Ainob 2booM fi R 83-2678

An Interlaboratory Evaluation of

the 1980 Version of the National

Bureau of Standards Test Method

for Assessing the Acute Inhalation

Toxicity of Combustion Products

U.S. DEPARTMENT OF COMMERCE

National Bureau of Standards

National Engineering Laboratory

Center for Fire Research

Washington, DC 20234

April 1983

Final Report

10G

.1156

83-2673

U.S. DEPARTMENT OF COMMERCE

NATIONAL BUREAU OF STANDARDS

NATIONAL I>»n>T k: or sTwDFAue

MAY 2 1983

/7 0~f C

C

£ C /OO

NBSIR 83-2678

AN INTERLABORATORY EVALUATION OF

THE 1980 VERSION OF THE NATIONAL

BUREAU OF STANDARDS TEST METHOD

FOR ASSESSING THE ACUTE INHALATION

TOXICITY OF COMBUSTION PRODUCTS

Barbara C. Levin, Maya Paabo, Merritt M. Birky

U.S. DEPARTMENT OF COMMERCE

National Bureau of Standards

National Engineering Laboratory

Center for Fire Research

Washington, DC 20234

April 1983

Final Report

U.S. DEPARTMENT OF COMMERCE, Malcolm Baldrige, Secretary

NATIONAL BUREAU OF STANDARDS, Ernest Ambler, Director

TABLE OF CONTENTS

Page

LIST OF FIGURES iv

LIST OF TABLES - v Abstract i

1.0 INTRODUCTION 2

2.0 THE NBS TOXICITY TEST METHOD 3

3.0 THE INTERLABORATORY EVALUATION OF THE 1980 TEST METHOD 6

4.0 VARIATION IN EQUIPMENT AND TECHNIQUES 7

4.1 Analytical Instrumentation 7 4.2 Furnace 8

4.3 Exposure Chamber 8

4.4 Animal Information 9

5.0 RESULTS AND DISCUSSION 10

5.1 Temperature Measurements 10

5.1.1 Autoignition Temperatures 10

5.1.2 Flaming and Non-flaming Temperatures 10

5.1.3 Chamber Temperatures 11

5.2 Chemical Measurements 13

5.2.1 Carbon Monoxide 13

5.2.2 Carbon Dioxide 16

5.2.3 Oxygen 16

5.2.4 Hydrogen Cyanide 17

5.3 Animal Measurements 18

5.3.1 Incapacitation 18

5.3.2 Lethality 20

5.3.3 Blood Measurements 21

6.0 SUMMARY 24

7.0 ACKNOWLEDGEMENTS 27

8.0 REFERENCES 27

iii
LIST OF FIGURES

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Page

1. Exposure chamber 29

2. Pyrolysis /combustion furnace 30

3. Animal restralner ...... 31

4. Exposure chamber with separate furnace. .... 32

5a & b. Autoignition temperatures determined for each

material by each laboratory

6a & b. Flaming temperatures determined for each material

by each laboratory

7a & b. Non-flaming temperatures determined for each

material by each laboratory

8. Chamber temperature at animal nose positions during

30 minute exposure to flaming wool and Douglas fir

9. Average carbon monoxide concentrations (ppm) from

Douglas fir decomposition as a function of the mass loading /chamber volume (mg/H). A. Non-flaming

results. B. Flaming results. Solid line:

Slope of all laboratory results. Dashed lines:

laboratories with greatest and smallest slopes

10. Carbon monoxide generation from Douglas fir

decomposed in the flaming mode in both a large

and small cup furnace (NBS data) . . .

11. Average hydrogen cyanide concentrations (ppm) from

the non-flaming decomposition of ABS as function of

the mass loading/chamber volume (mg/&) . . . .

12. Time-to-incapacitation vs mass loading/chamber

volume hyperbolas for Douglas fir in the non-flaming

mode from six laboratories . . .

13.

14.

Concentration-response curves resulting from animal

incapacitation, death within exposure (30 min) and

death both within and post-exposure (30 min +

14 days) from the thermal decomposition of wool

in the flaming mode

Determination of percent carboxyhemoglobin at

EC Prt , LC (30 min), and LC.q (30 min + 14 days)

blood values obtained at various mass

loadings. (NBS data from flaming red oak.) . .

, 50 from

33

34

35

36

37

38

39

40

41

42

iv
LIST OF TABLES

Page

Table 1. Laboratories that Participated In the

Interlaboratory Evaluation 43

Table 2. List of Materials 44

Table 3. Experimental Design of Interlaboratory Evaluation 45

Table 4a. Standard Laboratory Information 46

Table 4b. Standard Laboratory Information 47

Table 4c. Standard Laboratory Information 48

Table 5. Measurement Techniques for Carbon Monoxide, Carbon

Dioxide, and Oxygen 49

Table 6 . Modifications of the Experimental Procedure 50

Table 7. Autoignition, Flaming and Non- flaming Furnace

Temperatures 51

Table 8 . Toxicity of Modacrylic at Different Temperatures 52

Table 9. Maximum Chamber Temperatures Experienced by Animals 53

Table 10. Highest Average Chamber Temperatures Experienced by

Animals 54

Table 11. Carbon Monoxide Production Per Unit — 55 Chamber Volume

Table 12. Carbon Monoxide Production for Douglas Fir in the

Flaming Mode 57

Table 13. Carbon Monoxide Production for Douglas Fir in the

Non-Flaming Mode 58

Table 14. Laboratories Statistically Similar on Basis of "w"

Test on Carbon Monoxide Concentrations from Douglas Fir .... 59

Table 15. Maximum Average Carbon Dioxide Concentrations Produced

During Animal Exposure 60

Table 16. Carbon Dioxide Production Per Unit ——r ^— 61 Chamber Volume

Table 17. Minimum Average Oxygen Concentrations 63

Table 18. Average Hydrogen Cyanide Production for Nitrogen

Containing Materials Decomposed Under Flaming and

Non-Flaming Conditions, 64

Table 19. Hydrogen Cyanide Production Per Unit SS

, — 66 J J Chamber Volume

v
Pa$e

Table 20. Incapacitation Times After Exposure to Non-Flaming PVC .... 67

Table 21. Constants for Time-Concentration Hyperbodas (Y Q + R/X) . . . 68

Table 22. EC^q Values (mg/1) 69

Table 23. LC^q (30 minutes + 14 days) In mg/1 70

Table 24. Slopes of LC_

Q

, 30 min, + 14 days (95% confidence

limits of slope) 71

Table 25. Multiplication Factor Between Lowest and Highest LC_

Q Value for Each Material 73

Table 26. NBS Control Blood Values for Fischer 344 Rats 74

Table 27. Carbon Monoxide, Carboxyhemoglobin, and Hydrogen

Cyanide Concentrations at LC__ (30 minutes) and

EC^q (30 minutes). Mean Carboxyhemoglobin

Concentrations at Time of Incapacitation 75

Table 28. Distribution-free Sign Test on COHb Values at the LC

n (30 minutes + 14 days) 79

Table 29. Distribution-free Sign Test on COHb Values at the LC _ (30 minutes) 80

Table 30. Distribution-free Sign Test on COHb Values at EC,.g 81

Table 31. Distribution-free Sign Test on COHb Values at Time

of Incapacitation 82

vi
AN INTERLABORATORY EVALUATION OF THE 1980 VERSION OF THE NATIONAL BUREAU OF

STANDARDS TEST METHOD FOR ASSESSING THE ACUTE INHALATION TOXICITY OF

COMBUSTION PRODUCTS

Barbara C. Levin, Maya Paabo and Merritt M. Birky*

Abstract

Seven laboratories selected from academia, industry, and

government evaluated the 1980 version of the NBS test method for

assessing the toxicity of combustion products in order to determine the operability of the procedure and the reproducibility of

results across laboratories. The experimental design specified

that each laboratory was responsible for testing Douglas fir and

three other materials from a total of twelve natural and synthetic

materials. All laboratories were required to use similar exposure

and combustion systems, to measure the autoignition temperatures

of their materials, to determine the toxicity of the gaseous

products released by the materials under both flaming and nonflaming conditions, to monitor chamber environmental conditions

(temperatures, and oxygen, carbon monoxide, and carbon dioxide

concentrations), and to measure blood carboxyhemoglobin in the

test animals (rats). In addition, a few laboratories measured the

hydrogen cyanide generated from nitrogen-containing materials.

Toxicity was evaluated on the basis of incapacitation (hind-leg

flexion behavioral avoidance response) during the 30 minute exposure and of lethality during the exposure and 14 day post-exposure

observation period. The results of this interlaboratory evaluation were statistically analyzed and, in most cases, demonstrated

reproducible results across laboratories. Possible reasons for

any inconsistencies are discussed. Sensitive experimental factors

are identified and modifications to the test method which resulted

from the experimental data collected during the interlaboratory

evaluation are described.

Key words: carbon monoxide; carboxyhemoglobin; combustion; com- bustion products; hydrogen cyanide; inhalation; interlaboratory

evaluation; LC^q; test methods; toxicity.

*Current address: Birky Associates, Inc., Route 3, Box 497, Boonsboro,

MD 21713.

1
1.0 INTRODUCTION

The National Bureau of Standarda (NBS) hae been developing a small-scale

test to asaeas the acute Lnhalation toxicLty of combustion products from

materials thermally degraded under specified laboratory conditions. The need

for this test became apparent with the realization that the majority of fire

fatalities were due to smoke inhalation end not to burns. The dLetinct possibility that toxicants other than carbon monoxide might be present in the smoke

and could be contributing significantly to the lethal atmospheres provided an impetus to design a means to evaluate these toxic atmospheres using both

biological and chemical analyses.

The early studies at NBS were supported by the Products Research Committee (PRC) through a grants program designed to investigate the behavior of

cellular plastics in fires [1]. As a result of the PRC-supported research and

considerable input from an ad hoc working group (composed of members from

academia, industry, and government knowledgeable in fire and toxicological

problems), an early vers Lon of the test method was formulated in 1980

[appendLx A of reference 2] . This version is the basis of this report and

must be distinguished from the more recent 1982 version [3],

Nine laboratories agreed to participate Ln an interlaboratory evaluation

(ILE) of the 1980 test method to determine the reproducibility of the experimental results. This ILE differed from a typical round robin evaluation of a test procedure in that all the laboratories did not examine all the materials

at specified temperatures and concentrations. This decision was dictated by

the large number of test materials (twelve), the expense of the experiments,

the time necessary to test each material, and the toxicological nature of the

research. According to the experimental design, each participating laboratory

would examine three materials plus Douglas fir and each material would be

tested by at least three laboratories. (This initial design changed, however,

when two of the nine original laboratories decided not to participate in the

ILE.)

i

• Numbers in brackets refer to the literature references listed at the end of

this report.

2
In addition, as the ILE progressed, the experimental results were presented at meetings of the ad hoc working group to help solve issues pertaLning

to the methodology of the test. This continuous input of data resulted in

changes in the test method procedures. Thus the procedures being evaluated by

the ILE were subject to change throughout the duration of the testing. The

final result of the efforts of NBS, the ad hoc working group, and the ILE

participants is the 1982 NBS version of the toxicity test method [3]

.

The

present report describes the 1980 toxicity test method, the experimental

design and the results of the ILE, the statistical analysis on the reproducibility of the data across laboratories and the subsequent modifications of the

test method. When possible, this report also examines intralaboratory repeatability and sensitivity of the test method results to variations in experimental procedures and equipment.

2.0 THE NBS TOXICITY TEST METHOD

This test method was designed to assess the acute inhalation toxicity of

the combustion products of materials thermally decomposed under specified

laboratory conditions and was primarily intended for research and preliminary

screening purposes by product researchers and material manufacturers. This

test was not designed to address the problem of total toxic hazard which a fire produces or to which a specific material may contribute in a "real fire"

situation although it may provide one of the input factors necessary for such

a fire risk assessment. To predict the toxic hazard of a fire encompassing

many materials or the added contribution by any one material to that hazard,

additional factors must be considered. These factors include, among others,

the amount of material and its fire properties (ignitability , rate of heat

release, rate of flame spread, smoke generation, quantity of irritants present

In the smoke, configuration) and the environmental conditions (ventilation

conditions, presence of ignition sources, proximity of other combustibles,

volume of compartments to which the smoke may spread, presence of fire protection systems, and the type of occupancy of the building). For thLs report,

acute toxicity is defined as the harmful effects of a single short exposure

(30 minutes) to combustion products generated by the thermal degradation of

materials; toxic hazard is defined as the probability that a toxic atmosphere

will be produced and an injury will occur as a result of the combined effect

of the material's properties and environmental conditions.

3
A complete description of the 1980 version of thLs method whLch was the

subject of the interlaboratory evaluation may be found in appendix A of reference [2]

.

Briefly, the test method consists of three major components: (1) a combustion system, (2) a chemical analysis system, and (3) an animal exposure

system. The combustion system is a closed design in which all the combust Lon

products are generated in a furnace located directly below the 200 liter

rectangular exposure chamber (fig. 1) and are kept within the chamber except

for that volume which is transferred for chemical analysis and subsequently

returned. The cup furnace is similar to that designed by Potts and Lederer

(fig. 2) [4], Materials are thermally degraded at a furnace temperature 25°C

above the material's autoignition temperature (flaming mode), 25°C below its

autoignition temperature (non-flaming mode), and at 440°C, the temperature at

which Douglas fir (the reference material in the 1980 version of the test

method) was tested in the non-flaming mode. The 440°C temperature was not

used if the material's autoignition temperature was less than 490°C. The

autoignition temperature was determined separately for each material and was that furnace temperature which caused the material to ignite spontaneously

during the 30 minute exposure period. In an actual flaming exposure, ethanol

and/or an electric spark was used to ensure immediate flaming. The maximum

furnace temperature for any exposure was 800°C.

Before experiments, all test materials were conditioned for at least 48

hours in a room with 40-50 percent relative humidity and a temperature of

22-24°C. One piece samples were tested unless the material was supplied as pellets or a powder.

The combustion products were pumped from the chamber to analytical instruments which continuously measured the concentrations of carbon monoxide

(CO), carbon dioxide (CO

2 ), and oxygen (O2 ). After analysis, all products

were returned to the chamber. If continuous measurements were not possible,

atmospheric samples were to be measured every five minutes for CO, CO

2

, and

O

2

. In the 1980 test method, O

2 concentrations were not to fall below 18

percent. The temperature of the exposure chamber at the level of the animal's

noses was also to be monitored throughout the exposure and was not to exceed

35°C

.

4
The animals used for these experiments were male rats weLghing 200-300

grams and were observed for at least 10 days prior to testing to assure the

animals were healthy and acclimated to the laboratory conditions. In some laboratories, animals designated for blood analysis of carboxyhemoglobin

(COHb) underwent cannulation 24 hours before experiments; this procedure

Involves the surgical insertion of a cannula into the animal's femoral

artery [5] thereby allowing blood samples to be taken during the exposure.

The blood levels of COHb are indicative of the amount of carbon monoxide

inhaled by the animals. Six animals were exposed in each experiment. Each

animal was placed in a restrainer (fig. 3) which was then inserted into one of

the six port-holes located along the front of the exposure chamber such that

only the heads of the animals were exposed to the combustion atmosphere.

Exposures were for 30 minutes, during which time blood was taken from the

cannulated animals (one or two animals were cannulated). If no animals were cannulated, one or two animals were removed at the time of incapacitation or at the end of the exposure to obtain blood samples.

The biological endpoints examined were incapacitation and lethality.

Incapacitation was measured by the hind-leg flexion conditioned avoidance

response test developed by Packham et al. [6]. The time-to-incapacitat Lon of

each of the six animals in each experiment was noted and the mean and standard

deviation of those times were calculated for each mass loading. In addition,

the EC^q [mass loading of material per unit chamber volume (mg/ Z) that caused

50 percent of the animals to become incapacitated in the 30 minute exposure]

was determined. The lethality endpoint required by the proposed test method

was the LCcjq for 30 minutes plus 14 days [the mass loading of material per

unit chamber volume (mg / Z) which was necessary to cause 50 percent of the

animals to die during the 30 minute exposure plus a 14 day post-exposure

observation period]. In addition, the LC^q for the 30 minute exposure period

was also calculated when enough data were available. Both the EC^q's and

^^50 s ’ their 95 percent confidence limits, and the slopes of the concentration-response curves were calculated via the statistical method of Litchfield

and Wilcoxon [7], (Concentration, when indicating the total amount of combustion products generated during an experiment, is defined as the mass loading

of material per unit volume of exposure chamber.)

