4 2.9
36.7 16.2
5.8 1.2
33.9 1.4
S Sr
24.0
2.0
24.5
3.4
S XRSO
11.1 46.3
7.8 32.0
Material 2: Sawdust/Kerosene
Laboratory No.
102 105 106
21.5 87.2* 13.3
2.2 68.3* 2.9
4.8 4664* 8.3
24.2 40.0 20.3
3.8 11.0 4.8
14.6 121 22.6
107 111
37.5* 16.2
22.7* 1.2
515* 1.4
ND 16.2
6.1
37.9
Summary
X S,.
16.0-
2.4
23.5
6.5
Statistics
S XRSO
4.3 27.2
11.1 47.4
* * Data rejected as outliers by Cochran's test
ND ' No Data reported or sample did not Ignite
-------
Table 3: Phase I Results - Radiant Heat Ignition Test
Reference Material
Laboratory No.
Summary Statistics
Day 1
Sample Mean (Sec)
Std. Deviation
Variance
I
S
S2
101
(n-2)
54.2
2.3
5.4
102
(n-4)
49.3
0.9
0.8
105
(n-3)
53.7
11.0
121.0
106
(n-4)
43.0
7.4
55.1
107 111
(n-4)
ND 47
4
20
.1
.5
.2
^
Laboratory No.
Day 2
Sample Mean (Sec)
Std. Deviation
Variance
co coxl
ro
101
(n-3)
51.0
1.7
2.8
102
(n-4)
50.6
4.3
18.6
105
(n-3)
50.7
3.8
14.3
106 '
(n-4)
94.4*
8.4*
70.6*
107 111
(n-4)
ND 53
1
36
.4
.9
X Sr S XRSD
49.5
6.3 7.0 14.
Summary Statistics
1
X ST S *RSD
51.4
3.2 2.9 5.7
* Data rejected by Gochran's test
ND - No data; sample ,d1d not Ignite
-------
Table 4. Phase I Results - Flame Propagation Test
Test Material 1: Coal/Xylene
Laboratory No.
Summary Statistics
Day 1
Day 2
Sample Mean (cm/Sec)
Std. Deviation
Variance
Sample Mean (cm/Sec)
Std. Deviation
Variance
I
tz
S2
101
0.33
0.02
0.0005
0.39
0.05
0.002
102
0
0
0
0
0
0
.54
.18
.03
.68
.04
.002
Test
105
0.57
0.13
0.02
0.63
0.15
0.02
Material
106
0.31
0.11
0.01
0.65
0.16
0.02
107
0.80
0.26
0.07
0.62
0.22
0.05
111
0.49
0.09
0.01
0.52
0.03
0.001
112
0.36
0.09
0.01
0.48
0.10
0.01
% Sf S XRSD
0.49
0.15 0.21 43.3
0.57
0.12 0.14 25.4
2: Sawdust Kerosene
. Laboratory No.
Day 1
Day 2
* a
ND *
Sample Mean (cm/Sec)
Std. Deviation
Variance
Sample Mean (cm/Sec)
Std. Deviation
Variance
S2
y
§2
Data rejected by Cochran's
No cjata reported. No flame
101
ND
ND
test
propagj
102
0
0
0
0
0
0
it1<
.10
.01
.0001
.08
.01
.0001
on
105
ND-
'ND
106
ND
ND
107
0.06
0.04
0.001
0.01
0.003
111
0.03
0.01
0.002
0.14*
0.20*
0.04*
112
0.07
0.03
0.001
0.02
0.003
. Summary Statistics
X Sp S XRSD
0.06 -
0.03 0.02 40.9
0.04
. 0.02 0.02 50.0
-------
Table 4. Phase I Results - Flame Propagation Test
Reference Material
Laboratory No.
Summary Statistics
Day 1
Sample Mean (cm/Sec) I
Std. Deviation S
Variance S2
101
(n-2)
0.48
0.03
0.001
102
(n-4)
0.46
0.03
0.001
105
(n=4)
0.51
0.05
0.003
106
(n-2)
0.32
0.014
0.002
107
(n-4)
0.40
0.01
0.0001
111
(n-4)
0.33
0.04
0.001
112
(n-4)
0.38
0.04
0.001
X
0.41
Laboratory No.
Day 2
Sample Mean (cm/Sec) J
Std. Deviation S
Variance S2
101
(n-2)
.0.43
0.11
-0.01
102
(n-4)
0.50
0.07
0.004
105
(n-4)
0.52
0.03
0.001
106
(n-2)
0.41
0.11
0.01
107
(n-4)
0.40
0.04
0.002
111
(n-4)
0.37.
0.05
0.003
112
(n-4)
0.35
0.025
0.001
X
0.42
Sr
0.03
Summary
Sr
0.06
S XRSD
0.08 19.0
Statistics
S XRSD
0-.08 19.1
-------
F*
01
Table 5. Phase I Results - Water Ext1ngu1shabH1ty Test
Test Material 1: Coal/Xylene
Summary Statistics
Day 1
Day 2
Day 1
Day 2
* a
NO »
Sample Mean (ml)
Std. Deviation
Variance
Sample Mean (ml)
Std. Deviation
Variance
-
Sample Mean (ml)
Std. Deviation
Variance
Sample Mdan (ml)
Std. Deviation
Variance
Data rejected as
No data reported
I
S2
I
la
7
S
S2
I
S2
outliers
. Sample
101
11.3
0.7
0.5
9.6
7.1
50.4
101
ND
ND
102
39.2
7.7
58.8
41.9
2.1
4.5
Test
102
3.8
0.6
0.4
3.9
0.6
0.3
105
35.4
8.7
74.9
38.3
5.4
29.6
106
6.3
1.7
2.8
8.7
3.0
9.1
107
17.3
5.9
35.6
78.0*
32.3*
1045*
111
7.5
2.6
7.0
7.1
2.7
7.5
11
7
1
3
1
0
0
2
.6
.9
.5
.4
.3
.1
Material 2: Sawdust/Kerosene
Laboratory- No.
