------- ------- 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 ------- 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. ------- 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 ------- |