5
3.0 THE INTERLABORATORY EVALUATION OF THE 1980 TEST METHOD

The purpose of the ILE was to determine the reproducibility of the test

results from different laboratories. In addition, the III helped refine the

necessary conditions of the test. Nine laboratories Initially agreed to

follow the 1980 test procedure and to determine or to monLtor the following

parameters) the autolgnltlon temperature of each required material; the

temperatures generated In the cup furnace and In the animal exposure chamber;

the CO, CO

2

, and 0

2 concentrations generated during each material's decomposition In the flaming and non-flaming modes and, If conditions warranted, at

H0°C; t Lme-to-incapac ItatLon of each animal exposed and the mean and standard

deviation of the tlme-to-incapacltat Lon for all six animals used at each mass loading; the number of animals Incapacitated or killed during the exposure at

each mass loadLng and the number who died during the 14 day post-exposure

observation period; and the COHb at Incapacitation and at the end of each 30

minute experiment. Enough experiments were to be performed to allow an ec50

for the 30 minute exposure and an LCjq for the 30 minute exposure plus the 14

day post-exposure observation period to be statistically calculated by NBS

from the data. The paper by Litchfield and Wllcoxon [7] describes the procedure for calculating the LCjq values. (Formulas from the appendix of the

Litchfield and Wllcoxon paper were used instead of the nomographs Included in

the text.)

The seven partLcLpants in the ILE are listed alphabetically in table 1. Each laboratory was assigned an Identification number whLch will be used

throughout this report and in tables of results. These numbers do not correspond to the order of the laboratories given in table 1. Twelve materials,

both synthetic and natural and having a broad range of thermal and toxicological properties, were chosen for this study. The list of materials and the

abbreviations used throughout this paper are shown in table 2. A common stock

of materials was collected, stored, and sent to the participants

by NBS. The detailed composition of each of the polymers and co-polymers was

not available. Assemblages of non-uniform structure, such as carpets or layered wall materials, were not tested in this ILE.

6
The statistical design of the ILE was generated by one of the participating laboratories by randomly numbering each material (1 to 12) and each

laboratory (1 to 9) and then selecting three materials which were assigned at

random to a laboratory for study. In addition, each laboratory experimental

design is shown in table 3. When two laboratories (7 and 9) withdrew, the

design was changed. Some of the other laboratories agreed to study additional

materials and NBS agreed to examine all twelve. These changes are noted in

table 3 by the letter A representing additional materials, and N.D. representing not done. The ultimate result was that laboratories 1 and 8 tested four

materials, laboratories 3 and 5 tested five materials, laboratory 2 evaluated

six materials, laboratory 4 studied seven and laboratory 6 (NBS) evaluated all

twelve. Thus all materials except poly(vinyl chloride) (PVC) were examined by

at least three laboratories; PVC was studied by only two.

All participants were required to complete standardized data sheets for

each material in each temperature mode (tables 4a, 4b, 4c). All data sheets were sent to NBS for analysis.

4.0 VARIATION IN EQUIPMENT AND TECHNIQUES

Although all participants were requested to follow the 1980 test method

as outlined in section 2.0, certain options were left to the discretion of the

investigators, for example, the type of analytical equipment, the rat strain,

the animal restrainer material, and the method of blood sampling. Other

items, although specified, were still varied by some of the laboratories.

These differences are summarized in tables 5 and 6 and will be discussed Ln the following sections.

4.1 Analytical Instrumentation

The 1980 test method required the continuous or intermittent (every 5 minutes) measurement of CO, CO

2

, and O

2

. For CO and CO

2

, five laboratories

(1, 2, 4, 5, and 6) used continuous flow nondispersive infrared analyzers

which monitor the absorption of specific wavelengths characteristic of the

chemical species of interest (table 5). Two laboratories (3 and 8) made

intermittent measurements using gas chromatographs equipped wLth thermal

7
conductivity detector*. Oxygen measurement* were performed with paramagnetic

(laboratory 1), polarographic (laboratories 2, 5, and 8), galvanic (laboratories 4 and 6), and chromatographic (laboratory 3) techniques.

Although the test method did not require the determination of hydrogen

cyanide (HCN), three laboratories (1, 3, and 6) volunteered to measure HCN in

the combustion atmospheres of those ILE materials containing nitrogen. Laboratories 3 and 6 analyzed HCN with a gas chromatograph equipped with a thermionic detector [8]. Laboratory 1 used a specific ion electrode.

4.2 Furnace

All laboratories were to use a cup style furnace based on the design of

Potts and Lederer [4]. In this system, a quartz beaker with a thermocouple

well was surrounded by ceramic with recessed heating elements, all of which

was encased in a galvanized steel box (fig. 2). The quartz beaker in which

the sample was degraded was heated to a predetermined temperature which was monitored by a temperature controller. The materials were degraded by a combination of convective, conductive, and radiant heat.

In the ILE, the furnaces were made by the participants and the sizes of

both the furnaces and quartz cups differed to some degree (table 6). Most of

the laboratories used a cup of approximately 300 mil volume; however, lab 6 (NBS) also tested a cup furnace with a capacity three times greater

(954 mil) and laboratory 8's cup was much smaller than the others with a capacity of only 79 mil . The two cup sizes used by NBS are designated 6a

(362 m&) and 6b (954 mil) in the tables of results.

4.3 Exposure Chamber

The exposure chambers of all the laboratories except laboratory 8 were based on the design shown in figure 1 and had a volume of approximately 200

liters (table 6). The exposure chamber of laboratory 8 was separated from the

furnace and is shown in figure 4. This figure also shows rotating cages which were present but not used in this ILE.

8
4.4 Animal Information

The information pertaining to the animals is summarized in table 6. All

laboratories exposed male rats to the combustion atmospheres in a head-only

mode, not whole body. The strain of rat varied; four laboratories used

Sprague-Dawley , three laboratories used Fischer 344, and one laboratory used

Long-Evans. The animals upon receipt from the supplier were between 2 and 4

months of age and were allowed to acclimate to laboratory conditions for 7-14

days before testing. All laboratories except 8 exposed six animals per test

(at each mass loading); laboratory 8 exposed only three, but repeated each

exposure four times—twice for lethality measurements and twice for incapacitation measurements.

Laboratory 3 cannulated three animals and laboratory 6 cannulated two

animals per test in order to sample blood during the exposure without removing

the animals from the combustion atmosphere. Laboratory 5 cannulated one or two animals occasionally. Laboratory 3 kept the cannulated animals throughout

the 14 day post-exposure observation period, but laboratory 6 sacrificed the

cannulated animals after the 30 minute exposure and only kept the non-cannulated animals for post-exposure observation. The other laboratories (1, 2, 4,

and 8) removed their animals from the chamber and obtained blood via cardiac

puncture (with and without open chest) or intraorbital venous puncture. A co- oximeter was used by all laboratories to analyze the percent carboxyhemoglobin

present in the blood.

For testing, animals were placed in aluminum (laboratories 2, 5, 6) or plastic restrainers (laboratories 1, 3, 4, 8) which were inserted into the

port-holes along the front of the chamber (fig. 1) such that only the animals'

heads were exposed to the combustion atmosphere. The animals were observed

for both time-to-incapacitation and death. Incapacitation was measured by the

hind-leg flexion conditioned avoidance behavioral model [6] in which wires are attached to one of the hind legs of the rat such that the animal receives an electrical shock whenever the foot touches a metal plate located below the

animal. The shock current varied among the laboratories from 1-3 ma to about

13 ma (table 6). The animals learned rapidly (approximately 15 min) prior to

the test not to touch the plate and were considered incapacitated when they

9
failed to respond to the shock. Laboratory 3's electrical circuitry waa designed such that after an animal became incapacitated and the electric Lty to

that animal was shut off, the electrical current to the rest of the animals

increased.

5.0

RESULTS AND DISCUSSION

5.1 Temperature Measurements

5.1.1 AutoLgnition Temperatures

Each laboratory was responsible for independently determining the autoLgnitLon temperature of each of their designated materials plus Douglas fir.

The temperatures found by the laboratories are summarized in table 7 and

illustrated in figures 5a and 5b. The solid black part at the top of the bars

in these figures indicates the intralaboratory variability (low and high

values) in the autoignition temperature data. Part of this variability waB

attributed to the initLal determination of the autoignition temperature with

relatively small sample sizes. In the course of the non-flaming experiments

(25°C below the autoLgnition temperature), larger sample sizes sometimes

underwent an exothermic reaction which caused the sample to ignite. Consequently, both the autoignition temperature and the non-flaming temperature were lowered. Laboratory 4 did not submit autoignition temperatures for most

of their materials and the missing values were .estimated by calculating the

mean values between the highest non-flaming temperature and the lowest flaming

temperature reported (table 7 and figures 5a and b)

Good agreement among the laboratories is seen by the small scatter of

data around the mean of the autoLgnition temperature for each material

(table 7). Most of the standard deviations ranged between 12 and 35°C; only

polystyrene had a standard deviation which exceeded these values.

5.1.2 Flaming and Non-flaming Temperatures

Once the autoLgnition temperature of a material was determined, experiments were to be conducted 25°C above (flaming mode) and 25°C below this

temperature (non-flaming mode). If this requirement were followed rigorously,

10
there would be no need to report the flaming and non-flaming temperatures.

This information is provided, however, because some of the laboratories did

not perform their experiments on any one material at a constant temperature

and, in some cases, they did not adhere to the 25°C requirement. The flaming

temperatures are listed in table 7 and figures 6a and 6b. The non-flaming

temperatures are in table 7 and figures 7a and 7b. The black part of each bar

in these figures indicates the range of temperatures that a laboratory used in

the examination of any one material (their intralaboratory variability).

The variation in methodology between laboratories was used to evaluate

the sensitivity of the results to furnace temperature. For example, the

auto Ignition temperature of acrylonitrile butadiene styrene (ABS) was determined to be 555°C by laboratory 3 and to be 500°C by laboratory 5. Both of

these laboratories then used flaming temperatures of between 694°C and 723°C

disregarding the specification of the test method to do flaming experiments

25°C above the autoignition temperature. However, the LC^q results from these

laboratories for flaming ABS are not significantly different from the other

two laboratories who did follow the specification. On the other hand, data

from laboratory 4 showed that in the non-flaming mode the LC^q values for

modacrylic decreased as the furnace temperature approached the autoignition

temperature, indicating the non-flaming mode results may be more sensitive to

furnace temperature (table 8).

5.1.3 Chamber Temperatures

To minimize the effects of heat stress on the animals, the 1980 test

method recommended that the temperature of the exposure box not exceed 35°C at

any time during the 30 minute exposure period. Temperatures were measured

close to the animals' noses and also in the middle of the exposure chamber.

Both average and maximum temperatures were reported for the 30 minute period

for each experiment.

Preliminary analysis of the data indicated that the temperatures measured

in the vicinity of the animals' noses were usually lower than those measured

in the middle of the exposure chamber. Therefore, to estimate the heat stress

that the animals experienced at any time, only the temperature readings near

11
Che animals' noses were considered. The highest nose temperature during the

30 minute exposure period for each material over the mass loading range

studied was reported to NBS and is listed In table 9.

These data Indicated that a maximum nose temperature of 3S°C as specified

in the proposed test method was exceeded for many materials. In the flaming

mode, examination of the maximum nose temperatures showed results above this

specified limit in 23 out of 29 sets of experiments. In the non-flaming mode,

the maximum temperature rose above 35°C in 13 out of 27 sets of experiments.

The worst case, a maximum temperature of 109°C, was observed by laboratory 6 (NBS) during the decomposition of 41 mg/i. of wool in the flaming mode. In

this experiment, 50 percent of the exposed animals died. Another wool experiment at a lower mass loading (22 mg /l) had a very similar temperature profile,

but no animals died (fig. 8). These results indicated that temperatures of

this magnitude for short durations do not necessarily produce enough heat

stress to cause death of animals exposed in a head-only mode.

Instead of the maximum temperature, the average temperature over the

exposure time may be a better indicator of the total heat stress experienced

by the animal. Table 10 shows the highest average nose temperature found

during the flaming and non-flaming decomposition of each material by each

laboratory. It was on the basis of these data that the specified upper limit

of 35°C at any time during the exposure was changed to an average temperature

llmLt of 40°C. Only three values out of 77 exceeded this limit and one of

these values is suspect as the non-flaming average nose temperature was greater than the average flaming temperature, a situation unlikely to occur.

It is not clear from this study what temperature level or exposure time

is necessary before the head-only exposed animals will show visual or physiological effects of heat stress. It is also not known what temperature level

Ls needed to produce additive or synergistic effects with the toxicants that

also are likely to be present. *

12
5.2 Chemical Measurements

The 1980 vers Lon of the test method [2] required the continuous or Intermittent measurement of CO, CO2 , and O

2 in the exposure chamber atmosphere

during the thermal degradation of materials. In addition, HCN was measured by some laboratories if a nitrogen-containing material was tested. In this

study, the average concentration of a chemical species for any one mass loading of material (one experiment) was obtained by integrating the area

under the instrument response curve and dividing by the duration of the experiment, 30 minutes.

5.2.1 Carbon Monoxide

CO concentrations generated by the thermal decomposition of each material

except polytetraf luoroethylene (PTFE) were measured. The CO in the combustion

products from PTFE was not routinely measured in order to avoid possible

instrument damage by fluorides. Laboratories 1 and 4, however, measured the

concentration of CO in a few PTFE experiments and found that the average

concentration over the 30 minute exposure was never greater than 60 ppm.

To compare the results from various laboratories, the average concentration of CO generated over the 30 minute experiments was plotted against the mass loading of material per unit chamber volume (mg/Jl). The slopes of the curve for each laboratory were calculated by a least squares linear regression

analysis.

Douglas fir results are shown in figure 9A (non-flaming mode) and figure

9B (flaming mode), in which the dashed lines indicate the laboratories with

the greatest and smallest slopes, and the solid line is the slope of results

from all the laboratories. The production of CO in the non-flaming mode was proportional to the mass of material loaded into the cup furnace up

to 30 mg/il. When the sample loading was greater than 30 mg/Jl (for the 200

liter chamber, this is a 6 gram sample), the increase in CO with increasing mass was no longer linear. This lack of linearity was also noted for flaming

Douglas fir when the mass loading per the chamber volume exceeded

50 mg/Jl (fig. 9B). This occurrence was attributed to the inability of the cup

13
furnace to decompose the large mass of material In the allotted tLme. (Note,

however, that this overload was not vLsually apparent as this mass of material

fits easily Into the cup.) An Increase In the size of the cup furnace

to 954 mi. did not correct this problem. Concentrations of CO from mass loadings of Douglas fir above 30 mg/i. (non-flaming) and 50 mg /

i

(flaming) were

not Included In the determination of slopes via least square linear regression

analysis or in the statistical analysis as presented below. No such

overloading of the cup was observed for the other materials examined during

this study.

Within the limits of the cup heating capability as noted above, the CO

production is proportional to the mass loading/chamber volume. Consequently,

the statistical analysis of the CO data across laboratories was performed on

CO concentrations averagea over the 30 minute exposure and normalized to the mass of material loaded into the cup furnace divided by the chamber volume:

This normalization enabled the comparison of data from different laboratories

even when materials were tested at different mass loadings. Each laboratory's

mean values and standard deviations of the ratios of average CO (ppm) to mass loading/chamber volume (mg/i.) for each material except Douglas fir are shown

in table 11. Douglas fir results are presented along with the data used to

calculate the means and standard deviations in tables 12 and 13.

To facilitate comparisons of results between a pair of laboratories

chosen from the participating laboratories, an interval "w" was computed such

that any two laboratory results may be considered (1) similar if the absolute

difference between means is less than "w" or (2) not similar if the absolute

difference between means exceeds "w". The "w" statistic was computed as shown

in table 14 following the procedure in section 3.4 of reference [9], and uses

the within-laboratory precision as a measure to compare differences of means

2 among laboratories.

As all the laboratories examined Douglas fir, the "w" values for the

Douglas fir CO results were computed and those laboratories with similar and

average CO over 30 minutes

mass loading/chamber volume

14
dissimilar results were determined (table 14). More similarity was seen Ln

the non-flaming mode in which only the results from laboratory 8 were different from laboratories 2, 3, 5, 6a and 6b. All the other laboratories

showed no significant differences in their CO results. Although laboratory 8 was similar to laboratories 1 and 4, the reason that its values were significantly different from most of the other laboratories is likely related to its

very different exposure chamber and combustion furnace (fig. 4 and table 6).

The results of the flaming mode tests showed that most of the laboratories

were statistically similar with at least three other laboratories. Laboratory

3, however, was statistically different from all the other laboratories. The

reason for this difference is not clear, however, it should be noted that the

better intralaboratory precision for the flaming mode resulted in a smaller

"w" value and thus a more stringent interlaboratory comparison which indicated more dissimilarities.