105
5.3
2.7
7.1
5.1
0.9
0.9
106
5.3
2.1
4.3
3. '6
1.7
2.8
107
- 8.6*
8.1*
66.8*
1.4
0.5
0.3
111
1.8
1.0
1.0
2.5
1.3
1.6
112
13
2
7
1
0
0
.2
.71
.3
.4
.2
.04
% Sr S XRSD
17.8
5.1 14.5 81.3
17.8
1.8 17.6 98.8
Summary Statistics
X Sr S XRSD
5.9
2.1 4.7 79.1
3.0
« 0.9 1.7 55.1
by Cochran's test
did not Ignite
-------
Table 5. Phase I Results - Water Extingu1shab111ty Test
Reference Material
Laboratory No.
Summary Statistics
101
(n-2)
Day 1
Day 2
Sample Mean (ml)
Std. Deviation
Variance
Sample Mean (mL)
Std. Deviation
Variance
I
S
S2
7
so
S2
11.
7.
52.
5.
0.
0.
4
2
3
1
3
1
102
(n-4)
4.1
0.5
0.3
3.5
0.5
0.3
105
(n-4)
3.5
0.7
0.6
3.7
1.1
1.3
106
(n-4)
3.6
0.3
0.1
3.0
1.3
1.7
107
(n=4)
8.7
8.1
65.3
3.8*
3.7*
13.4*
111
(n-4)
1.2
0.3
0.1
1.2
0.6
0.3
112
(n-4)
1.2
0.2
0.03
1.5
0.4
0.2
X Sr S XRSD
4.8
3.8 4.9 102.9
3.0
0.8 1.6 53.3
-------
Outliers
Because of the small amount of data received for Phases I and II, minimal
outlier testing was performed. During Phase I, the number of data sets ranged
from 4 to 7. For these data, only Cochran's test was applied to eliminate
laboratories with the worst precision. Those laboratories had 1n most cases,
also returned study data that were abnormally high as compared to other
laboratories. In Phase I, 5 of 71 triplicate measurements were rejected while
in Phase II, 1 of 98 triplicates were rejected.
Phase II Results
A compilation of the raw data obtained during Phase II of the study can be
found 1n Tables 6-22 (Appendix C). Only five Phase II laboratories reported
radiant heat Ignition data. Four of those five also reported flame
propagation and water ext1ngu1shabH1ty results. Ideally, each of the
responding laboratories should have returned complete data sets for seven
waste types for each of the three Ignltablllty tests. Test materials 3 and 4,
cotton fiber and polyurethane foam, respectively, failed to Ignite within five
minutes under the radiant heat source. The radiant heat Ignition procedure
was performed, therefore, on only five sample types by five laboratories.
The flame propagation test yielded even fewer useable data than the
radiant heat test. Test materials 6 and 7 could not be analyzed by the
procedure. For this test, five test materials were examined by an average of
only three laboratories, making statistical evaluation of the methods
difficult. Likewise, 1n the water extlngulshablllty test, three to four
laboratories reported data from five test materials.
Statistical Summary and Precision Statement
For ease of discussion of the radiant heat Ignition, flame propagation,
and water extinguishabilHy tests of Phase II, the statistical portions of
Tables 6-22 (Appendix C) have been combined In Table 1. Five test materials
were analyzed by each of the three tests. Since only one laboratory reported
extinguishability data for test materials 6 and 7, those data are not being
considered in this discussion. Radiant heat ignition measurements yielded
overall percent relative standard deviations 1n the range of 19-101X. Data
obtained from flame propagation and extinguishability tests, had relative
standard deviations of 12.3-100.OX and 41.g-77.6X, respectively.
Evaluation of Methods
The quantity of data from Phase II laboratories was considerably smaller
than required for a meaningful statistical evaluation of the 1gn1tab1lity
methods. Thorough correlation of results of the three methods for each test
material is not possible because 1n most cases only two tests were performed
on each waste. Examination of the data 1n Table 1, however, reveals
considerable variation 1n both single-laboratory and overall precisions for
all three tests. It 1s not possible to state which test exhibits the greatest
17
-------
variability either day-to-day or across waste types. The most reliable
evaluation of the methods 1s likely therefore, to be qualitative. As part of
the study, participants were encouraged to submit narratives of their
experiences with the test apparatus, and to provide comments as to the
applicability of the methods to waste characterization. One laboratory
observed while conducting the radiant heat Ignition test that the relationship
between the rheostat setting and the source temperature was not constant. As
a result, replicate radiant heat measurements were highly variable even at the
same rheostat setting. Another laboratory noted that the Interior temperature
of the chamber changed as a function of the length of time the Instrument was
In use and soot deposited on the chamber walls and heat source. It was
further noted that fluctuations In Interior chamber temperature resulted when
the chamber door was opened to Introduce samples. Since Ignition times are
dependent on chamber temperature at the beginning of the test, a second heat
source should be Introduced to the chamber accompanied by automatic activation
of 1) the radiant heat source at a predetermined chamber temperature and 2) a
timing device that would measure and record time elapsed between activation of
the heat source and a signal from the flame-detecting thermocouple. This
would eliminate the need for a strip chart recorder, which in this study was
itself the source of considerable error. The test procedure requires a chart
speed of 0.5 inches/minute (0.02 cm/sec). Since the chart distances recorded
in the study were commonly 1n the 0.2-0.4 cm range, a possible 10-20% error
was introduced by the recording step alone.