One of the factors which could influence the material decomposition and

CO generation is the size of the cup furnace. As noted in table 6, most

laboratories had cup volumes of approximately 300 mil (236 - 362 mJl). Laboratory 8 used a 79 raJl cup and laboratory 6 (NBS) used a 954 mil cup in addition

to their 362 mil cup. Figure 10 shows the NBS results on CO generation from

flaming Douglas fir in both the small and large cup furnaces. When the

average CO generated over the 30 minute experiments was plotted against the

mass loading/chamber volume, the larger furnace results had a slope that was

12 percent steeper than the smaller furnace results irrespective of whether

the material was degraded in the flaming mode or non-flaming mode. As the

within-laboratory variation in CO generation from Douglas fir [as indicated by

the relative standard deviations (tables 12 and 13)] ranged from 6-26% in the

flaming mode and from 6-34% in the non-flaming mode, a 12 percent difference

in slope due to the cup furnace size is probably not significant. Since the

larger cup can accommodate larger samples of low density materials, the recommended size of the cup furnace was increased from 300 mil to 1000 mJl.

o We note that a number of assumptions underlying this comparison procedure may

not be fulfilled, namely: the presence of outliers, unequal number of test

results, and unequal variances. Dunnett [10, 11] treats unequal sample sizes

and unequal variances, but the presence of outliers still poses a different

problem.

15
5.2.2 Carbon Dioxide

CO

2 is produced during the combustion of all organic materials, and the

ratio of CO/CO2 is one indicator of the completeness of combustion. Toxicologically, CO 2 is not lethal until the concentrations reach 12 percent (120000

ppm) [12], levels far greater than those observed during this study. The

maximum average levels of CO2 generated over 30 minutes from each material

observed by a laboratory and the respective mass loadings are shown in table

15. However, CO

2 does act at lower concentrations (1.8 percent or 18000 ppm)

to stimulate the respiratory center of the brain causing increased respiratory

rates and thus acts to increase the rate at which other toxic gases are inhaled. It is important to note that the measured concentrations of CO2 are

a result of both material combustion and animal respiration in addition to the

CO

2 content already present in ambient air. In experiments at NBS, the normal

respiration of six rats placed in the closed exposure chamber for 30 minutes

(with no combustion) produced an average concentration of 2900 ppm of CO2 and

a maximum concentration of 6900 ppm. These results, however, could not be

used as control values to determine the CO

2 from only the material decomposition as the animals' respiratory rates were also dependent upon which material

was burned and the other toxicants present.

For the above reasons, statistical analyses were not performed on the CO

2 data. The average values of CO2 were calculated over the 30 minute exposure

time and normalized to the mass loading per unit chamber volume. The mean and

standard deviations of all the normalized values for a material in a particular mode (flaming or non-flaming) found by each laboratory are tabulated in

table 16.

5.2.3 Oxygen

Both the material combustion and the animal respiration rate will reduce

the oxygen levels in the animal exposure chamber. To prevent the compounding

of the toxicity information with possible O

2 deprivation effects, the 1980

method specified that the O

2 concentration not fall below 18 percent. The

average percent O

2 over the 30 minute exposures and the minimum percent O

2 were determined by the ILE participants and reported to NBS. Preliminary

16
analysLs of the data showed that the average concentration was a better

Indicator of O

2 deficiency than the lowest O

2 reading. In other words, an individual reading does not accurately represent the concentration that the

animal experiences over the 30 minute exposure.

The minimum average O

2 concentrations from each laboratory for each of

their respective materials are summarized in table 17. In the non-flaming

mode and at 440°C, only two sets of data out of 58 fell below 18 percent and

those two were 17.5 percent. In the flaming mode, on the other hand, 17 sets

of data out of 39 were below 18 percent. However, only one value (14.2

percent for flexible polyurethane) was below 16 percent. Recent studies by

Mat t jak-Schaper and Alarie [13] indicated that O

2 levels could fall as low as 10 percent before the respiratory rate of their experimental animals (mice)

showed a slight decrease; therefore, the requirement of maintaining the O

2 level at no lower than 18 percent in the exposure chamber was changed in the

1982 test method [3] to an average concentration of no lower than 16 percent.

5.2.4 Hydrogen Cyanide

The determination of HCN concentrations was not required by the 1980

method. However, three laboratories (1, 3, and 6) did measure the HCN concen

trations generated by the thermal decomposition of the nitrogen-containing

materials [ABS, flexible polyurethane, modacrylic, poly(vinyl chloride) with

zinc ferrocyanide, rigid polyurethane, and wool]. Not all of the three laboratories, however, measured HCN from all six materials in all three modes

(flaming, non-flaming and 440°C). Table 18 shows the average concentrations

of HCN at each mass loading.

The generation of HCN was found to be proportional to the mass loading

per unit chamber volume (mg/&). The results for non-flaming ABS are shown in

figure 11. To compare the other material results from the three laboratories

the HCN concentrations were normalized to the mass loadings/chamber volume

(table 19). Although a statistical analysis of the results was not performed

due to the limited amount of data, visual inspection shows reproducibility to

within a factor of 2.5 as measured by the ratio of the maximum value to the

minimum value.

17
5.3 Animal Measurements

5.3.1 Incapacitat Lon

The biological endpoints examined in this ILE were incapacitation of the

animals during the 30 minute exposure and death during the 30 minute exposure

and 14 day post-exposure observation period. The experimental results on incapacitation provided by the ILE participants were analyzed on the basis of

both t Lme-to-incapacitat ion and the numbers of animals incapacitated at each mass loading in order to determine an EC^q [mass loading/chamber volume (mg/ l)

necessary to cause 50 percent of the animals to become incapacitated in the 30

minute exposure]. All ILE participants used the hind-leg flexion conditioned

avoidance response as the behavioral model for incapacitation [6].

Time-to-incapacitation can be examined in two ways. In the first, the mass loading of material is kept constant and the times-to-incapacitation of

each of the six exposed animals are measured during each experiment which

lasts until all animals are incapacitated. In this manner, the mean time-toincapac Ltation could be compared for the same mass loading of materials. This

procedure worked better for some materials than for others. Those materials

whose combustion products caused post-exposure deaths rather than withinexposure deaths produced extremely variable results when examined by this

method. Poly (vinyl chloride) is an example of such a material. Upon thermal

decomposition, PVC produces HCJl, a potent toxicant and highly irrLtating acid

gas. The irritating effects of the combustion products from this material are

so Intense that the animals temporarily fail to react to the shock. This

seemingly incapacitated state will recur repeatedly during the exposure.

Within the same experiment the actual time of incapacitation varied widely

(table 20) and some animals died before others were incapacitated. Other

materials, mainly those which produced within exposure effects, showed good

repeatable results with this method.

In the second procedure, the exposure duration is set (for example, at 30

minutes) and the mean and standard deviation of the time-to-incapacitat Lon for

the exposed animals is calculated for different mass loadings of material.

The lower the mass loading, the more time needed to incapacitate the

18
animals. These poLnts were represented by a function which asymptotically

approaches a threshold time-to-incapacitation on one axis and a concentration

of material needed to produce incapacitation in the specified time limit on the other axis.

The mean times-to-incapacitation that were obtained in each mode were

used to best fit a hyperbolic curve (Y = Q + R/X). Six examples of these

hyperbolic curves for Douglas fir in the non-flaming mode are shown in

figure 12. The hyperbolic equations are shown on each graph. Similar timeconcentration hyperbolas were generated for all the materials in both flaming

and non-flaming modes from the NBS data and that supplied to NBS by the other

laboratories. The Q and R coefficients calculated for each material in each

mode from all the laboratories are presented in table 21. Visual inspection

and comparison of the coefficients indicate the differences between the curves. The problems that arise with the use of the hyperbolic curves for the

analysis of relative toxicity of the combustion products of materials are:

(1) differences in time-to-incapacitation of 5-10 minutes are equivalent to

16-30% of the total 30 minute time frame, i.e. , substantial experimental

scatter is inevitable, (2) the 30 minute exposure time limits the number of

data points at lower mass loadings (where less than six animals are incapacitated), and (3) comparison of the various curves to determine relative

toxicity of materials is difficult.

Another means of analyzing the incapacitation data is to determine the

EC^q. The percent of animals incapacitated at each mass loading tested is

plotted on logarithmic probability paper to obtain a concentration-response

curve. The EC^q's and their 95% confidence limits were statistically determined by NBS for all the materials in both the flaming and non-flaming modes

by the method of Litchfield and WLlcoxon [7], In some cases, however, a small

change in concentration (e.g., 0.5 mg/A) would cause the number of animals

incapacitated to change from 0% to 100%. In these cases, the EC^q was obtained graphically from a plot of the data in which successive data points were connected by straight line segments (fig. 13). Whenever a value was estimated by this latter method, the approximate sign (~) is placed before

that value and the extremes used to obtain that value are placed in

brackets. Table 22 shows the EC^q values (those statistically determined and

those approximated) with their 95% confidence limits in parenthesis.

19
As a result of the analysis of the data provided by the ILE participants,

Incapacitation (as evaluated on the basis of the hind-leg flexion behavioral

model) was found to provide less toxicological information (did not detect

materials which caused post-exposure effects), was a less sensitive Indicator

of acute toxicity (false positives were noted with smoke containing high

concentrations of irritants) and was a more difficult procedure to measure practically than the biological endpoint of lethality. Additional incapacitation results and a detailed explanation for excluding the incapacitation

endpoint from the 1982 test method are provided in reference [3]

.

5.3.2 Lethality

The assessment of the acute inhalation toxicity of combustion products in

the 1980 version of the test method is based on the determination of a statistically calculated LC^q [the mass loading of material/chamber volume (mg/Jl)

necessary to cause 50 percent of the test animals to die within the 30 minute

exposure and/or 14 day post-exposure observation period]. Briefly, the determination of an LC^q is as follows: Six animals are exposed to the combustion

products from a specific mass loading of material and the percent of animals

which respond in the set time period are noted. A new set of animals are then

exposed to a higher or lower mass loading in order to generate a concentration-response curve in which the percent deaths are plotted as a function of

the amount of material loaded into the furnace (fig. 13). This concentrat Lonresponse curve provides a means of estimating the LC^q. The actual

statistical determinations of the LC^q's and the slopes of the concentrationresponse curves from the data provided by the ILE laboratories were carried

out at NBS according to the method of Litchfield and Wilcoxon [7]. Table 23

shows the LC^q values and their 95 percent confidence limits calculated for

the 30 minute exposure and 14 day post-exposure observation period from the

data provLded by all the laboratories. Table 24 shows the concentrationresponse slopes for the same data. The 95% confidence limits shown in tables

23 and 24 are indicative of the intralaboratory variability. Visual

inspection of the LC^q values listed in table 23 shows the reproducibility

between laboratories for each material in each mode is within a factor of two

except for PTFE and PPS in both the flaming and non-flaming modes and wool in

the flaming mode (table 25).

20
No laboratory found the LC^q (30 minutes and 14 day) values determined at

the 440°C furnace temperature to be lower than the lowest LC^q value determined in either the flaming or non-flaming mode. As the test method is designed

to evaluate materials under their most toxic conditions, the 440°C temperature

mode was made optional in the 1982 version of the test method [3]

.

The sensitivity of the LC^q values to the cup furnace size was examined.

Complete concentration-response curves were generated by NBS, and separate

LC^q (30 minutes and 14 day) values were calculated for Douglas fir decomposed

in the NBS large furnace (954 m£) and the NBS small furnace (362 mA). The

flaming and non-flaming results are shown in table 23 under the material

heading Douglas fir and laboratory numbers 6a (small furnace) and 6b (large

furnace). Visual inspection of these LC^q values and their 95% confidence

limits indicates that these values were not sensitive to the different size

cup furnaces tested by NBS.

I 5.3.3 Blood Measurements

Each laboratory participating in the ILE measured both carbon monoxide

levels in the exposure chamber atmosphere and blood carboxyhemoglobin (COHb)

in each test. If the animals were cannulated as described earlier (section

2.0), arterial blood could be sampled during the exposure without removing the

rats from the exposure chamber. If the rats were not cannulated, they were removed from the chamber before sampling. Those laboratories who did or did

not routinely use cannulated animals are identified in section 4.4.

A great amount of blood data was generated during this study. Table 26

shows the blood parameters measured by NBS and the mean and standard deviations determined in 138 - 180 control animals. This table provides an indication of the intralaboratory precision of one of the laboratories, namely

NBS, in the determination of these values. (A more extensive evaluation of

the blood measurements will be published by NBS in a separate report.) For

the purposes of this report, the blood values of interest were the COHb values

determined at the biological endpoints of incapacitation and death. There

were two reasons for this interest: (1) to determine if the values were reproducible across laboratories and (2) to examine the COHb levels in order

21
to assess whether carbon monoxide was the principal toxicant responsible for

the death of the animals. This latter reason is the primary purpose for

Including the COHb measurements in the test method*

Table 27 shows the COHb levels and corresponding average concentrations

of CO calculated for each material examined by each laboratory at two bLological endpointsi (1) the LCjq (30 minutes) , and (2) the EC^q (30 minutes).

The LC^q for 30 minutes is used here since all the blood samples were taken at

the end of the 30 minute exposure and the COHb values are related to the

average CO concentration to which the animals are exposed over the 30 minutes.

In addition, the COHb levels determined at the time of incapacitation are also

provided in table 27. To determine the percent COHb at the LC^q and EC^q, the

COHb values that were obtained at the end of each exposure were plotted

against the mass loading of material/chamber volume (mg/A). The LC^q and IC^q

values were superimposed upon the graph and the percent COHb at that mass loading was determined (fig. 14). To determine the percent COHb at the time

of incapacitation, the mean and standard deviation of the percent COHb at the

time of incapacitation for each material was calculated utilising all values

of COHb obtained from one laboratory at Incapacitation regardless of mass loading. The mass loading would change the actual time of incapacitation, but

the percent COHb at incapacitation should theoretically remain constant. The

difference between the percent COHb at the EC^q and the percent COHb at the

time of incapacitation ia that the former is calculated from blood taken at

the end of the exposure at the mass loading which causes 50% of the anLmals to

be incapacitated. The latter is the mean of the actual percent COHb calculated from blood taken from animals as soon as possible after the animal

became incapacitated, although there is always a time lag during whLch the

COHb levels will Increase if the animal is not removed from the exposure

atmosphere or decrease if the animals are removed.

A distribution-free statistical test (the sign test) was performed on the

COHb values for all the laboratories to determine if any laboratory's results

were consistently lower or higher than the overall mean results [14]. In table

28 (LC^q, 30 minutes + 14 days), table 29 (LCjq, 30 minutes), table 30 (EC^q),

and table 31 (time-to-incapacltation) , the mean COHb value for all the laboratories for a particular material in one mode was subtracted from the value

22
obtained by each laboratory. When the value from an individual laboratory was lower than the mean, the difference is listed as a negative value and when the

laboratory value was higher than the mean, the difference is listed as a positive value. One can now check how many times a laboratory had negative

versus positive numbers and how many times a laboratory had the lowest value

or the highest value. The results of this statistical sign test on COHb at

the LC^q (30 minutes + 14 days) and LC^q (30 minutes) are shown on the bottom

of tables 28 and 29, respectively. These tables show that laboratories 1 and

4 were frequently lower than the mean; whereas laboratories 3 and 6 were frequently higher than the mean. (In these two tables, only laboratory 6b's

results are statistically significant at the 5% level. However, in many

cases, the split between the number of negative effects and positive effects

was not sufficient to evaluate for significance, i.e., at least a 0/6 split

was necessary.)

These results reflect the method of obtaining blood. Those laboratories

that took blood via cannulated animals without removing the animals from the

smoke atmosphere had values that were higher than the mean. Those laboratories that never cannulated but rather removed their animals from the

exposure chamber to obtain blood had COHb values that were lower than the mean. Post-exposure recovery rates from pure CO exposures in rats is very

rapid (NBS data, to be published). At these high COHb levels, the COHb drops

50% in 15 minutes, which indicates that a Short delay in obtaining the blood

samples after removal of the animal from the exposure chamber will produce low

values.

A similar evaluation of the incapacitation data (bottom of tables 30 and

31) does not show a relationship with the method of obtaining blood. In this

case, there Is both variability in time-to-incapacitation and variability in

time-to-blood sampling. For example, reference to the EC^q values in table 22

shows that laboratory 3 consistently obtained lower EC^q values. Thus it is

not surprising that laboratory 3 has a high percentage of low COHb values in

both tables 30 and 31.

The second reason for examining the blood COHb data is to determine

whether CO was the primary toxicant generated by the thermal degradation of

23
Che mater Lai beLng tested. Pure gas studies at NBS have shown that an average

concentration of 5000 ppm of CO and 89% COHb are necessary to kill 50 percent

of the rats in 30 minutes under the laboratory conditions specified by this

toxicity test method. Table 27 shows that 5000 ppm of CO and 89% COHb are higher values than those determined for any of the twelve ILE materials at the mass loadings/chamber volume needed to kill 50 percent of the rats within the

exposure time (30 minutes). The lower levels of CO and COHb found at the LC^q

( 30 minutes) for the various materials indicates that other factors or toxicants are acting in conjunction with the CO to produce the within-exposure

deaths. As the pure CO experiments did not cause post-exposure deaths, the

death of animals during the 14 day post-exposure observation period must be

due to other toxicants or unknown factors.