Operational difficulties were also experienced In the flame propagation
test. The leading cause for the small amount of data was non-propagation of
the flame or non-ignition. One laboratory reported that the propagation rate
for some samples depended on the depth of the sample in the trough. One
analyst reported that flames had a tendency to propagate erratically or in the
opposite direction of the second thermocouple. A narrower trough would
minimize the possibility of misdirected propagation. Some false starts were
reported when ignition of the sample was attempted. This problem could be
solved by lengthening the trough so that the sample can be ignited without
activating the first thermocouple.
In the water extinguishability test, several factors undoubtedly
contributed to the overall error of the measurements. Perhaps the greatest
source of error was the confusion over whether extinguishment of only visible
flames or also the embers constituted the endpoint of the analysis. If the
latter endpoint is assumed, larger amounts of water would be used.
Modifications in the water delivery system would solve some problems which
were reported by analysts. The system 1s designed to deliver a cone-shaped
spray, the diameter of which 1s the same as that of the sample dish. More
accurate results might be achieved by using a spray pattern that delivers
water to the entire surface of the sample. .Direct measurement by weight, of
the amount of water delivered to the flaming sample would be preferable to
calculating the value from time and delivery rate, both of which contribute
separately to the total error of the extinguishability measurement.
18
-------
The three 1gn1tab1l1ty tests studied 1n this collaborative effort have the
potential of being useful and precise techniques for determining the potential
Ignition hazard of solid wastes. Before the methods, particularly the water
ext1ngu1shabH1ty test, can be considered fully reliable, substantial
modifications and refinements of the test chamber Itself are mandatory. Many
of those modifications have been discussed 1n this section, but only further
testing on actual waste samples will determine the extent of the changes
ultimately required.
In the current study, although eight laboratories agreed to participate 1r
the full study, data/test were reduced to as few as three sets, resulting 1n
only limited statistical treatment of the results and evaluation of the
methods. Once the method 1s refined, the 1gn1tab1l1ty tests should again be
collaboratlvely tested with sufficient laboratories that are paid, 1f
necessary, to assure full participation.
19
-------
REFERENCES
1. Federal Register, Vol. 45, No. 98, May 19, 1980, p. 33122
2. Michael, L.C., PerHtt, R.L., and PelHizarl, E.D. Single-Laboratory
Evaluation of IgnltabllUy and Related Methods. Environmental Protection
Agency, Las Vegas, NV, 1984, 49 pp.
3. McFarren, E.F., Llshka, R.J., and Parker, J.H. Criterion for Judging
Acceptability of Analytical Methods. Analytical Chemistry 42 (3), 358,
1970.
20
-------
APPENDIX A
IGNITABILITY METHODS
RADIANT HEAT IGNITION TEST PROCEDURE
1.0 SUMMARY OF THE METHOD
A sample 1s placed 6 cm beneath a preheated radiant heat source and the
time to Ignition detected by a thermocouple sensor and recorded on a strip
chart recorder.
2.0 APPARATUS AND REAGENTS
2.1 Test chamber - as shown 1n Figure 1..
2.2 Sample container - aluminum weighing pan, 6 cm diameter X 1.7 cm deep.
2.3 Controller/sensor - as shown 1n Figure 1.
2.4 Recorder - strip chart, variable speed and Input Impedance.
2.5 Safety Equipment
2.5.1 Flameproof gloves (Lab Safety Supply 1915M or equivalent)
2.5.2 Tongs - 53 cm (Fisher, 15-207 or equivalent)
2.5.3 Respirator (Fisher, 13-995-11 or equivalent)
2.6 Balance (minimum accuracy to nearest 100 mg)
3.0 TEST PROCEDURE
3.1 Locate the test chamber in a fireproof fume hood with the exhaust fan
turned on.
3.2 If the hood 1s large enough, locate the controller/sensor and the
recorder outside the hood but 1n proximity to the test chamber.
3.3 With an empty sample container on the sample platform, (Figure 1;
part no. 5) position the sample platform to provide a heating element
(Figure 1; part no. 1) to sample container (top r1m) distance of 6 cm.
3.4 Position the thermocouple (Figure 1; part no. 7) 1 cm above the top
rim and centered over the sample container.
3.5 Connect the thermocouple to position 33 (Figure 1) on the controller/
sensor using the cable supplied.
3.6 Connect the heater/solenoid cable (Figure 1; part no. 16, 17) to
position 34 (Figure 1) on the controller/sensor.
3.7 Connect the power cord on the controller/sensor to a 110 VAC power
source.
3.8 Set the variable transformer to 0.
3.9 Position a dummy (blackened with carbon soot) sample container
(centered) under the heat source. Close the chamber door.
3.10 Turn on the controller/sensor.
3.11 Turn on the heater. Set the variable transformer to the setting
determined during the temperature adjustment procedure.
3.12 Preheat the radiant heat source for 30 minutes.
3.13 Transfer sample to the sample container to a depth of approximately
1 cm, making sure that the sample surface 1s level and smoothed.
21
-------
WARNING
Extreme care must be exercised In testing materials known or
suspected of being extremely flammable. Preliminary tests using
greatly diminished sample sizes should be conducted prior to
performing the actual test to Insure the safety of the analyst.
A reduced test sample depth should be used In cases where sample
Ignition 1s extremely rapid and/or violent.
3.14 Place the filled sample container outside, but In proximity to, the
test chamber.
3.15 Start the recorder at a chart speed of 0.5 1n/m1n and a full-scale
sensitivity of 1 volt/Inch.
3.16 Open the chamber door and remove the dummy sample container.
3.17 Using tongs and flameproof gloves, pick up the filled sample
container and place 1t, centered, under the radiant heat source.