6.0 SUMMARY

Seven laboratories from academia, industry, and government participated

in an interlaboratory evaluation of the 1980 version of the toxic Lty test

method developed by the NatLonal Bureau of Standards. This interlaboratory

evaluation was designed to serve two purposes. The first was to examine the

reproducibility of results from the toxicity test method across laboratories.

The second purpose was to test the operability of the procedure and to

identify the modifications necessary to improve the method. Although the ILE was not designed to specifically examine the repeatability of experimental

results within each laboratory or the sensitivity of the test method results

to variations in procedures and equipment, these factors are examined in this

report wherever possible.

This ILE was not a round robin, i.e. , not all laboratories examined all

materials or used exactly the same methodology and instrumentation. In

addition, the test method itself continuously changed during this study,

primarily as a result of the information collected and presented to the ad hoc

working group by the ILE participants. The small number of laboratories which

examined some of the materials and the variations in procedure between laboratories (e.g., concentrations tested) limited the use of some kinds of statistical analyses on the reproducibility of results.

24
Data collected during this study and examined for reproducibility of

results across laboratories included: a) the autoignltion temperatures, b)

the CO concentrations, c) the HCN concentrations from the decomposition of

nitrogen-containing materials, d) the LC^q values calculated for the 30 minute

exposures and 14 day post-exposure observation periods for each material, and

e) the COHb values. The main conclusions follow:

1. The autoignition temperatures Independently determined for each material

showed good agreement across laboratories.

2. CO concentrations generated by the decomposition of Douglas fir were more reproducible across laboratories in the non-flaming mode than the flaming

mode. However, even in the flaming mode, many of the laboratories were statistically similar.

3. HCN results across laboratories showed reproducibility to within a factor

of 2.5.

4. A change in the cup furnace volume from 300 mil to 1000 mil does not significantly influence the CO concentrations generated from the decomposition of

Douglas fir nor the subsequently determined LC^q values. Also, this increase

in the volume of the cup furnace did not solve the problem of overloading the

heating capability of this particular furnace design. An increase in cup

furnace volume was recommended, however, in order to accommodate greater

quantities of low density materials.

5. The biological endpoint - the LC^q values for the 30 minute exposure and

14 day post-exposure observation period - appears to be less sensitive to

changes in the flaming decomposition temperature than to the non-flaming

decomposition temperature.

6. Brief excursions of the chamber temperatures to as high as 100°C did not

produce deaths.

7. The LC^q (30 minutes and 14 day) values were reproducible to within a factor of two for all materials decomposed in both the flaming and non-flaming

modes except for poly tetrafluoroethylene, polyphenylsulf one and wool.

25

s
8. The COHb data indicated that the results were *very dependent upon the

time of sampling and whether or not the animals were removed from the toxLc

atmospheres to obtain samples.

The second purpose of the ILE - to determine the modifications necessary

to improve the effectiveness of the test method - was fulfilled by the refinements which resulted in the 1982 NBS test method [3]. The changes which

resulted from the ILE are presented here:

• examination of materials at 440°C is now optional,

• the recommended size of the cup furnace has been increased from 300 mil

to 1000 mil,

• the highest average chamber temperature permitted in the vicinity of

the noses of the animals for the 30 minute exposure was raised to

40°C,

• the minimum average oxygen level permitted in the chamber was lowered

from 18 to 16 percent,

• for the 30 minute exposure, the only biological endpoint now required

is an LC^q [the mass loading/chamber volume (mg/il) which causes lethality in 50 percent of the animals in the 30 minute exposure plus

a 14 day post-exposure observation period]. The incapacitation

endpoint has been eliminated, and

• blood from non-cannulated animals must be taken in the first 5 minutes after the end of the exposure.

Other changes in methodology which resulted from information presented at the

ad hoc working group meetings are detailed in the report on the 1982 version

of the test method [3].

26
7.0 ACKNOWLEGEMENTS

We gratefully acknowledge the time and effort of the many investigators

who participated in this interlaboratory evaluation. We also thank those

companies who supplied the specific materials for testing. Further, we acknowledge the aid of Mr. Alan Stolte, Ms. Dolores Malek, Ms. Mary Diephaus and

Ms. Alison Durham in the reduction and analysis of data. A very important

part of this interlaboratory evaluation has been the statistical analysis of

the data and for guidance and assistance in this area, we are especially

thankful to Dr. James J. Filliben and Dr. Hsien H. Ku from the Statistical

Engineering Division, Center for Applied Mathematics, NBS, and Dr. Pearl

Fisher from the Applied Statistics Training Institute, National Center for

Health Statistics. We are also grateful to Dr. Richard G. Gann for many

helpful discussions.

8.0 REFERENCES

1. Becker, W.E., Clayton, J.W. , Emmons, H.W. , Fristrom, R.M. , Glassman, I.,

Graham, D.L. Long, R. , McDonald, D.W., Nadeau, H.G. and Lyons, J.W.,

Chairman, Products Research Committee. Fire research on cellular

plastics: the final report of the Products Research Committee

[Washington, D.C.] 1980. 213 p.

2. Birky, M.M., Paabo, M. , Levin, B.C., Womble, S.E., and Malek, D. Development of recommended test method for toxicological assesment of inhaled

combustion products. Nat. Bur. Stand. (U.S.) NBSIR 80-2077, September

1980. 63 p.

3. Levin, B.C., Fowell, A.J., Birky, M.M. , Paabo, M., Stolte, A., and Malek,

D. Further development of a test method for the assessment of the acute

inhalation toxicity of combustion products. Nat. Bur. Stand. (U.S.) NBSIR

82-2532, June 1982. 143 p.

4. Potts, W.J. and Lederer, T.S. A method for comparative testing of smoke

toxicity. J. Comb. Tox. _4_: 1 1 4—162 , 1977.

27
5. Packham, S.C., Frena, D.B., McCandlesa, J.B., Petajan, J.H., and BLrky,

M.M. A chronic intra-arterial cannula and rapid technique for carboxyhemoglobin determination. J. Comb. Tox. _3_:4 7 1—47 8 , 1976.

6. Packham, S.C., Jeppaen, R.B., McCandlesa, J.B., Blank, T.L. , and Petajan,

J.H. The toxicological contribution of carbon monoxide as a component of

wood smoke. J. Comb. Tox. _5_: 1 1—24 , 1978.

7. Litchfield, J.T., Jr. and Wilcoxon, F. A simplified method of evaluating

dose-effect experiments. J. Pharmacol, and Exp. Therapeut. 96 ; 99—1 13,

1949.

8. Paabo, M., Birky, M.M., and Womble, S.E. Analysis of hydrogen cyanide In fire environments. J. Comb. Tox. _6_: 99—108 , 1979.

9. Natrella, M.G. Experimental statistics. Nat. Bur. Stand. (U.S.) Handbook

91, Chapter 3, Section 4, pp. 3.40-3.42, 1966.

10. Dunnett, D.W. Pairwise multiple comparisons in the homogeneous variance,

unequal sample size case. J. Am. Stat. Ass. 15JL1M-795 , 1980.

11. Dunnett, C.W. Pairwise comparisons in the unequal variance case. J. Am.

Stat. Ass. 7Jk796-800 , 1980.

12. Kimmerle, M.G. Aspects and methodology for the evaluation of toxicological parameters during fire exposure. J. Comb. Tox. _1_:4— 5 1 , 1974.

13. Mat Ljak-Schaper, M. and Alarie, Y.A. Toxicity of carbon monoxide,

hydrogen cyanide and low oxygen. J. Comb. Tox. _9_: 2 1—6 1 , 1982.

14. CRC Handbook of Tables for Probability and Statistics. Table for the

critical values for the sign test. The Chemical Rubber Co., Cleveland,

Ohio. p. 163, 1966.

15. Products Research Committee. Materials bank compendium of fire property

data. Nat. Bur. Stand. (U.S.), [Washington, D.C.] 1980. 167 p.

28
29

Figure

1.

Exposure

chamber.
30

Figure

2.

Pyrolysis/combustion

furnace.
31

Figure

3.

Animal

restrainer.
32

Figure

4.

Exposure

chamber

with

separate

furnace.
ro in _a

cO

<rH CVJ CO ^ ID o _Q °0

10 CO

ro -'T o -Cl IQ lO

CXI -ST ID 0

CD

oj lo _o<o LABORATORY NUMBER

o

o

o

o

IDo

o

in o

U

oc

Z)I—<

CL

LlJ CL

OO

'fr

LJ

I— O

o

OJo

o

o

b.

PSTY

SPTFE

^PVC

SPVCZ

Ml REDO

QRPU

m wool

cvj^todi vh o cOjd -<hcvjxj in co _o co oi to o co

iD iD COO <D o' ^ cD CO LABORATORY NUMBER

Figure 5a & 5b. Auto-ignition temperatures determined for each

material by each laboratory. (Solid black portion

of some bars indicates intralaboratory variability.)

33
LABORATORY NUMBFP

Figure 6a & 6b. Flaming temperatures determined for each material

by each laboratory. (Solid black portion of some

bars indicates intralaboratory variability.)

34
co in -g

<0

,h oj co o- in g -g co

cO o

co cO cO

cj o- in

cOg gj -<r in -go

LABORATORY NUMBER

o

o

COo

o

r-o

o

co

u

o:z>

t—<

QLU

Q_

LJ

O

o

in

o

o

COo

o

OJo

o

o

b.

PSTY

0PTFE

SPVC

SPVCZ

I] REDO

BRPU

[D WOOL

OJ o _o

co co

o- o

co

CO -Oco

OJ -gco

in -q. co oO' -g CO

co OJ CO g CO cO

LABORATORY NUMBER

Figure 7a & 7b. Non-flaming temperatures determined for each

material by each laboratory. (Solid black portion

of some bars indicates intralaboratory variability.)

35
(Go) 3am>/a3drGl 3S0N

r\

W

<PD

C

£

LU

z:H

I36

Figure

8.

Chamber

temperature

at

animal

nose

positions

during

30

minute

exposure

to

flaming

wool

and

Douglas

fir.

(NBS

data.

Furnace

temperature

for

flaming

wool

was

675°C

and

for

flaming

Douglas

fir

was

490°C.)
AVERAGE

CO

(ppm)

Figure 9. Average carbon monoxide concentrations (ppm) from

Douglas fir decomposition as a function of the mass

loading/chamber volume (mg//)- A. - Non-flaming results.

B. - Flaming results. Solid line - Slope of laboratory results

up to 30 mg/I (A) or 50 mg/I (B). Dashed lines - Laboratories

with greatest and smallest slopes.

37
38

Figure

10.

Carbon

monoxide

generation

from

Douglas

fir

decomposed

in

the

flaming

mode

in

both a

large

and

small

cup

furnace

(NBS

data).
SYMBOL

LABORATORY

39

Figure

11.

Average

hydrogen

cyanide

concentrations

(ppm)

from

the

non-flaming

decomposition

of

ABS

as

a

function

of

the

mass

loading/chamber

volume

(mg/7).
T1ME-T0-INCAPACITATI0N

(min)

CHAMBER VOLUME

|mg/l)

Figure 12. Time-to-incapacitation vs mass loading/chamber volume hyperbolas

for Douglas fir in the non-flaming mode from six laboratories.

(Symbols refer to the mean and standard deviation of the timesto-incapacitation of the 6 animals tested at each mass loading.)

40
100

oocLU

Q_

90

80

70

60

50

40

30

20

10

0

5 10 15 20 25 30 35 40

MASS LOADING , /n mg/I

CHAMBER VOLUME

Figure 13. Concentration-response curves resulting from animal

incapacitation, death within exposure (30 min.) and

death both within and post-exposure (30 min. + 14 days)

from the thermal decomposition of wool in the flaming mode.

41
DETERMINATION

OF

COHb

AT

EC50

AND

LC50

qHOO %

</> 3Ou

<0> o

in U6

in O

LU

CO AO

o>oE

Q) A

>sXoAk_(0oc

0)ok_0)aco

'A

(0cE

k_a>

0) Q

a>3

O)

CO "O

a>c

'co AO

(0

<D j*

_3 CO

CO o > a

~o

a

o

k- o 0) A c E E

JO o

*- E

'in o

>s

CO

k_

**-

O CO

+-> CO TJ + cn • m c z Eo </> CO U) '—

c o -o

in <0 o o

_i

(/)

ac

CO

</> COE

42
Table 1

Laboratories that Participated in the

Interlaboratory Evaluation

o Armstrong World Industries, Inc.*

Lancaster, Pennsylvania 17604, and

B.F. Goodrich Company*

Cleveland, Ohio 44131

o Center for Fire Research

National Bureau of Standards

Washington, DC 20234

o Federal Aviation Administration (FAA)

Aeronautical Center

Oklahoma City, Oklahoma 73125

o Haskell Laboratory, E.I. DuPont de Nemours & Co.

Wilmington, Delaware 19899

o Southwest Research Institute (SwRI)

San Antonio, Texas 78284

o University of Utah

Salt Lake City, Utah 84112

o Weyerhaeuser Co.

Longview, Washington 98632

*These two laboratories worked together and submitted one set of data.

43
TABLE 2

List of Materials

Material Description Abbreviations

Acrylonitrile butadiene styrene pellets ABS

Douglas fir slabs 10" x 10" x 1" DFIR

Flexible polyurethanep,t flexible foam FPU

Modacryllc knit fabric MOD

Polypheny Isulf one pellets PPS

Polystyrene^ rigid foam PSTY

Polytetrafluoroethylene powder PTFE

Poly(vinyl chloride) pellets PVC

Poly (vinyl chloride) with

zinc ferrocyanide

pellets PVCZ

Red oak flooring boards REDO

Rigid polyurethanep,c rigid foam RPU

Wool unbleached unwoven fibers WOOL

p: PRC materials were obtained from the Products Research Committee , Office of

Standard Reference Materials, National Bureau of Standards, Washington, D.C.

20234 [15].

a: PRC material, GM-21

b: PRC material, GM-51

c: PRC material, GM-30

It is important to note that the results shown in the following tables pertain

to the particular samples tested during this study. The materials used were

selected to represent a wide range of properties. No attempt was made to provide

statistically valid samples of a given material. Therefore the results should

not be used to judge any particular class of material.

44
Experimental

Design

of

Interlaboratory

Evaluation

Q

O

E

< X <

a

2

O

Q

W

Pi X X X

2

PhPi X

Q

<3 • X 2

to

PH

Pi X X X <

o

>

Ph X X

cO •H

Pi0) 4J

«3 S

2

Ph

Ph

X

X X

X

Q

2

Q

2

M

U

>

Ph X X

pHM

pHQ

O Q X X X X X X • X

2 2

O

O2

X X X

W

PhH

Ph X X X

to

CP<

X X X <

03

03 •H

Vhou

0) p

o

rO

to 2

CO rsito<fLOPQr^.ooc^ 2

03C

O

T3O2

n

2

45

Additional

material
Room

Conditions o

rOGJ

03UG

T3C

03

G

C (0

0) 3

•9

G

M

U

0)

O

UG

ja

u

u

0) o

42u * o GM

T3

G

O rH

42 44

i—I 00

rH <D 3 rH

4-1 03 - C

rH rC co

03o

42

u

u

GG

42 0 3 cd •H U I ^

iH >%

Cd 4-1 •H r O

CO (1) cd a h co 00

*HX C2 G o H 3

cd 0) G CO G *H

S'

G

a)MG •• 3< /~N

cd

w

uH 44G

0) /-v CJ 55 3

CO

PQ o

•H ,X rH U

<3 03 « rH

PQ

G 42 rH a)

u CD

G

os a) 4-1

u

G cd 0)

M 03 Cd 03 59 COOM 44

a)O CL)O 44 0 G 55H •H cd

a *h 42 0 G •H ,3 ^ M s-x (1) u 5 O

03 cd 0 d) rH -X

03 3 00 0) G G G <3 a a *H *

/*“N •H

GM

•*

O 44 CJ 3 M • W *H 03 <3 -S’ P* H . *. > •H wH 0) a w 03 O 1 3 G p- <3 rJ a* C/3 1 *H 03

44 Cd C/3

Q (3 II

44 44

XO

G o 44 o G >•» •H

M •H

(fl cd 03

O p- o 0 G 44 rH COOQ

H

a

g

UX •H 44 ^ <3G

G »—1 P C cd Q* <3 U (3 •H O U 3 0) O o o a G M CJ O G o CJ •• 44 44 g G U > 3 G 42 1—4 >% G G *H w G H CO cu CO G T) <3 G 44 H H G £

<3 o G 0 0 M ,3 iH

MG CO Pa •HOO 0 rH

cd >> rH 44 00 3 rGX

G 3 H •• 0 0 59 *d- H G CO C O w H < PQ CO C/3 C/3 0 0 0) 44

(3 44 •H T3 <3 rH cd 3 * • • • • • • • O

^5

u < H CM co

m v£> r- oo CJ

Q wdd 0 S H a

coM

0) •u

/*> 0 0 0 *H g o a a

03

iH

G

G

G

a 0 O

•H /-s

G 44

C

G fi

Ga

H 03

G 3 G 03

-GG 44

G

G

aM 44

G 3 0 03

G

G 44

O

G

U

M

G Xi o O 44 CO M •H

44 44 •H 42 rH

•U

W

G

G 44 CO >>

a

a CO

G rH 44

GG -c

GG

G

a CO 44G

G

a

U

C o H

G 0 G

G 3 rH 3 a

44 CJ 44 03

G

w

G rH

G •'d' 44 G CJ 44

03

03

G CO M 44G

00

G

G 0

*H 3

»HM & 4J

00G

a

a fl 4J 42 42a 4J o G

G • aj 0 44 o 00 44 OO G G 44 a G N G a rH J3 •H C T3 •H rH a U a G •H s—' *H *H G o CJ CO G *H G o c G *H M 44 CO 03 03 > a rH ^ xi > G a 0 G G G 44 G G ? rH

cu

a

U 0 CO

O

p

OG ^ <3 « 42 a 3W

•HQ

G 42 CJ 03

•H • • • • • • Q G 42 O 03 G 44

G sQ

rH

CH S O x

C3 0 • • x • • 0 • • rH CN1 w rH CM CO rH CM CO

•H CM CO 4J CNO O C ^OUU-H

rt

_ s 4 «* x> o as

n ^ u

46
47
Table

4c

48
Techniques

for

Carbon

Monoxide,

Carbon

Dioxide,

and

Oxygen o Gu

mm

g

O

G0 G 3 g u G 4J 2 Gc g

a) •H a 43

O

a MMG

O •H CU *H •H *H

G

*H 43

G 43 43a 4J

U 4J cu

M CU CU

G C/3

G

G

G 00GG cu

4-4 d)

GM 0 o U

aU CO 4-4

O 0 00 00 4-» •H 00 •H 00O P G o G G O G O >v

G

U 0 u 0 Gu

Gu rH P

cu 4J

GGO > G > G

GG

co

M rH

u pH pH rH pH 4M <D

H c cd

O 6 GO

G o G

M

M Pm CU o P4

O Pm 3 3 G G • /-s CM G G o o O O CO CJ CJ 4-1 *H O

4J cu • M G u G <r m m <j- m G 2 3

4-1 vO vO CO vO VO vO o CU 4M G 00 00 d) 00 00 00 o M G o G no *H o O 43 G 0 G G u 0) M G G G 00 U 43

0) 3 G

G <!

M 4JG

G

G

G 4-1 0 *M 0 0 S G CO 0 0 0 G *H ^ G 4-1 J2 M l »M 3 M S2 3 rH 43 u

25 CO

a

a 3 Mm *d o o aM

M o G D 0) o G G G 0) G G 4-1 MM M P3 « o hM M CQ « pq O CU G

g§u3

COG

a) 2

<u •HXO

•HQGO

43

JmG

CJT3GGg

*HXogo2go

4>

V4G

cj

a

4-1

g ° i

0)

M

a 4-1 CO H G o ug ^ 0) a B G a)

a)

m 3 3

U* CO

a) Cd U <D Pm g Uo

4-> cdMO

43

cd

h-3 §o oI 'd*

43a

cd 43O

cd « oo

CJo o o

CM

co3O3a

•H

4-1 ao

CJ

C ft CO

H

CO CO co

G 0 G 43G 3 3 3 4-1 *H a 4-1 O O O 4-1 ir* 3 G 3 3 3 *H CO 0 G G G 0 4-1 • •H *H •H U U G CO U T)

4-1 4J 4-1

G

GGG

O

G

GGG 4-1 > 0 o U

OO o G

G 4-1G

CJ CJ CJ

H <? *H

G

U

v-x 3 G

G MM

cr CO 0 G • G G CU •H 43 a *H CU rH 3 G G G o a* > M

•H

G

G •H 00

a CO o M G G M 4J G H 43 G (rt B 4-1 CU B B CO O o • 4-1 •H u

cr* vO 00 o G

G 43

H

G

a

G 3 4-1O

•H T3 2 w G G G

4-1

a rH o M o CU • • G u 0 pc5 U CU HM ••

cd *h up CO

a) a) 3-S MG M a o x a

0)

a) co 43 *GM

cd

cr «

a) T3 pH

Cd 0)G

(X 0 H G 43

co co cd •H M rH 43 O *H w d cd c > g <u cd H 4-1 T) O W G G

•H

G 43

44

O

*H •H

G

4-1 4J 43 G G 4-1 G X) T3 G

•HG rH 0 •H

G 0 H M O G G u G G G

CO

U

G

pH

a

G

G

•H «H

G

U CU G 0 G

4-1

H •H

G0 GO

G

U *H *H O 4-1 MM G *H O 4-1 CO •H G

4-1 MM

G

G

H -d

ga c 3 g

Jm TJ

4J

CJo

49
Modifications

of

the

SO

co c/5 o 3 o q gg«S J«!<3

<T3 X) O -O 01 4^

50
Table 7

Autoignition, Flaming and Non-flaming Furnace Temperatures

Material Laboratory _____

Temperatures (°C) Autoignition Mean* S .D. * Flaming Mean* S.D.* Non-flaming Mean* S.D.*

ABS 1 525 550 500

3 555 725 530

5 500 694-700 475

6b 550-575 533 25 600 642 81 525 508 25

DFIR 1 465 490 400

2 465-475 500-515 440-450

3 475 490 430-450

4** 490 495-550 440-485

5 440-515 546-581 404-494

6a 465 478-490 440-442

6b 465 490 440

8 510 472 21 535 503 24 480 439 21

FPU 3 395 420 370

4** 385 390-415 344-380

6a 395 402 370-372

6b 370 386 12 420 408 15 355 360 13

MOD 2 725 685-715

4** 740 760-775 710-720

5 710 736-740 679-683

6a 725 725 12 750 749 12 699-701 693 14

PPS 2 675-695 700-705 650 4** 694 712-720 665-675

5 645 670 615-620

6b 650 666 23 675 689 20 624-625 639 23

PSTY 2 450-460 475-480 425

4 550 540-560 515-540

6a 590 605 574

6b 490 520 62 515-565 534 55 465 495 64

PTFE 1 650 650-675 600-625

If** 685 695-725 635-675

6a 620 652 33 645 663 28 595 610 22

PVC 3 625 675 600 6b 600 613 18 625 650 35 575 588 18

PVCZ 1 625 650 600

2 625-640 665-685 600 6b 675 642 29 700 672 26 649-651 616 28

REDO 5 465 485-492 438-440

6a,

480 505-530 455

8 510 485 23 535 508 25 480 458 21

RPU 4** 594 610-625 560-577

6b 550 570-575 525-550

8 615 586 33 640 607 35 590 558 33

WOOL 2 660-685 680-685 635-665

3 695 700-720 670-720

6a 650 675 625-650

8 675 670 20 700 689 13 650 645 20

*The Mean and the Standard Deviation (S.D.) are based on values listed in the preceeding columns

Where a range of values are provided , the lowest value was used in calculating the mean and the standard deviation.

**The autoignition temperature was not given by the laboratory. Value used in table is the calculated

mean between highest non-flaming temperature and lowest flaming temperature.

51
Table 8*

Toxicity of Modacrylic at Different Temperatures

Mode Temperature (°C) LC^q, 30 minutes + 14 days

8

iM/il

Flaming 760 - 775 7.1 (6.4 - 7 . 9)

b

Non-Flaming 710 - 720

445 - 460

390 - 400

295 - 305

250 - 260 ^23.8° [17.

0

d

- 28.

3

e

] >22.

6

f

10.0 (6.9 - 14.4)

13.6 (10.7 - 17.3)

21.8 (18.4 - 25.8)

7.8 (6.3 - 9.7)

200

a: Data from laboratory 4

b: 95% confidence limits

c: Approximate value determined from values in brackets

d: 0/6 animals died at this mass loading/chamber volume

e: 5/6 animals died at this mass loading/chamber volume

f : No animals died at this mass loading/chamber volume

*: In this table and subsequent tables, the numbers quoted are as calculated

from the data provided by various laboratories. The 95% confidence limits

reflect only statistical variations.

52
Table 9

Maximum Chamber Temperatures Experienced by Animals*

Material Laboratory Flaming Mode Non-Flaming Mode 440°C Mode Temperature Mass Loading Temperature Mass Loading Temperature Mass Loading

(°C) Chamber Volume (°C) Chamber Volume (°C) Chamber Volume

(rng/f) (mg/ 1) (mg/ a)

ABS 1 N.I. N.I. N.I.

3 N.I. N.I. N.I.

5 33 35.0 29 40.0 26 37.6

6b 40 19.0 32 30.0 N.D.

DF1R 1 N.I. N.I. H

2 40 45.3 N.I. H

3 32 38.4 N.I. H

4 41 5.6 35 17.0 H

5 N.I. N.I. B

6a 42 52.2 31 40.2 H 6b 37 46.4 31 27.5 H

8 N.I. N.I. B

FPU 3 N.I. N.I. H

4 N.I. N.I. B

6a 47 25.1 30 47.7 H

6b 64 37.5 33 20.0 H

MOD 2 N.D. 37 5.0 N.D.

4 40 6.2 38 5.5 34 11.7

5 40 6.0 36 10.0 31 6.0

6a 37 5.5 38 3.3 28 4.7

6b N.D. N.D. 33 5.3

PPS 2 43 26.2 39 18.7 30 19.9

4 37 39.6 49 9.9 34 8.8

5 31 18.5 32 12.0 24 40.0

6b 53 20.0 39 10.0 N.D.

PSTY 2 45 39.9 30 50.1 H

4 35 17.1 N.I. H

6b 56 40.0 36 34.1 H

PTFE 1 N.I. N.I. N.I.

4 N.I. 36 0.05 N.I.

6a N.I. N.I. N.D.

PVC 3 N.I. N.I. N.I.

6b 37 30.0 35 18.0 35 20.0

PVCZ 1 N.I. N.I. Ntrl. 2 43 19.9 40 11.2 30 12.4

6b 37 12.0 40 12.0 33 12.5

REDO 5 34 60.0 30 45.0 B

6a 46 50.2 29 45.2 B

6b 37 25.8 N.D. H

8 N.I. N.I. H

RPU 4 29 0.1 25 33.9 32 0.1

6b 40 20.0 31 41.1 N.D.

8 N.I. N.I. N.I.

WOOL 2 50 39.9 34 40.1 31 27.2

3 N.I. N.I. N.I.

6a 109 41.0 36 17.6 N.D.

6b N.I. N.D. 36 25.1

8 N.I. N.I. N.I.

*Measured at nose position of animals.

a NBS small furnace

b NBS large furnace

N.I. no information provided

N.D. not done

H not determined as non-flaming temperatures were less or within 50°C of 440°C.

53
Table 10

Highest Average Chamber Temperatures Experienced by Animals*

Material Laboratory * Flaming Mode Temperature Mass Loading

CO Chamber Volume

Non-Flaming Mode Temperature

CO Chamber Volume

440‘C Mode Temperature Mass loading

(*C) Chamber Volume __ isaZ.42 Cm/O

ABS 1 N.I. N.l. N.l.

3 N.I. N.I. N.l.

3 31 20.0 28 40.0 25 37.6

6b 32 19.5 30 25.0 N.D.

DFIR 1 N.l. N.I. H

2 N.I. N.I. H

3 N.I. N.I. H

4 39 11.3 35 17.0 H

5 N.I. N.l. U 6a 33 52.2 31 30.4 H

6b 30 46.4 29 27.5 H

8 34 36.2 33 32.1 U

FPU 3 N.I. N.l. H

4 N.I. N.I. H 6a 30 25.1 29 47.7 H 6b 36 37.5 29 20.0 H

MOD 2 N.D. 35 5.0 N.D.

4 39 6.2 38 7.1 32 11.7

5 37 6.0 34 10.0 30 6.0

6a 35 5.4 36 3.3 27 4.7

6b N.D. N.D. 31 5.3

PPS 2 38 30.0 37 18.7 28 19.8 4 3? 1.0 47 9.9 33 8.8

9 29 18.5 30 12.0 23 40.0

6b 41 20.0 37 10.0 N.D.

P8TY 2 33 34.9 29 35.0 H

4 N.I. N.I. H 6b 35 40.0 27 34.1 H

PTFE 1 N.l. N.l. N.I.

4 40 0.14 38 .08 33 5.7 6a N.I. N.I. N.D.

PVC 3 N.l. N.l. N.I.

6b 34 15.0 33 18.0 29 20.0

PVC2 1 N.I. N.I. N.l.

2 42 19.9 38 11.2 29 12.4

6b 35 10.0 36 10.0 30 12.5

REDO 3 33 60.0 30 45.0 H 6a 34 50.2 28 40.2 H

6b 36 25.8 N.D. H

8 37 60.2 34 49.2 a

RPU 4 27 0.1 N.l. 33 20.8

6b 33 20.0 30 41.1 N.D.

8 34 12.5 31 29.3 28 35.2 WOOL 2 38 44.9 33 30.2 30 27.2

3 N.I. N.I. N.I.

6a 38 41.0 34 17.6 N.D.

6b N.I. N.D. 26 25.1

8 39 77.5 32 21.7 29 35.2

*For explanation of letters, see legend to table 9,

54
Table H

Carbon Monoxide Production Per Unit Mass Loading

Chamber Volume

Material Laboratory Flaming Mode Non-Flaming Mode

Mean* S.D. n Mean S.D. n

ABS 1 54 23 8 15 12

3 110 22 3 140 160

5 66 12 3 13 2.1

6b 75 16 7 22 2.5

FPU 3 78 80 4 130 83

4 26 14 7 47 22

6a 19 1.8 2 39 18

6b 26 1.5 3 30 19

MOD 2 N.D. 35 12

4 86 45 4 52 12

5 100 46 5 76 5.4

6a 77 34 10 82 2.4

PPS 2 70 14 6 150 39

4 120 39 4 150 116

5 200 19 5 340 56

6b 180 17 6 470 26

PSTY 2 46 1.8 5 2.3 1.

1

4 70 5.3 10 13 2.3

6b 34 3.6 4 1.8 0.4

PVC 3 115 82 5 65 40

6b 54 19 4 32 5.2

PVCZ 1 52 11 6 44 13

2 72 7.4 7 48 9.6

6b 150 12 7 100 10

RKIX) 5 69 6.6 7 87 7.8

6a 57 9.4 7 83 7.5

6b 37 2.4 6 N.D.

8 49 3.0 16 96 5. 7

RPU 4 36 10 2 28 29

6b 130 12 9 45 8.8

8 94 12 16 41 5.0

3

5

22

11

2

5

4

5

6

7

3

5

7

2

4

3

5

6

7

6

2

5

9

16

2

11

4

55

O'

m

m
Table 11. Continued

Material Laboratory Flaming Mode

Mean* S.D. n Non-Flaming Mode

Mean S.D. n

WOOL 2 22 2.6 8 30 7.5 6

3 68 16 5 69 15 5

6a 25 4.1 12 39 7.8 8

6b 25 4.3 2 N.D.

8 24 2.2 18 26 6.6 18

*Mean of Average gas concentration ..(BJgEl.-for each 30 minute exposure

Mass loading/chamber volume (mg/ 5,) S.D.: standard deviation

n: number of values used to calculate mean

a: NBS small furnace

b: NBS large furnace

N.D.not done

56
Carbon

Monoxide

Production

for

Douglas

Fir

in

the

Flaming

Mode <3 vO

<300 • <073 U O

<11 U Qj £

a

<u00 • <073 u o

<3 CJ

r

<u00 • /-> <073 0 MOP. OOP

<3

o

00 • <073 M O

O$

o

oo • <ot3 a MOP d) U P

<i

<300 • <ot3 a MOP <3 O P $

o ocs'

(300 • <ot3 a MOP <3 U Oj

<i

<300 • . <0 t3 a MOP <3 O P 3

rO

<0 J

OOOOOOOOOOOOOQOOOOOO OOOOOOOOOOOOOOOOOOOO OJH(7n<fCNCO^^vO'<ff7^'}COiri'4, v0^fO

cMCMcMCMcMCMcMcMcMcMcocococococo<r<f-3-<Jooooinmminoooovovovo'ococococo

o o o o o o

o o o o o o 00 00 O O vO N

H «h cm co co <r

O H ON ON M ^

o <r <f oo h vo

CM CM CM CO <f <J- oooooooooooo OOOOOOOOOOOO cooon-n-ooONOcMcomo<f HHHHHHCMCMCNCMnn

vDrHvOvor^iHcooor^cMOr^

NOOtMNmONONCMlOONN H CM CM CM CM CM CM CM CO CO CO

O O O O

O O O

o is co oo

co co <r co

o-o-oo

cn oo <r

co CO <f

oooooooo OOOCMOOOOO rH p*- -o- o oo o m rH CM CM CO

OOvOCOCMOOmO

HHiOHcMM'tC^

rH co co co <r

o o o o

o o o o fO CO H ON

rH CM CO CO

O rH 00 <T o on oo oo H H CM co OOOOOOOOOO

<rvDONvor^r^tHvOrHO oooooooooo

HHHHHHCM(MCO<f

o o r- o CM

CO VO N 00

00

vO CM vO 00

r-» rH

o <r m co

CM rH rH

rH

ON O CM r-* VO rH rH «H CO o o O O O H rH CO ON m O m o o O m o m ON <3 <3 00 rH CM CM CO CO CO co <r -a- *3- O

<0a

u

<da d

73 M u <d 0 p o

4H IH -J o O o o o O o o o rH <3 <0 o o o o o O o o o rH 00 CO CM P-. r- CO CM r- rH vo r-*» <0 u

rH rH •H CM CM CM CO CM CO CO -d- a <d X

rH CM CM CM CM CO 00 CO moocotnocsimo

rH CM CM CM CM CO CO CO e

<d

0) •• - CO X P CO pd Q Q

I

rPo

<d<3U

<3>

o

73

<300

<0u

<3>

<d

P <3 rO

§£

(0

_ c

w

c <d —

o B 2

*-> u .2

td <u c h a 5 - X

w

id a) T3

4-1 T3 0 h

<0 M

TJ 0)

a

2 § « u 3 aS w Z

" *? Q. .. ^3 “ c 8

5^|o

57
Carbon

Monoxide

Production

for

Douglas

Fir

in

the

Non-Flaming

Mode

V

00Sis I

Q)OO • 2^ I

HI U Cl

5 ocj r

a)oo • , cfl'd n o

<u u

I

2^ b hi u a 3

O? 5 *ob| S

0)00 • N «TJ 6 n o a

di u a I

pO

.3

0)00 • 2^ I

HI CJ Cl

a oce

aioo • 2*0 8.