Immediately mark the recorder chart by gently touching the tip of the
thermocouple with the tongs. Lower the door on the test chamber.
CAUTION
The placement of the sample beneath the radiant heat source, the
marking of the recorder chart and the closing of the chamber
door must be executed as quickly as possible to optimize the
precision of the test results.
3.18 Raise the chamber door and remove the Ignited sample from beneath the
radiant heat source and carefully place 1t 1n the bottom of the
chamber.
WARNING
Raise the fume hood and test chamber doors just to a level that
facilitates removal of the sample from beneath the radiant heat
source. Flameproof gloves should be used 1n combination with
tongs to protect the analyst from the burning sample.
3.19 Extinguish the fire by smothering.
3.20 Prepare the chamber for the next sample by positioning the dummy
sample container beneath the radiant heat source.
3.21 Lower the fume hood door to one-half the height of the chamber.
3.22 Measure the distance (cm) from the Initial mark to Ignition on the
recorder. Calculate the time to Ignition from the calibrated
recorder speed.
3.23 Proceed with the analysis of subsequent samples by repeating steps
3.13 through 3.22.
22
-------
FLAME PROPAGATION TEST PROCEDURE
1.0 SUMMARY OF THE METHOD
A sample 1s placed 1n an aluminum trough and Ignited at one end. The time
required to burn a premeasured distance 1s sensed by thermocouples and
recorded on a two-pen strip chart recorder.
2.0 APPARATUS AND REAGENTS
' *
2.1 Test chamber - as shown 1n Figure 1.
2.2 Sample container - prepared by molding heavy-duty aluminum foil 1n a
20.5 X 6.6 X 3.5 cm (Inside dimensions) stainless steel trough.
2.3 Controller/sensor - as shown 1n Figure 1.
2.4 Recorder - two-pen, strip chart, variable speed and Input Impedance.
2.5 Safety Equipment i
2.5.1 Flame proof gloves (Lab Safety Supply, 1915M or equivalent)
2.5.2 Tongs - 53 cm (Fisher, 15-207 or equivalent)
2.5.3 Respirator (Fisher, 13-995-11 or equivalent)
2.6 Wood splints
3.0 TEST PROCEDURE
3.1 Locate the test chamber in a fireproof fume hood with the exhaust fan
turned on.
3.2 If the hood is large enough, locate the controller/sensor and the
recorder in the hood. If sufficient space Is not available in the
hood, locate the controller/sensor and/or the recorder outside the
hood but in proximity to the test chamber.
3.3 Connect the thermocouples, located in the bottom of the test chamber,
to the. strip chart recorder.
3.4 Prepare the sample container by molding heavy-duty aluminum foil in
the stainless steel trough.'
3.5 Transfer sample to the sample container to a depth of approximately
1 cm, making sure that the sample surface is even and smoothed.
WARNING
Extreme care must be exercised in testing materials known or
suspected of being extremely flammable. Preliminary tests using
greatly diminished sample sizes should be conducted prior to
performing the actual test to insure the safety of the analyst.
A reduced sample depth should be used 1n cases where sample
ignition is extremely rapid and/or violent.
3.6 Place the filled sample container centered between the two thermo-
couples in the bottom of the test chamber.
3.7 Start the recorder at a chart speed of 0.5 in/min and a full-scale
sensitivity of 100 millivolts/Inch.
3.8 With a lighted wood splint, Ignite the sample at one end of the
trough. Immediately lower the test chamber door.
3.9 Lower the fume hood door to one-half the height of the test chamber.
23
-------
3.10 Record the distance (cm) between the two thermocouples and the linear
distance traveled by the recorder (cm) peri during the burn period.
HOTE % ..&** < A
If the flame does not propagate the full distance between the
thermocouples, manually measure the distance propagated and the
distance travelled by the recorder pen.
3.11 Raise the fume hood and test chamber doors slightly. Cover the
sample with the stainless steel trough I1d.
WARNING
The fume hood and test chamber doors should be raised only as
high as required to cover the burning sample. Flameproof gloves
should be used In combination with tongs to protect the analyst
from the burning sample.
3.12 Prepare the chamber for the next sample by removing the extinguished
sample.
24,,
-------
WATER EXTINGUISHABILITY TEST PROCEDURE
1.0 SUMMARY OF THE METHOD
An Ignited sample 1s placed 6 cm beneath a sprayer nozzle and extinguished
by delivering water at a calibrated rate to the sample. The volume of water
required to extinguish the sample 1s determined from the duration of the spray
and the flow rate of water.
2.0 APPARATUS AND REAGENTS
2.1 Test chamber - as shown 1n Figure 1.
2.2 Sample container - aluminum "tart" pan, 1.5 cm diameter (top, Inside)
X 3.2 cm deep.
2.3 Controller/sensor - as shown 1n Figure 1.
2.4 Recorder - strip chart, variable speed and Input Impedance.
2.5 Safety Equipment
2.5.1 Flameproof gloves (Lab Safety Supply, 1915M or equivalent)
2.5.2 Tongs - 53 cm (Fiaher, 13-995-11 or equivalent)
2.5.3 Respirator (Fisher, 13-995-11 or equivalent)
2.6 Balance (minimum accuracy to nearest 100 mg)
2.7 Wood splints
2.8 Water - municipal supply
3.0 TEST PROCEDURE
3.1 Locate the test chamber 1n a fireproof fume hood with the exhaust fan
turned on.
3.2 If the hood 1s large enough, locate the controller/sensor and the
recorder in the hood. If sufficient space 1s not available in the
hood, locate the controller/sensor and/or the recorder outside the
hood but in proximity to the test chamber.
3.3 Connect the copper tubing containing the water pressure regulator and
gauge to a suitable supply source using the brass fitting (3/8" male
NPT - 1.4" tube) provided.
CAUTION
This tubing should be connected to a water supply source with
the regulator and gauge located close to the source. If the
fitting supplied for this connection is incorrect, substitute
the appropriate alternative.
3.4 Connect the long end of the copper tubing to the solenoid valve
(Figure 1, part no. 13).
3.5 Install the sprayer nozzle (Figure 1,'part no. 10) in the bulkhead
fitting on the inside right side of the test chamber.
3.6 Turn on the water at the source and test for leaks. Tighten fittings
as required.
3.7 Set the water pressure to the solenoid valve to 10 psi.
3.8 Position the sample platform centered and exactly 6 cm under the
sprayer nozzle.
25
-------
3.9 Place the aluminum divider between the support brackets located near
the bottom of the test chamber.
3.10 Turn on the power to the controller/sensor.
3.11 With an empty sample container on the sample platform, activate the
sprayer continuously for 1 minute to eliminate air from the copper
tubing.
3.12 Read the water pressure (1n the absence of flow) from the pressure
gauge. Adjust to 10 ps1, 1f necessary.
3.13 Activate the sprayer 1n several short bursts and again note the water
pressure. Adjust, 1f necessary.
3.14 Repeat step 3.12 until the pressure gauge reads 10 ps1 without flow/
3.15 Using an empty sample container, activate the sprayer 1n twenty short
bursts (approx. 100 millisecond), approximately 1 second apart.
Record the cumulative time.
3.16 Carefully transfer the water 1n the sample container to a 25 ml
grduated cylinder. Record the volume delivered.
3.17 Calculate the water flow rate 1n m1H1l1ters per second.
3.18 Transfer sample to the sample container to a depth of 1 cm, making
sure that the sample surface 1s level and even.
WARNING
Extreme care must be exercised 1n testing materials known or
suspected of being extremely flammable. Preliminary tests using
greatly diminished sample sizes should be conducted prior to
performing the actual test to Insure the safety of the analyst.
A reduced test sample depth should be used 1n cases where sample
Ignition 1s extremely rapid and/or violent.
3.19 Place the sample on the aluminum divider near the bottom of the test
chamber.
3.20 Ignite the sample, 1n the center, with a lighted wood splint. Lower
the test chamber door completely and the fume hood door to one-half
the height of the chamber.
3.21 Allow the fire to burn until the entire surface of the sample is
burning.
3.22 Open the fume hood and chamber doors. Using tongs, center the
ignited sample on the sample platform directly beneath the sprayer
nozzle.
3.23 Lower the test chamber door completely and the fume hood door to
one-half the height of the test chamber.
3.24 Depress the switch which activates the sprayer and timer, in short
bursts (approximately 100 milliseconds), approximately 1 second apart
and observe for continued burning between bursts.
CAUTION
This delivery process mayn require practice before 1t can be
executed successfully.
3.25 Record the time to extinguishment to the nearest 0.01 seconds.
3.26 If the water was not effective in extinguishing the fire, extinguish
the flame by smothering.
3.27 Prepare the test chamber for the next sample by resetting the timer
and removing the extinguished sample.
26
-------
APPENDIX B
IGHITABlllTY TEST CHAMBER
u
0
0
a
D
20
°rs
o L5
30
Ds 9
0*
3 i i.
Figure 1. Ignitmbllity Test Chanber and Controller/Sensor.
27
-------
PARTI LIST
Pm *°- Description
1 Heater, 750 watt, 120 volt (American Scientific Products,
61856); lever clay aaaeably forPrecision KJeldahl flask
heater; element cemented to ceramic base with Savereisen
sealing cement (No. 93 powder).
2 Heater support, Uoistrut P-1000.
3 Aluminum rod-, 1/2 in diameter (Fisher, 14-666).
4 Right angle connector (Fisher, 14-666-20).
S Plate support (Fisher, 14-666-24).
6 Thermocouple protection tube, Omegatite 450 , 3.16 x
1/4 x 12 in (Omega Engineering, PTRA31614-12); with
closed end saved off.
7 Thermocouple, sub-miniature, Type'K, Inconel sheith,
0.020 x 12 in (Omega Engineering, SCAIN-020U-12);
Thermocouple extension (Omega Engineering, EXTT-K-24);
Thermocouple connectors.
8 Foot plate (Fisher, 14-666-25)(Omega Engineering, SMP-K-MP).
9 Transite* box, 45 x 45 x 60 cm, hinged top.
10 Hollov spray nozzle, stainless steel, 1/4 x 1-5/16 in
male (McMaster-Carr Supply- 34505K76); female connector,
1/4 x 1/4 in NPT (Swagelok ,.SS-400-7-4).
11 Bulkhead union, stainless steel, 1/4" (Swagelok9,
SS-400-61).
12 Tubing, stainless steel, 1/4 in O.D.
13 Solenoid valve, 1/4 in, normally closed (McHaster-Carr
Supply, 4639R58).
Not shown: Copper tubing, 1/4 in O.D.; pressure gauge,
0-15 psi (Matheson, 63-3115); vater pressure regulator
(Fisher, 15-529); Female branch tee, 1/4 x 1/4 in NPT
(Swagelok , SS-400-3-4TTF).
14 Terminal board, double row (Kulka, 601-GP-2).
15 High temperature cable, copper, 14AWG (W.K. Hile, 9G-PUT-1);
solderless connector, spade terminals.
16 Cable, 2 conductor, 18AVG copper (power supply to heater).
17 Cable, single conductor, 18AVG.
18 Chromatography trough (Fisher, 15-729,54).
19 Door, Transite, sliding; thermal-resistant glass vindow.
20 Angle bracker, 4 hole.
28
-------
PACTS LIST (cont'd.)