<u o a 3

u oo( 6

a)oo • 2 ^ 8. hi u a 3

5 *

8888 ._ O^lOlOONrT-.n, NNNNfncsinn^

8888 ‘ co 888888 H (N <r co co ctn <r

1^1 m sf iA O <0 N N

N H H

vO\OiAiAvO\OiAiASSO\^HHHH

>3->tf>3->3'00a00000«<J->3, HHHHHHHHNNNNnnmn >3-'sr<N<N<N<N oooooooooo

OOOOONOO'OOmoOONCS HHHHNNMNCO

romomaN^somoin

ONnn^OONiAN rHr-|,HrHrHCMCMCMCMCM

O O O O

O O

cn oo m r>. H H N H

O O O CM

O O O O O O O

m o o o o o o s n o ri a rH CM CM CM CM M

o o on r* o m o mo nocoo

•H H CM CM CM CO

O Mf On S

OOOOOOOOOOOOOOOOO COOf^OOOOOOOOOOOOOO

H iHHCMCMCNr|COCMCMCMCOCM<rvO

OONiooNCMOr^r^coooo-frONOr^ONO

cNNcoa>on<r^mM^O'jOHnm HHHfHrHrHrHCMCMCOCOCOCO

O O O O O O m O 00 O O O ON CM ON 00 O O

rH rH CM CO

MA VO ON N N

M1 ON ON CO on 00

O O O O O O O

CO O O O O O O ia m vo on cm <r vo H rH rH CM CM CO

O H N CM CM ON CM

lA O CM lA O O rH H »H CM CM CO OOOOOOOOOOO ONOOOOOOOOOO yotAoocMcoo\rsrsONN(0 HHNNHCMCMCMCOCO

OrHvOrHrHrHI^CMCMr^CM

O S ^ H »H ^ CO

O VO rH <r

cm <t cn

O rH 00 m ^ rH

lAONiAiAinsOONiA HHHHHHCMCMCMCM

O O

C cn c2

oo

CD

M-)0

MO

fa*

58
Table 14

Laboratories Statistically Similar on Basis of "w"

Test on Carbon Monoxide Concentrations from Douglas Fir

Mode Laboratory Number (mean**)

Non-Flaming 43 5(110) 6a(110) 6b(l20) 2(120) 3(120) 1(140) 4(140) 8(170)

Flaming 19 2(69) 6a(76) 6b(83) 1(87) 5(95) 4(98) 8(100) 3(120)

Laboratories connected by a line are similar and laboratories not connected by a line are not similar (i.e. statistically significantly different)

*w - q

, 95

s e "h

**Mean of Average CO concentration (ppm) for each 30 minute exposure

Mass loading/chamber volume (mg/5,)

q (t,v) from Table A-10, reference [9].

t = number of laboratories

v = (n

1 + n

2 + ... + n

g

) -t

n = number of experiments done by each laboratory

S =

e

(n

x -1) S^ + (n

2 -1) S2 + ... + (n

g

-1) S

g

1/2

(n^ + n

2 + . . . + n

g

) -t

S = standard deviation

n^ = t/(— + + ... + ~ ) H n^ n

2 ng

(a) NBS small furnace

(b) NBS large furnace

59
Table 15

Maximum Average Carbon Dioxide Concentrations Produced

During Animal Exposure

Mode

Maximum

Material Average CC^

(ppm)

Laboratoryb Mass Loading

Chamber Volume

(mg/S,)

Flaming

ABS 14000 6b 30.0

DFIR 42000 6b 46.4

FPU 46000 6b 37.5

MOD 17000 5 2.0

PPS 37000 5 10.0

PSTY 42000 4 37.4

PVC 13000 3 38.1

PVCZ 10000 6b 15.0

REDO 63000 8 88.4

RPU 14000 6b 14.0

WOOL 56000 8 77.7

Non-Flaming

ABS 6300 5 40.0

DFIR 14000 2 30.2

FPU 7800 4 3.0

MOD 8100 5 12.0

PPS 9400 4 26.7

PSTY 7500 4 32.9

PVC 5400 3 14.3

PVCZ 6400 6b 14.0

REDO 15000 8 49.4

RPU 8700 8 35.1

WOOL 7800 6a 25.1

a: CO2 concentration (ppm) averaged over the 30 minute exposure,

b: Laboratory which found the maximum average concentration.

60
Table 16

Carbon Dioxide Production Per Unit Mass Loading

Chamber Volume

Material Laboratory Flaming Mode Non-Flaming Mode

Mean* S.D. n Mean £;.d. n

( PPm \

\mg/ l

)

( 2PB

\ mg/ & )

ABS 1 500 190 8 230 80 5

3 530 220 3 530 420 5 5 440 89 3 150 48 6

6b 550 58 7 170 15 3

DFIR 1 640 63 9 400 150 11

2 740 300 10 440 90 7 3 1000 310 4 490 240 6

4 990 760 8 330 210 17

5 730 44 4 200 55 3

6a 690 83 7 290 66 5

6b 930 71 6 300 70 9

8 800 56 20 210 85 16

FPU 3 2000 1000 4 550 500 5 4 450 220 7 460 730 22

6a N.I. 110 53 10

6b 1200 17 3 130 27 2

MOD 2 N.D. 710 140 3

4 830 680 4 310 150 4

5 2600 3300 5 940 410 5

6a 900 400 10 1000 240 6

PPS 2 800 84 6 380 200 7 4 1900 2500 4 2100 3200 3

5 1700 1200 5 580 190 5

6b 1100 59 3 540 120 5

PSTY 2 880 80 5 50 19 2

4 1300 570 10 160 50 4

6b 500 84 4 52 6 3

•PVC 3 840 560 5 420 220 5

6b 320 98 4 230 87 6

PVCZ 1 560 200 6 670 280 7

2 540 100 7 430 86 6

6b 650 79 7 470 20 2

REDO 5 790 140 7 300 67 5

6a 650 62 7 240 43 9

6b 780 110 6 N.D # 8 770 49 16 290 50 16

61
Table 16, Continued

Material Laboratory Flaming Mode

Mean* 97b. n Non-Flaming Mode

Mean 8 ,d 7 n

22

4

18

*For explanation of superscript symbols and letters,

aee legend to table 11

.

RPU 4 180 75 2

" 200 100

6b 900 82 4 230 60

8 570 79 16 230 22

WOOL 2 700 54 8 200 43

3 1400 500 5 570 310

6 a N.X. 280 90

6b N.I. N.D.

8 819 120 18 160 28

62

QD

Hjm
Table 17

Minimum Average Oxygen Concentrations*

Oxygen Concentration (%) Material Laboratory Flaming Mode Non-Flaming Mode 440 °C

AES 1 20.1 20.7 21.0

3 20.4 20.7 20.8

5 20.3 20.1 20.2

6b 18.9 20.1 N.D.

DFIR 1 19.0 20.0 H

2 N.I. N.I. H

3 18.2 20.5 H

4 18.1 19.8 H

5 17.8 19.9 H

6a 17.8 19.9 H

6b 16.3 19.2 H

8 19.1 19.6 H

FPU 3 16.4 20.6 H

4 N.I. N.I. H

6a 17.4 19.3 H

6b 14.2 19.9 H

MOD 2 N.D. N.I. N.D.

4 N.I. N.I. N.I.

5 19.7 19.8 20.1

6a 18.7 18.5 20.3

6b N.D. N.D. 19.9

PPS 2 N.I. N.I. 20.3

4 19.5 N.I. N.I.

5 18.2 19.8 20.5

6b 17.7 19.7 N.D.

PSTY 2 N.I. N.I. H

4 N.I. N.I. H

6b 17.9 20.2 H

PTFE 1 20.1 21.0 21.0

4 19.9 19.8 20.0

6a N.I. N.I. - N.D.

PVC 3 19.5 20.6 N.I.

6b 19.2 19.3 19.7

PVCA 1 20.6 20.9 20.8

2 N.I. 18.3 N.I.

6b 19.3 19.9 19.5

REDO 5 16.6 18.8 H

6a 17.2 19.6 H

6b 16.8 N.D. H

8 17.9 19.2 H

RPU 4 N.I. N.I. N.I.

6b 18.8 19.7 N.D.

8 20.4 20.1 20.3

WOOL 2 17.3 17.5 N.I.

3 16.7 19.3 20.7

6a 16.2 20.7 N.D.

6b 17.5 N.D. 19.8

8 19.5 19.7 20.7

Concentration of O

2 from the experiment which produced the lowest average

O2 concentration over the 30 minute exposure •

a ; NBS small furnace

b : NBS large furnace

N.I. : No information provided

N.D. : Not done H : Not done as non-flaming temperatures were less or within 50°C of 440°C

63
Table 18

Average Hydrogen Cyanide Production for Nitrogen Containing Materials

Decomposed Under Flaming and Non-Flaming Condition*?

Material Laboratory Flaming Mode Non-Flaming Mode

Maas Loading Average* Mass Loading Average*

Chamber Volume HCN Chamber Volume HCN

(mg/ Jl) (ppm) (mg / Z) (ppm)

ABS 1 10.1 81 10.1 16

15.1 120 15.1 42

16.6 140 20.2 49

20.2 150 25.2 50

25.2 170 30.3 78

3 4.8 44 4.8 28

9.5 100 9.5 41

14.3 160 19.0 81

19.0 230 38.0 150

6b 17.5 91 25.0 120

18.5 84 27.5 160

19.0 120 30.0 170

19.5 44 32.5 160

20.0 140

20.0 190

30.0 250

FPU 3 5.0 11 2.5 4 9.6 22 4.8 3

18.9 7 9.6 3 38.0 32 19.1 8

37.9 8

6a, b 25.1 23 15.1 9 30.0 19 20.0 8

31.2 26 20.1 19

35.0 15 25.1 17

37.5 14 29.6 21

40.0 17 30.0 9 32.2 10

40.2 6

42.7 19

42.7 16

45.2 12

47.7 17

47.7 17

MOD 6a 2.5 110 2.8 120

3.0 110 3.3 130

3.3 110 3.8 200

3.5 160 4.5 220

3.8 170 5.0 260

4.4 180 7.0 320

64
Table 18. Continued

Material Laboratory Flaming Mode

Mass Loading Average*

Chamber Volume HCN

(mg/ A) (ppm)

Non-Flaming Mode

Mass Loading Average*

Chamber Volume HCN

(mg/&) (ppm)

MOD 6a

PVCZ 1

6b

RPU 6b

WOOL 3

6a

5.0 208

5.4 260

5.5 250

6.2 220

5.0 50 4.0 45

10.1 92 5.0 63

12.6 111 10.1 130

15.1 158 12.6 210

15.1 180

12.0 90 10.0 120

14.0 100 12.1 140

15.0 140 14.0 220

15.5 100

16.0 110

17.0 140

7.5 66 20.0 59

10.4 68 20.7 15

13.0 130 21.4 12

14.0 170 30.2 8

14.9 150 39.6 61

20.0 190 39.8 100

39.9 40

40.0 19

41.1 17

9.7 30 4.8 120

28. 3 130 9.5 310

28.6 280 14.3 250

28.6 480 19.0 120

23.8 230

20.1 70 12.6 160

21.4 70 17.6 320

22.0 80 22.6 330

22.

6

50 25.1 250

22.6 70 30.2 200

25.1 120 32.7 210

30. 2 110

30. 2 120

35. 2 150

37.7 190

41.0 310

42. 7 200

*Average HCN concentration (ppm) for each 30 minute exposure

a: NBS small furnace

b: NBS large furnace

65
Table 19

Hydrogen Cyanide Production Per U.-4* JMass Loading

Chamber Volume

Materials Laboratory Flaming Mode Non-Flaming Mode

Mean* S.D.

( PPm \

n Mean S.D.

im\ n

\mg/$J

ABS 1 7.8 0.6 5 2.4 0.7 5 3 11 1.2 4 4.6 0.8 4

6b 6.4 2.6 7 5.3 0.5 4

FPU 3 1.4 1.0 4 0.6 0.6 5 6a, b 0.6 0.2 6 0.4 0.2 13

MOD 6a 41 5.3 10 47 4.8 6

PVCZ 1 9.6 0.8 4 13 2.0 5 6b 7.6 1.0 6 13 2.2 3

RPU 6b 9.5 1.8 6 1.2 1.0 9

WOOL 3 9.1 5. 7 4 18 11 5 6a 4.1 1.4 12 12 4.7 6

*For explanation of letters and superscripts, see legend to table 11.

66
Incapacitation

Times

After

Exposure

to

Non-Flaming

PVC

co

o

coeu

too

c

o

CU

CO

• • ts t

CO

CMco

ONm

mt

+ 1 ON

CO

• • vO

CO

1—

1

o

cO <u m m o m o o

0 CO iH mT o Mf m CM

4-1 • • o c ON ON rH CM rH vO

<J r-H CM vO 00

m o o o rH in Mf CO

CM CO o CM rH CO Mf MT

I—I M

CM CO uo V£> cm co mi- in vo

c

O /-M

•U *H c

CO 4-> *H

CU CO S H M ' 3Q

o

ON o

vO

60

C3 •H

COO

CO

COCO S3

O

> ^H 60

cu a §~

cO 4=

CJ

ONoCO

Mf

• VO

mi67

46:00
TABUS 21

Constants for Time-Concentration Hyperbolas (Y • Q + R/X)

Material Laboratory Flaming

Q _A

ABB 1 3.2 188.0

5 12.6 56.7

DFiR 1 13.3 231.4

2 3.0 389.2

3 7.2 263.8

6a 13.2 317.3

6b 13.8 246.2

8 9.3 230.3

FPU 6a, b -42.9 2739.0

MOD 2 N.D.

S -2.3 79.8 6 -2. 8a 82.

9

a

PPS 2 10.3 239.8

4 e 9 12.1 92.3

PITY 2 -25.3 1689.4

6b -6.4 649.2

PTFE 3, 6.5 27.0

pve 3 e

PVCZ 1 -3.8 347.9

2 15.0 1.9 REDO 9 9.2 t 441.5

6 12.0a 'k 385.3a ' b

8 5.0 856.6

RPU 8 4.5 139.3

WOOL 2 2.2 586.0

3 -10.9 517.0

6 5.

7

a 409.

9

a

8 11.0 497.1

at Nil small furnaee

bi HIS large furnaee

Cl No idata points

di One data point

ei Two data points

Gi No incapacitation

N.D. Not determined

Hi Non'-flaming temperature within 50*C of 440*C

Non- flaming

0 440'G

-6.1 738.0 -13.8 1011.5

0.7 492.5 d

12.8 226.9 H 17.7 99.0 H 7.5 107.0 H 16.6 230.6 H 18.5 98.7 H 10.3 242.7 H

G H

-7.7 161.3 N.D. -0.3 62.9 4.3 78.4 , 18.

6

a 149.

9

a —3 . 4® i .b 157.4®*°

7.4 212.0 C 17.11 205.9 C 9.2 99.8 N.D.

G H

d H

4.9 16.7 d

2.8 161.4 e

2.1 78.6 6.5 130.0 51.7 888.9 d 16.8 172.5 H

5.

8

a 480.

Q

a

H 12.0 299.2 H

-3.9 940.6 Q

4.4 272.6 d

e e 12.0® 867.9® 11.2^ 332.