21 Auto transformer.
22 Fust holder, povtr.
23 Fuse holder, meters.
24 Fuse holder, beater controller.
23 Fuse holder, heater.
26 Fuse holder, spray.
27 Neon lamp, power.
28 SPST toggle switch, power.
29 Neon lamp, heater control.
30 SPST toggle switch, heater control.
31 Omega Model 650, digital thermocouple thermometer.
32 IMC Model 402, digital timer.
33 Miniature thermocouple jack.
34 Nine-pin Molax connector/panel mount.
35 Neon lamp, sprayer.
36 Double pole, double throw, center off, momentary/on-on
miniature toggle switch (for sprayer).
37 Minature push button switch, momentary switch (timer reset)
29
-------
APPENDIX C
PHASE II DATA
I
Table 6. Phase II Results - Radiant Heat Ignition Test
« *
Test Material No. 5 - Paint Waste
Laboratory No. Summary Statistics
Day 1
Mean (Sec)
Std. Deviation
Variance
Day 2
Mean (Sec)
Std. Deviation
Variance
7
s
S2
"X
S
S2
101
69
16
262
49
13
176
102
65
4
16
69
3
10
106
113
15
231
183
45
2033
Reference
111
155
114
12990
116
18
317
112
88
16
242
ND
X Sr S *RSD
98
52 56 58
104
25 63 60
Material
1
Laboratory No.
Day 1
Mean (Sec)
Std. Deviation
Variance
Day 2
Mean (Sec)
Std. Deviation
Variance
X
s
S2
7
S
S2
101
50
4
17
41
0
0
102
52
1
2
52
3
8
106
40
0
0
42
3
12
111
51
5
28
53
6
36
112"
44
55
3014
ND
Summary Statistics
X Sr S %RSD
47
25 21 45
47
3 7 15
ND = No data reported
30
-------
Table 7. Phase II Results - Radiant Heat Ignition Test
Test Material No. 6 - Waste Oil
Laboratory No. Summary Statistics
Day 1
Mean (Sec) I
Std. Deviation S
Variance S2
Day 2
Mean (Sec) X"
Std. Deviation S
Variance S2
101
91
9
60
80
9
81
102
124
7
56
191
27
745
106
85
18
,. 325
85
23
525
Reference
111 X
'175 119
27
720 '
249 151
27
752
Material
Laboratory No.
Day 1
Mean (Sec) Y
Std. Deviation S
Variance S2
Day 2
Mean (Sec) "X
Std. Deviation S
Variance S2
101
47
0
0
47
8
69
102
43
4
18
55
1
2
106
27
3
12
27
3
12
111 K
52 42
15
231
I
47 44
0
0
Sr S XRSD
17 38 32
23 152 101
Summary Statistics
Sr S *RSD
8 13 30
5 13 29
31
-------
Table 8. Phase II Results - Radiant Heat Ignition Test
Test Material 7 - Waste Oil/Sand Mixture
Laboratory No. Summary Statistics
Day 1
Mean (Sec) I
Std. Deviation S
Variance S2
Day 2
Mean (Sec) Y
Std. Deviation S
Variance S2
101
211
68
4622
210
18
323
102
122
35
1236
57
19
345
106
82
8
58
130
13
175
Reference
Laboratory
Day ]_
Mean (Sec) I
Std. Deviation S
Variance S2
Day 2
Mean (Sec) I
Std. Deviation S
Variance S2
101
43
6
39
46
10
108
102
38
8
72
41
10
98
106
25
0
0
27
3
13
111
191
12
152
113
100
9852
t
Material
No.
in
45
0
0
54 -
10
91
^ ^ Sr S XRSD
151
39 68 45
127
6 63 50
Summary Statistics
X Sr S XRSD
38
5 10 26
42
9 13 32
32
-------
Table 9. Phase II Results - Radiant Heat Ignition Test
Test Material No. 8 - Waste Solvent
Laboratory No.
Summary Statistics
Day 1
Mean (Sec) 7
Std. Deviation S
Variance $2
Da_y 2
Mean (Sec) 7
Std. Deviation S
Variance $2
101
31
4
20
38
3
9
102
54
4
16
49
7
50
106
65
18
325
52
10
108
Reference
Laboratory
Day 1
Mean (Sec) 7
Std. Deviation S
Variance S^
Mean (Sec) 7
Std. Deviation S
Variance S^
101
40
2
4
37
2
4
102
37
10
98
38
6
32
106
27
' 3
13
27
3
13
111
72
22
477
56
2
3
Material
No.
Ill
i
49
5
28
56
12
153
11.2 B Sr S *RSD
84 61
12 14 23 38
150
ND 49
6 9 19
Summary Statistics
112 X Sr S %R5D
59 42
'8 6 13 31
69
40
7 13 33
ND = No data reported
33
-------
Table 10. Phase II Results - Radiant Heat Ignition Test
Test Material No. 9 - Sawdust/Kerosene
Laboratory No. Summary Statistics
Day 1
Mean (Sec) I
Std. Deviation S
Variance S2
Day 2
Mean (Sec) I
Std. Deviation S
Variance S2
101
14
2
3
13
2
3
102
17
11
124
15
6
33
106
13
6
33
12
3
8
Reference
Laboratory
Day J
Mean (Sec) "X
Std. Deviation S
Variance S2
Day 2
Mean (Sec) J
Std. Deviation S
Variance S2
101
43
2
4
46
15
212
102
33
4
18
44
3
8
106
23
3
13
30
0
0
111
16
2
5
,
17
3
6
Material
No.
Ill
49 .
5
28
41
2
3
112
20
7
46
ND
112
71
25
623
ND
X Sr S *RSD
16
6 6 35
14
3 3 24
Summary Statistics
? c c tfDcn
A Ov« o *>i\oU
44
12 18 41
40
7 9 23
ND = No data reported
34
-------
Table 11. Phase II Results - Flame Propagation Test
i *
Test Material No. 3 - Cotton Fiber
Laboratory No. Summary Statistics
DayJ[
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
Y
S
S2
Y
S
$2
102
3.7
0.5
0.3
ND
106
2.6
0.9
0.8
2.65
0.92
0.84
112
6.5
2.2
5.0
ND
8 Sr S XRSD
4.3
1.4 2.3 53.8
2.6
* * *
Reference Material
I
Laboratory No.
Summary Statistics
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
X
S
S2
Y
S
S2
102
0.2
0.01
-
-
0.2
0.1
0.01
106
0.3
0.02
-
0.3
0.08
-
112
0.5
0.08
0.006
ND
X Sr S XRSD
0.3
0.04 0.16 52.1
0.3
0.1 0.1 36.1
ND = No data reported
* = Value cannot be calculated from existing data
35
-------
Table 12. Phase II Results - Flame Propagation Test
Test Material No. 4 - Polyurethane Foam
Laboratory No. Summary Statistics
106 111 112 1 Sr S *RSD
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
* 0.3 0.3 0.4 0.33
S 0.1 . - , - 0.05 0.07 21.4
5 _ -
X" 0.28 ND ND 0.28
S 0.01 - * * *
O
Reference Material
Laboratory No. Summary Statistics
106 111 112 X Sr S %RSD
I 0.4 0.2 0.5 0.4
S 0.10 0.1 0.1 38.2
S2 - - 0.01
I
, *
"X 0.4 ND ND 0.4
S - * * *
S2
ND = No data reported
* = Value cannot be calculated from existing data
36
-------
Table 13. Phase II Results - Flame Propagation Test
Test Material No.5 - Paint Waste
Laboratory No. Summary Statistics
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
y
S
y
s
s2
102
0.02
0.01
0.03
0.007
-
106 111
0.04 0.04
0.004 0.008
0.03 ND
0.003
I
112
0.04
0.005
ND
.
1 Sr S XRSD
0.04
0.01 0.01 28.8
0.03
0.005 0.004 13.6
Reference Material
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
X
s
S2
y
s
S2
102
0.2
0.02
-
0.2
0.04
Laboratory No.
106 111
0.3 0.4
0
0
0.3 ND
0
0
112
0.5
0.1
0.02
ND
Summary Statistics
X Sr S %RSD
0.4
0.1 0.1 38.2
0.3
0.02 0.07 24.2
ND = No data reported
37
-------
Table 14. Phase II Results - Flame Propagation Test
Test Material No. 8 - Waste Solvent
Laboratory No. Summary Statistics
102 106 111 112 X Sr S %RSD
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
I
S2
y
S2
Y
S2
I
s
S2
,
0.1 NO 0.2 0.1 0.1
0.1 0.2 Q.01 0.1 0.1 100.0
0.1 ND ND NO 0.1
0.03 * * *
Reference Material
Laboratory No. Summary Statistics
102 106 111 112 I Sr S *RSD
0.4 ND 0.5 . 0.66 0.5
0.01 - - 0.01 0.13 '26.3
0.4 ND ND ND 0.4
0.1 * * *
ND = No data reported
* = Value cannot be calculated from existing data
38
-------
Table 15. Phase II Results - Flame Progatlon Test
Test Material No. 9 - Sawdust/Kerosene
Laboratory No. Summary Statistics
DayJL
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
I
S2
I
S
S2
102
0.1
0.1
0.2
0.04
102
106 111
0.2 0.1
0.1
0.2 ND
0.02
Reference
Laboratory
106 111
112
.
0.04
0.01
' ND
Material
No.
112
X Sr S XRSD
0.11
0.04 0.11 104.3
0.20
0.03 0.02 12.3
i
Summary Statistics
I Sr S *RSD
Day 1
Mean (cm/sec) X
Std. Deviation S
Variance S
Day 2
Mean (cm/sec) X
Std. Deviation S
Variance S
0.4 0.4 0.4 0.4
0.02 0.07
0.4 0.5 ND
0.03 0.05
ND
0.4
0.4
0.04 0.03 8.2
0.04 0.08 19.5
ND = No data reported
39
-------
Table 16. Phase II Results - Water Ext1ngu1shab1Hty Test
Test Material No. 3'- Cotton Fiber
Laboratory No. * Summary Statistics
DayJ.
Mean (cm/Sec)
Std. Deviation
Varianr.o
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
7
S2
Y
S
S2
102
3.4
0.4
0.1
2.9
0.4
0.2
106
7.6
0.6
0.4
2.5
2.6
6.8
111
1.9
0.5
0.3
1.9
0.4
0.2
112 X
4.8** 4.3
4.0**
16.4**
ND 2.4
Sr S *RSD
0.5 3.0 69.4
1.5 1.3 55.3
Reference Material
Laboratory No.
Summary Statistics
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
Y
S
S^
I
S
S2
102
3.7
0.4
0.2
2.9
0.2
0.05
106
4.2
-
-
2.8
0.3
0.07
111 , 112 2 Sr S %RSD
.