3

b -9.5 891.1 -61.9 2595.9

68
Material Laboratory

TABLE

EC^q Values

Flaming

22

19

(mg/ i)

Non- flaming 440°C

ABS 1 10.6(7.4 - 15.2)

c* •V21.0U5.11 - 25.212

] d

•v-20.2115.11 - 25.

2

13

3 6. 0(4.1 - 8.9) 5. 8(2. 8 - 8.4) 9.0(4. 7 - 17.3) 5 yl7.0[15.07 - 20.

0

13

] -V-23.0U8.5

1 - 27.

5

13

] <37.

6

13

DFIR 1 20.0(16.4 - 24.3) 15.0(12.3 - 18.2) H

2 18.4(14.0 - 24.1) 10.1(7.2 - 14.2) H 3 VL4.5U0.01 - 19.

1

13

] 5. 6(3.1 - 9.9) B

4 N.D. 22.0(13.2 - 36.7) H

5 14.0(10.5 - 18.6) 19.2(14.3 - 25.8) H 6a 21.8(15.5 - 30. 7) 17 18.3(14.5 - 23.0) H

6b ,v23.5[23.01 - 24.

0

13

] 13.5(12.9 - 14.2) H

8 y20.9 3 ’ 13 14.7(13.3 - 16.2) H

FPU 3 9. 6(4.1 - 22.1) 7.0(3. 6 - 13.6) H

4 ^49.510 * 15 20.2(8.6 - 47.3) H

6a, b 37.5(35.8 - 39.3) 53.0(40.1 - 69.9) H

MOD 2 N.D. 2. 7(2.1 - 3.4) N.D.

5

,v2.8[2.01 - 3.09+

] V3.0I2.0

1 - 4.013

] 'v-5.0[4.0 1

- 6.0

13

] 6 3. 1(2. 2 - 4. 3) a ’ 17

3. 2(2. 8 - 3. 7) a

6. 4(5. 8 - 7.0) a,b

PPS 2 <15

12

8. 8(6. 8 - 11.2) >19.

9

1

4 21.8(12.9 - 36.7) 19.0(10.2 - 35.3) N.D.

5 <1013 <7.013 >40.

0

1

PSTY 2 %30.01050.

0

1 H

6b -v-28.7127.5 1 - 30.

4

13

] >40.

0

1 H

PTFE 1 M).80[0.063 - 1.51413

] 0.68(0.31 - 1.49) ''<15.2[15.1

1 - 25.

2

13

: 6a >0.251 >5.031 N.D.

PVC 3 6. 0(4.0 - 8.9) %9 .

4

10 * 16 13.5(4.9 - 36.8)

6b VL8.5[17.55 - 19.

8

13

] >30.

0

5 >30.

0

5

PVCZ 1 11. 8[10.

I

8 - 15.

I

13

] ~5. 4E5.1

1 - 10.

I

13

] 7. 6(4. 5 - 12.7)

2 13.2(11.3 - 15.4) 11.7(10.3 - 13.2) VL2.41U,ii

REDO 5 13

<40.

6

J"5 <25.

0

13

H

6 34.8(31.1 - 39.0) a,b ’ y23.0[22.51 - 24.213

] 8 H

8 51.0(46.1 - 56.5) -V24.1 3 * 13 H

RPU 8 8. 9(5.1 - 15.6) y29.36 [29.3

1 - 35.

I

13

] >35.

2

1

WOOL 2 23.8(16.0 - 35.3) yl7.0[15.05 - 20.

0

13

] >27.

0

7

3 yl7.2[9.78 - 19.

0

13

] 6. 8(4. 2 - 11.1) y23.3[19.34 - 30.

I

13

6 -v22.3[22.11 - 22.

6

13

] a 19.7(16.2 - 24.0)

a 24.5(23.0 - 26.1)

b

8 <45.

0

13 24.0(20.3 - 28.3) y29.36 [29.31 - 35.

2

1

a: NBS small furnace

b: NBS large furnace

c: (95% confidence limits)

•v: Estimated [values used to determine estimate]

H: 440°C is greater than or within 50°C of non-flaming temperatures

N.D. Not determined

1: 0% affected

Superscripts 2-12 refer to number of animals affected/number of animals tested

2 : 1/2

3: 1/3

4: 1/5

5: 1/6

6: 2/3

7: 2/5

8 : 2/6

9: 3/5

9+: 4/5

10: 3/6

11: 4/6

12: 5/6

13: 100% affected

14: No data points between 0% effect and 100% effect

15: One data point only

16: One data point between 0% effect and 100% effect

17: Significantly heterogeneous data

18: Late post-exposure deaths not counted

19: Litchfield, J.T. and Wilcoxon, F. , reference 7 69
TABLE 23*

LCj

Q (30 mlnutaa 14 days) in mg /l

19

Material Laboratory Flaming Non-flaming 440*C

ABS 1 15.0(12. 3-18. 3)

C 19.3(13.9-26.9) 30.0(26. 5- 34. 0) 18

3 15.6(13. 2-18. A) >38.

4

5 >38.

0

8

5 20.8(15.9-27.2) 33.3(23.1-47.9) >37. b

U

6b 19.3(16.7-22.3) 30.9(21.2-45.0) N.D.

DFIR 1 35. 8(28. 6-44. 9) 38 16.7(14.5-19.3) H

2 A5. 3(39. 0-52. 7) 27.6(22.9-33.3) H

3 *24(19.

0

1 -29.

0

12

] 16 26.8(21.3-33.7) H

4 29.6(22.7-38.6) 24.0(19.9-29.0) H

3 38. A(35. 2-A1 .9) 25.9(20.0-33.5) H

6a Al. 0(33. 0-50. 9) 20.4(16.4-25.3) H 6b 39.8(38. 2-A1. A) 22.8(20.2-25.8) H

8 29.8(23.9-37.1) 18.5(17.3-19.8) H

FPU 3 >38.

0

1 27.8(16.9-45.8) H

4 >A9.5 1 40.0(31.2-51.3) H

6a&b >40.

0

5 26. 6(15. 3-46. 2) 17 H

MOD 2 N.D. 5. 2(4. 9-5. 5) N.D.

4 7 . 1(6. 4-7 .9) 7. 8(6. 3-9. 7) 10.0(6.9-14.4)

3 A. 7(3.2-6.9) 7.0(5. 0-9. 7) ~S. 7[4

1 -69

] 16

6 4. 4(3. 9-5.0)® 5. 3(4. 0-7.1)" 7.3(6.3-8.5)®‘ b

PPS 2 25.3(22.0-29.2) 18.7(15.2-23.0) >19.

9

1

4 ~36[2A.

9

1 -39.611

) 16 32.2(27.7-37.5) >9.9 3

3 11.7(9.1-15.0) 10.7(8.4-13.6) >40.

0

1

6b 19.8(14.8-26.5) 9.5(9.1-10.1) N.D.

PSTY 2 53.5(41.4-69.1) >50.

0

1 H

4 32.6(30.5-34.8) >46.

2

1 N.D.

6b 38.9(37.9- 39.9) >40.

0

1 H

PTFE 1 0.164(0.073-0. 367) 0.125(0.083-0.188) ~15[5.

0

X -25.

0

13

] 14

4 0.400(0.02-6.81) 0.235(0.05-1.20) N.D.

6a 0.045(0.039-0.054) 0.045(0.017-0.120) N.D.

PVC 3 'vl5[10

1-19 12

] 16 *16[14 8 -19 13

] 16 20.7(14.0-30.7)

6b 17.3(14.8-20.2) 20.0(14.7-27.2) 25.0(20.2-31.0)

PVCZ 1 9.4(7.2-12.3) 7.6(5.5-10.5) 8.5(6.1-11.9)

2 14.3(12.5-16.3) 13.3(11.5-15.4) >12.

4

4

6b ~15tl5.0

1-15.

5

13

] 11.3(8.5-14.9) 12.8(12.1-13.6)

REDO 5 45.0(39.9-50.8) 25.0(18.7-35.5) H

6 56. 8(51. 6-62. 5) a,b 30.3(26.0-35.4)® H

8 60.0(56.6-63.6) 35.0(24.5-50.1) H

RPU 4 >38.

4

1 >34.

0

1 >39.

6

1

6b 13.3(12.2-14.5) >39.

6

1 N.D.

8 11.3(7.6-16.8) >35.

I

2 >35.

2

1

WOOL 2 42.8(36.6-50.1) 25.2(18.4-34.6) >27.

2

1

3 n.23119 1 -2413

] 14 15.8(13.5-18.6) ~25[19

1 -3011

] 16

6 28.2(23.0-34.5)® 25.1(22.3-28.3)® 32. 1(30. 2-34. l) b

8 60.0(46.6-77.3) 28.5(23.5-34.6) 32.6(28.7-37.0)

*For explanation of superscript letters and numbers, see legend to table 22.

70
TABLE 24

Material

Slopes of LC..^,

Laboratory

30 min. + 14 days

Flaming

(95% confidence limits of

Non-flaming

i v 19

slope)

440°C

ABS 1 1. 58(1.34-1. 85)

20

1.80(1.02-3.16) 1.20(1.07-1.36)

3 1.23(1.08-1.40) C C

5 1.46(1.13-1.89) 2.06(0.86-4.92) c 6b 1.37(1.09-1.72) 1.23(0.99-1.54) N.D.

DFIR 1 1.41(1.06-1.89) 1. 38(1.05-1.81) H

2 1.30(1.00-1.69) 1.26(1.04-1.53) H

3 E 1.64(0.0-3.85) H

4 1.69(0.66-4. 30) 1.69(1.29-2.22) H

5 1.14(1.01-1.28) 1. 73(1.25-2.41) H

6a 1.66(0.81-3.39) 1.43(1.09-1.88) H

6b 1.05(1.02-1.08) 1.25(1.10-1.42) H

8 1.51(0.61-3.73) 1.08(1.04-1.12) H

FPU 3 C 1. 87 (1.19-2.94) H

4 C 2.37(1.46-3.84) H

6a&6b C 2. 37(0. 93-6. 01)

17

H

MOD 2 N.D. 1.11(1.02-1.21) N.D.

4 1.14(1.00-1.30) 1.40(1.18-1.66) 1.91(1.04-3.52)

5 1.88(1.22-2. 89) 1.70(1.23-2. 36) E

6 1.30(1. 10-1. 53)

a 1.67(0. 99-2. 81)

a

1. 35(1.09-1.68)

PPS 2 1.23(1.09-1.38) 1.35(1.02-1.78) C

4 E 1.21(0.98-1.49) C

5 1.41(1.00-2.00) 1.31(1.07-1.61) C

6b 1.50(0.50-4.47) 1.07(1.04-1.11) N.D.

PSTY 2 1.51(0.71-3.20) C H

4 1.14(1.07-1.23) C N.D.

6b 1.03(1.00-1.07) c H

71
TABLE 24 (Continued)

Material Laboratory Flaming Non-flaming 440°C

PTFE 1 4.15(1.67-10.28) 2.07(1.29-3.31) E

4 5. 10(1. 80-14. 43)

17

5. 27(0. 79-35. 17)

17

N.D.

6a 1.33(0.98-1.81) 7.94(1.28-49.31) N.D.

PVC 3 E E 1.63(1.18-2.26)

6b 1.22(1.12-1.34) 1.47(1.03-2.09) 1.36(0.90-2.06)

PVCZ 1 1.51(1.19-1.91) 1.88(1.04-3.41) 1.52(1.19-1.93)

2 1.24(1.08-1.43) 1.30(1.07-1.58) C

6b E 1.42(0.65-3.1) 1.09(1.01-1.17)

REDO 5 1.30(1.00-1.70) 1.78(0.69-4.62) H

6a 1.15(1.07-1.24) 1.32(1.06-1.65) H

8 1.07(1.03-1. 11) 2. 29(0.49-10.69) H

RPU 4 C C C

6b 1.10(0.95-1.28) C N.D.

8 1.83(0.15-21.68) C C

WOOL 2 1.39(0.97-1.99) 1.62(0.89-2.95) C

3 E 1. 22(1.10-1.36) E

6 1.60(0. 91-2. 83)

a 1.17(1. 06-1. 29) a 1.39(0. 82-2. 36)

b

8 1.86(0.83-4.14) 1.47(0.89-2.41) 1.15(0.87-1.52)

a: NBS small furnace

b: NBS large furnace

C: No slope as > highest concentration tested

D: No slope as < lowest concentration tested

E: LC estimated

H: 440 °C is greater than or within 50°C of non-flaming temperature

N.D

.

Not determined

17: Significantly heterogeneous data

19: Litchfield and Wilcoxon - reference 7. 20: Units are % Lethality
Table 25

Multiplication Factor Between Lowest and

Highest Value for Each Material3

Material Flaming Mode Non-Flaming Mode

ABS 1.4 1.7

DFIR 1.9 1.7

FPU c. 1.5

MOD 1.6 1.5

PPS 3.1 3.4

PSTY 1.6 c. PTFE 8.9 5.2

PVC 1.2 1.3

PVCZ 1.6 1.8

REDO 1.3 1.4

RPU 1.2

b

c. WOOL 2.6 1.8

Values calculated from LC^ values presented in Table 23

b. Data listed as > (greater than) in Table 23 were not used.

c. No value calculated as the LC,.q values in Table 23 were all higher

than the highest concentration tested.

73
Table 26

NfiS Control Blood Values for Fischer 344 Rats

Blood Parameters Mean Standard Deviation Number of Values

Total Hemoglobin (g/100 m l) 14.6 1.2 180

Oxyhemoglobin (X) 94.1 1.8 180

Carboxyhemoglobln (X) 1.7 0.6 180

Methemoglobin (X) 0.7 0.3 180

Volume X Oxygen (tnl/lOO mS,) 19.3 1.7 180

PH 7.44 0.06 173

Partial Pressure C0

2 (mm Hg) 35.0 4.1 151

Partial Pressure 0

2 (mm Hg) 95.6 8.1 138

74
Carbon

Monoxide,

Carboxyhemoglobin,

and

Hydrogen

Cyanide

Concentrations

at

LC50

(30

minutes)

and

ECggOO

minutes).

Mean

Carboxyhemoglobin

Concentrations

at

Time

of

Incapacitation

0) T3 0 U

*H (d EhU cd G

td i

CO+|0- <d S

cd *h o >

01 C Q1 E M Q

25 0 U CL

DC CL

K 5^ o ^

CJ

O 6 O CL U CL

Qoj

m-. O GO W 0

E 0 o a

DC cl

o 0 o P- CJ CL

C /->. °-H o? in0 V

U GO JOSCO w

+

CO

• >v o* oc td \ in*H TC GO O0 0

sf w

O rH co

O *H CL ^ L C 0O 3 00 fljo < H H

a) T3OE

vvo CO

v-/ V/

rH

• CM 00

rH • • rH lO IO +1+1+1

vO Ov O •

• • • a

<T O VO • VfHN Z

Q

(O vO Is • CM CM CO 53 OOO • m av o Q m m cn • rH 55

VO O O

OvON

rH «H

«?

OOOO

av m m 00

-3- m <* w

m av o co + 1 + 1 . CO VO Q

H rs 5s

mm •

• • av CO CM + 1 + 1 + 1 CM CM m

<r 00

• • av ov m rH • • H H CO +I+I+I+I

rH Mf rH O

+ 1— +1 MOO

w \o

N-X ^ W

-S’ m 00 • o • • rH • <f N rH m

+I+I+I+I

^3 oo >3-

co

+ 1 Q O

ovr^oo • m o m m vo n o> • h n o ov 'd-mmzmvor^r^ «^m»H55r^r***vor^*

<ro

+ 1 CM Q . • • CM cm 25 m

o <r m cm

<? Q

Q vO 00 • M HZ

OOO • CM CO av Q CO rH CM • 25 o 00 o •

w . . O

rH m co . CM CM 23

OOO -OOOO OOOQOOOO 00 CM vO • CO vO O rH HHHZHHCMN

o <t m • o 00 m ov ... o ... . O 00 <f • *} H CO O (MHHZHCMCMN

<? <? <?

vo q <r • m f" vo o '3-MCOZ^C^vOM

00000000 000000000 HHmcocou'vom

CM rH CM rH rH rH CM OrHvDOCMCOmM

OOO OOO CO CM Ov

Ov Ov M

CO

<?

OOOO co m cm o CO 00 'J 1^

*3 VO 00 H ooom

OQvOmrH<fCOQ vOHOOvOCOCOOOH

00000000 00000000 iH<rMMvDCO<rrH

CO CO CM CM CO CO CO CO

OHOVVO^OCOO

00000000 00000000 OOVOVH^NM-'J

COM-COCOM-COCOCO

Noicoovmcoom

OOO

CM CM O

O vo 00 <0 CO CO OV

mO'3-ooomavo to m cm to (O sj (O co

<?

COCOOvO^OOOCO r^vDoooov<room

+ + +

m m o m

cm m o m

m m m m

I + + +

m m o m

cm m o m m m m m

mrn't ovoohovov COstCMCMCO^COCM

<?