0.02 1.9 2.4
0.8 0.5 1.9 81.0
0.7
0.02 ND 1.9
0.2 1.9 100.0
** = Data rejected by Cochran's test
ND = No data reported
40
-------
Table 17. Phase II Results - Water ExUngu1shab1l1ty Test
Test Material No. 4 - Polyurethane Foam
.Laboratory No. Summary Statistics
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
Y
S2
Y
S2
Y
S
S2
Y
S
S2
106
2.2
0.6
0.3
111 112 X Sr S XRSD
2.4 5.3 3.3
1.1 '3.8 2.3 2.6 77.6
1.2 14.1
5.7 2.3 NO 4.0
0.2 0.7 0.5 2.4 61.0
0.04 0.5
106
4.1
0.8
0.6
5.0
2.9
8.6
Reference Material
Laboratory No. Summary Statistics
111 112 I Sr S XRSD
1.2 1.7 2.3
0.2 0.7 0.6 1.6 70.7
0.05 0.5
)
0.9 ND 2.9
0.05 ' 2.1 3.4 116.2
NO = No data reported
41
-------
Table 18. Phase II Results - Water Ext1ngu1shab1l1ty Test
Test Material No. 5 - Paint Waste
Laboratory No. Summary Statistics
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
7
S
7
s
S2
102
3.5
0.6
0.4
3.4
0.5
0.3
106
2.8
1.2
1.5
3.5
1.2
1.4
in
1.7
0.1
0.01
1.6
0.2
0.02
112
1.4
0.1
ND
X Sr S *RSD
2.3
0.7 1.1 49.2
2 8
0.8 1.3 44.8
Reference Material
i
Laboratory No.
Day 1
Mean (on/Sec)
Std. Deviation
Variance
Day!
Mean (on/Sec)
Std. Deviation
Variance
X
s
S2
I
S
S2
102
2.8
0.2
0.05
2.7
0.2
0.05
106
3.7
0.7
0.4
3.9
1.1
1.3
111
0.9
0.1
0.01
0.9
112
1.7
0.7
0.4
ND
Summary Statistics
X Sr S %RSD
2.3
0.5 1.3 56.3
2.5
0.5 1.6 62.6
ND = No data reported
tffia'iiii MJhiiit
-------
Table 19. Phase II Results - Water Ext1ngu1shab11ity Test
Test Material No. 6 - Waste 011
_^ Laboratory No. Summary Statistics
102
106
111
112
X
XRSD
Day 1
Mean (cm/Sec) I 4.9 ND ND ND 4.9
Std. Deviation S 0.8
Variance $2 0.6
Day 2
Mean (on/Sec) Y 2.8 ND ND ND 2.8
Std. Deviation S 0.7
Variance S2 0.4
Day^L
Mean (cm/Sec)
Std. Deviation
Variance
Day_2
Mean (cm/Sec)
Std. Deviation
Variance
X
S
S2
I
S
S2
102
4.2
1.1
1.1
2.4
0.2
0.03
Reference Material
Laboratory No. Summary Statistics
106 111 112 X Sr S XRSD
ND ND ND 4.2
* * *
ND ND ND 2.4
* * *
ND = No data reported
* = Value cannot be calculated from existing data
43
-------
Table 20. Phase II Results - Water Ext1ngu1shab1l1ty Test
Test Material No. 7 - Sand/011 Mixture
Laboratory No. Summary Statistics
Day 1
Mean (cm/ Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
y
S
S2
Y
S
S2
y
S
S2
y
S
S2
102
2.5
0.3
0.1
2.9
0.7
0.5
102
2.7
0.9
0.8
3.3
0.3
0.1
106 111 112 X Sr S *RSD
ND ND ND 2.5
* * *
i
ND ND ND 2.9
* * *
Reference Material
Laboratory No. Summary Statistics
106 111 112 X Sr S %RSD
ND ND ND 2.7
* * *
ND ND ND 3.3
* * *
,
ND = No data reported
* = Value cannot be calculated from existing data
44
-------
Table 21. Phase II Results - Water Ext1ngu1shab1l1ty Test
Test Material No. 8 - Waste Solvent
t
Laboratory No. Summary Statistics
Day j^
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (on/Sec)
Std. Deviation
Variance
y
S
S2
y
s
S2
Y
S
S2
"X
S
S2
102
7.6
1.1
1.3
6.7
0.9
0.8
102
3.3
0.6
0.3
2.6
1.1
1.1
1C6 111
NO 3.9
0.2
0.04
NO 3.7
0.2
0.03
Reference
Laboratory
106 111
ND 1.0
0.04
-
ND 0.9
0.01
112
3.1
0.7
0.5
ND
Material
No.
112
t
»
2.1
0.3
0.1
ND
Jt Sr S XRSD
4.9
0.8 2.5 50.8
5.2
0.6 2.2 41.9
Summary Statistics
X ST. S %RSD
2.1
0.4 1.2 56.9
1.7
0.7 1.3 78.3
ND = No data reported
45
-------
Table 22. Phase II Results - Water Ext1ngu1shab1l1ty Test
Test Material No. 9 - Sawdust/Kerosene
Laboratory No. Summary Statistics
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
7
S
S2
7
S
S2
102
3.6
1.0
1.1
3.5
0.7
0.5
106
2.6
0.5
0.2
2.2
0.6
0.3
111
3.3
1.8
3.2
3.0
1.0
1.1
Reference
Laboratory
Day 1
Mean (cm/Sec)
Std. Deviation
Variance
Day 2
Mean (cm/Sec)
Std. Deviation
Variance
X
S2
7
S
S2
102
2.5
0.2
0.03
3.1
0.3
0.1
106
3.2
0.6
0.3
3.2
1.0
1.0
111
1.0
0.05
0.9
0.05
112
1 1.2
0.13
NO
Material
No.
112
2.5
0.2
0.05
NO
1 Sr S XRSD
2.7
1.1 1.4 51.8
2.9
0.8 1.3 43.2
Summary Statistics
I Sr S %RSD
2.3
0.3 1.0 41.7
2.4
0.6 1.4 57.9
NO = No data reported
46
------- |