I I + CD C/3 + + I

vOvDSCO* mmmmommo 3 vOvOH

l 1 + w w + + 1

vOvONOOM’vOvOH mmmmommo m m o

Ov 00 m

co co co

Q .

* rH ZH

CM 00 rsj co <r ^

o o o o o o

^ o r,m

m vo cm

vo m vr,

c3 a o o o o O o CM 00 S

OV OV fs M O com

^ o ^ CM <r CM

+ I + + + +

m m o £^ 5COg £n

75
Matl.

Mode

Deaths

Lab.

Auto.-

Animals

LC

50

LC

50

CO

COHb

HCN

EC

50

CO

COHb

HCN

Mean

COHb

at

Time

of

//

Ignit.

Cannul.

30

min.

+

30

min.

(ppm)

(%)

(ppm)

(mg/j.)

(ppm)

(%)

(ppm)

Incap.

+

Standard

Temp.

14

days

(mg/ji)

Deviation

(n)

sr

oo oo

sr co + 1 + 1 O ON

o’ o*

CM m cm

co rH fs. +3 rH +1

# + 1+1

00 O H vO

sO Z sO CM

/s O

m

+ 1 00 • 00 • • P • P O • CM • m z Z

m

CM+ 1

• p • p O • CO . so Z Z

o

oo+ 1 oo

ONW

O'

rHrH+1 a • »—

1

• P^ m z^r

CMm

rH

# +1

p’ P* co

Z* z’ CO p o pz z’ z

POO • CO 00 z CM CM

Q

Q • Os Os M Z *H

O Q O O

O'* • CO vO Z CM CM

O Q 1 H N • Z z

O O O • O O Q o o o . rH CM CM Z V V

P CM CM O • in n n z

o o o • o o o p m -a- sr • rH rH CM z

P P. . vO

55 Z sO

O • O

O P

-a • rH z rH

p VO . SO A z A

o • o

O P

rH • A

A z

p p

55 z’

p p p

Z Z* z’

P P

z’ z’

p p p

z z’ z*

p • •

• cm CO

55 <?

. o cm

• P • • CM • CO CO

55 <?

00 o o •

• • • p 00 Ol N • rH V Z

o • r>. o oo <0 z <N o • o • p • o • o n z ^ z o o z in

P• co in Z rH CM O O O N CM vO m sr sr

P

q • co m

W Z *H »H o o o o rs o co cm

rH sr m sr o o o o

o o o o co so o in

co co co co o o o o

o o o o rH <r co m co cm co MT o o o

o o o m co co

CM CM rH O O

o o o

h vO p p p

55 55 z’ P P P

z* z z’

CO O O

n* m m

cm as m cm o so cm o cm o m oo n* m

<?

B

H

sr

cm oo o co

in r>* r-» m

O os in o

m co rH cm

<?

CO O N CO N CM N m

sr o m

SO O ST

rH <3- O m m m

cm co sr H CM O

m so rH as

CM CO rH rH

I I + 111 + + + I CO + I I + I I + I CO + C/0 +

o o m

<r rH cm r- r". m o O m

CM «3" H CM

r-.

+-m sr m o r^. as s3

- m

so so so so m sr m o rs as sr m so so so so o o o m m as

sr m sr o o o m in as

•a m sr o m o o m o

m oo cm m oo cm sO sO sO sO sO sO

76

I
QJ0

*H 03 H T3

fl w (fl C

cd -u ^

CO £ +i§

;

O -H

CJ • 4J a cd c cd -h

cd u >

CL) d d) E H P

53 e

cj a

33 P<

03

33 *3 O

CJ

o 6 O P< O P,

53 0

CJ P33 Po 0 O Pu CJ PC ^ O *H o* m 0 \

CJ 00

hJ o 0

CO w

CO

• ^ o* oc cdx

uo«h -a oc CJ 0 P P <r

• o «H

O *H P4J c 0 CJ P 00 0) o < M H NJp

cd : P

• m lA

vO+ c•

• ON

r* vo

o o

<r o CO rH

O lA vO 00rH

<?

o o

o o

CN ON

o CO

iA

rH rH

<?

iA O

CNvO vO

w O

ON CO

• rH

CN+ii

o o vO 00 CO 00

ON o

o o

o o

iH

o o

vO O

rH CN

<?

+ + + +

/-N CN CO w v-/ CO ^ • • ^ CN CN +1 +1 iA CN

co

V-K W

ON IA

*3- On

. +, + l . Q iA On Q O . . . . CN CN ss 00 r* 25

iA h«

V-/ CO ON

r- co + 1 + 1

• <r ^3- P • •

• 00 iA 2 >A N

• o co • CN co + 1+1

• a* ia P • •

• CN 00 2 IAN

+ 1

• • P Q •

• • rH

53 53 <T

O

sj- + 1

• • o

a o •

• • 00

53 53 IA

P Q Q

• O • ON ON . 2 iA 2 cn 25 o o • o o • H IA Q CN N Q

VO ON . CN lA • 2 2

o o o

o o o r^. vo

CN rH CN o o o

o o o

CN ON CO

CN rH CN

53 53 CO O • O

O Q 00

CN • 00

rH 53

oo cn • <3 r". • • • Q • • Q rH CO • lA H • HH 2 c> H 2

ia co <r

CN CN CN V <? <?

P G• • P

53 53 H

• • O

P P o • • CN 2 2 H

P P ON

• • CN

53 !3 <?

G O 00 On On ^ • lA vO CN >3- 53 A

O O O O O O

O O O ON rH O r>« H CN CO S >3 H CN rH O O O O O 00 ON CO

CN CN CO O O O

O O IA VD <r

CO CO co o o o

o o o CN 00 <3 o o oo o o v£> s N

3 3 CN vD CO O

CO ia IA ON lA <3 lA ON lA lA v£>

cf> O lA iA

<r co

<t co o vo co co

ON 3 iA O H

rH rH rH rH

«?

» + i + i + i i +

mo mmmmmm CN O IS CM N M N N

vO vD cC S) vO cO vD vO iAOO IAOO 3 O in

VO 00 rH vo 00 H ON lA H N *3 lA -3 -3 in ID IA vo

I +

3 O lA

ON IA H lA lA vO

77
Table

27

(com

u W a * u &

- " s i

+| i

“s!w

sS£

s*I

JN|S

sits

5r

Pifl w * of) P «

^ P

.*'• ©

e

m CM m w« o

fs id n in a

9>

i * in +I+I+I+I +i

CM

4. 1 +1+1 < CM H m o

“ 1 CM »> a

00H as a sO a60H

gg ss

77 pH

>45 48 28

<57 ID 23 39 26

520

1200 550

<1100

470 460 720 710

S6NW9 o con o a??s f»‘ se o! ** H H N

e

OSZ"^ 061 1

90

280

>46 57 47 57 esss

>1100 1600 1000 1400 aaa*

o oo os m H oo m H

o n o’ «

m cm 3 m

A ?

m* in as os

•0 pH CM CM

00 O CM O CM 00 pH m

cm cn oo © CM CM ©

f

in in m oo

CM pH CM CM

1 + + 1 1 + + 1

6601 695 650 675

660t

695 650 675

M PI 'C 00 Nnoto

fc 0.

E> #

Eh &

* SflS, " *

0) 0) Qj _ _ <S q*3 W V) w oo <3 H

DAUVMBZhJtH- + I 60 U. SE

78
Table 28

Distribution-free Sign Test on COHb Values at the LCjq (30 minutes + 14 days)

Material Mode

COHb Values (%) Mean ± S.D. (n) Lab 01 2 Laboratory Effectt

3 4 5 6a 6b 8

ABS F

NF

42.3 +

22.5 +

15.2(4)

6.4(2) -19.3 17.7 1.7 -4.5

-0.3

4.5

DFIR F

NF

76.3 +

75.0 +

10.8(6)

11.7(7) -15.3 -26.0

8.7 6.0 -12.3

3.0

4.70

7.7 5.0

6.7 6.0 6.0

FPU NF 57.3 + 5.8(3) 6.7 -3.3 -3.3

MOD FNF17.5 +

15.0 +

6.4(2)

1.4(2) -4.5 -1.0

4.5

1.0

PPS FNF

80.5 +

81.8 +

1.3(4)

6.3(4) 0.5

6.2 -0.5

-8.8 -1.5

0.2

1.5

2.2

PSTY F 74.0 + 6.1(3) 3.0 -7.0 4.0

PVC F

NF

45.0 +

23.5 +

5.7(2)

5.0(2) -4.0

-3.5

4.0

3.5

PVCZ F NF59.0 +

24.7 +

12.7(2)

14.0(3) -15.7 -9.0

4.3

9.0 11.3

REDO FNF79.7 +

78.0 +

5.8(3)

6.2(3) 3.3 -7.0

3.3 2.0

-6.7

5.0

RPU F 50.5 + 14.8(2) 10.5 -10.5

WOOL F

NF

50.8 +

35.3 +

7.3(4)

8.1(3) -4.8 6.2

3.7 -7.85.7

6.2 -9.3

Total Number of effects 4 6 8 6 10 9 12 6

Number Negative

Number Positive

effects

effects

4

0

24

2

6

5

1

54

2

7 1*

11

33

% Negative effects

% Positive effects

100

0 33.3

66.7

25

75 83.3

16.7

50

40

22

78 8.3 91.6

50

50

Number

Number Minimum

Maximum

effects effects

4

0

11

2

3 2

0

50

13

0

8

31

/ Minimum effects

% Maximum effects

100

0 16.7

16.7

2537.5 33.3

0 50

0

1133.3

0

66.7

5016.7

Mean: Mean of COHb values from all laboratories who tested material

S.D.: Standard deviation of mean of COHb values

(n) : number of values used to calculate mean

t : laboratory values minus mean value

F : Flaming NF : Non- flaming

a : NBS small furnace

* indicates ^statistically significant number of positive or negative effects at the 5% level, reference 14

79
Distribution-free

Sign

Test

on

COHb

Values

at

the

LC

(30

minutes) 01

00

eg

sO o0

4-1

4-1 w

m

fc* o

4J

rt

t-i sr o3

co

CN10

CM

CM

CM

r*»

00os

pH1

CMm

oo• CMNT

Crt

cost

in cn • • som co • • r>. m m

srm co • • H O pHI m co • • OS Nf m• • SO pH

pH CM I I

sO SO

pH Os • • H O

pH pH

P4WQ

OO• • sO H O O• • SO pH I I

CM CM m *o • • 00 H

00 CM • • o o

00 CM • • pH O

CM 00 • • O oo I I

CM CM • • O so I

sr «o o co • • pH SO

O

Nf

© o• • Os O 0

r>-1 O

CO 0

OS1 ©0

pH1

CO CM CM

pH Is* pH • • • SO CM Nf

co

m• • CO oI I

r»

m• • pH O

CO CM

Os f- • • CM O 0

SO1 o

sO

CM

in

00

CO CO • • CO osI

1^ o* • • so mI

co r- • • CO CO

CO co

00 pH • • in oo

m o o CN 00 o o o co

m o i-n CO CO CO • • • • • • • • • • • • • • c0

05 CO 4-1 4-1 co 0

so 00 On ^ iH tH sr Os OS rH *'3‘ r- co

m 4J 0 0 0 0 CO CO 0 0

rv rH fH 00 00 r>

m pH 00 00mm co

O

O

O 0 0 4J 4J 0 0 0 0 0 4H 4H 0 0 0 0

4-4 4-4 4-1 4H 44 0 0 44 44 4H 4H 4H 0 0 4H 4-4 44 4-1 0 0 0 4H 4H 0 0 0 0 0 0

pH 2 Ph 2 Ph 2 P< Ph 2 Ph S 1 w

pHPh

CO

Ph

No>

Ph i3

*o cm f* co -o

© n»o so co so

oo o oo oo ©m o co o so

00 pH n. CO S pH CO CO 00

pH 00 pH CO

oo cm so mm cm cm mm CM Is* CM CM m Nf pH OO CM O OO oo cm -a- m om oo o cm oo o sf

CM CM OO pH pH mm mm cm cm

-a- o o o <o o

4HOM

0)

rt 0oH 0 a) > >

•H -H 0 4-1 CO *pl 00 CO

01

O

fl

a

MM 0 0 2 2 > >

•H iH 0 0 0 pH oo m 0 o 0 PH

4J 4J 0 0 0 0 O O M U 0 0

Ph Ph 0 M 0 0

SB S3 0 0 0 0 O O 0 0 0 0Ph Ph

oo

CM300

0500

0000£

80
Distribution-free

Sign

Test

on

COHb

Values

at

EC

oo

iJQ VO

+-

4-1 CJ

a)

4-4

cd vO

w

m om

Fmo

cduoXcd HI

00

CMXcd HI 6M

cd >CO

x

Pdoo

a) T3

cd

•rlP4

CU

4-4 cd S o m• • vO 00 I I o <r m o

rH VO i-1

00 oo

rH iH

O

VO !"• iH

oo• • <r <f omi o m o

vo oo o ov

rH

LO

O• • m vo o -m- • • oo m om

co r*o CM oo m o• • m vo i l O vo !•". 00 ov mCMI

oo

m

CM rH I i m o• • 00 oorH rH I I O CO • • O vO

iH I Oo o

rH

O VO

CO CO

CM rH I I oo

iHI

CM CM

m

m oo co CM CM CM CM CM CM CM CM CO

00O

V0 vO

00 OV

CO CM

Pm

Pm 3

Pm

Pm !3

Pm

Pm 3

Fm Pm !3

Fm

Fm 13

Fm

Pm 3

co

pj

PmQ P3PM

Fm §a

CO

PM

P-l

CJ>

PM

CMo>

PM

On§HIOO&

00

CO

4-1 O

CD

<4M

MMOU

a) X

cO

4-4 oH

81

COO OO CM o r^-o O vo

rH <3- o oo o oo om o rov CV| IN CM 00 CM in CM vo

(M IV. CM in

m iH<r oo o co oo CM 00 vo

CO

O 00 o oo

rH

co co

4-1 4-4 o a

<U cu MM MM

4M 4M

CU (U

a) cu 3.3

4-1 4-1 cd *H 00 CO <u o

CP PM u u

<U (U la 'a

53 53

rH CM CO S

CO vo

O 00 CM OO 00 iH OO rH 00 CM 00 rH

CM rH rH OO

HH OO mm mm

co coo oo cm o n- o o vo

co co

4-1 4-4 CJ o

CU CU 4M 4M

4M 4M

cu cu

cu cu > >

•H *H

4-1 4-4 cd *H

00 CD

CU

O

C PM

CD CD

4-4 4-4 CJ CJ CU CU 4M 4M

4M 4M

CU CU I i

•H *H

4-1 4-1 PS CJ

CU <U O CJ Fm Fm

(U <U PM PM

UU

CU (U *s a

pj pi 3 3

CD CD

4-1 4-1 O CJ

(U CU 4M 4M

(U cu g § a a

CJ •Ha

x

4-4 CJCU <u

CJ CJ

Fm Pm

CU CU Pm CM

00

CMX

cd HT3

CJcuW

(U

FmO
Table 31

Diatribution-free Sign Test on COHb Values at Time of Incapacitation

Material Mode

COHb Mean

Values

S.D. W

in) Lab 9 1 2 3 Laboratory Effect

4 5 6a 6b 8

ABS F 27.2 16.9 (3) 17.4 -16.3 - 1.2 NF 4.5 4.5 (2) - 3.2 3.1

DFIR F 61.8 9.7 (7) -12.6 - 4.6 - 3.3 - 4.7 - 1.4 13.3 13.2 NF 58.9 21.1 (7) -12.2 - 1.3 -39.9 12.8 18.5 1.9 20.5

FPU 7 27.5 35.7 (2) -25.3 25.2 NF 9.6 3.2 (2) - 2.3 2.2

MOD F 10.5 0.6 (2) - 0.5 0.4 NF 5.2 2.3 (3) 1.6 0.9 -2.6

PPS F 61.8 15.6 (2) -11.0 11.0

NF 66.6 9.2 (2) - 6.5 6.5

PSTY F 49.3 2.9 (2) 2.0 -2.1

PVC 7 38.5 43.7 (2) -30.9 30.9 NF 15.8 17.7 (2) -12.5 12.5

PVCZ 7 23.9 4.7 (2) - 3.4 3.3 NF 8.2 0.4 (2) 0.3 - 0.3

REDO 7 66.9 12.0 (2) - 8.5 8.5 NF 65.6 18.2 (2) -12.9 12.9

WOOL F 29.1 11.1 (4) -0.7 -10.9 - 4.0 15.4

NF 17.7 7.7 (4) 3.3 -11.0 6.5 1.2

Total number of effects 5 10 10 - 8 10 5 6

Number negative effects 3 6 10* _ 3 5 1 o* Number positive effects 2 4 0 “ 5 5 4 6

Percent negative effects 60 60 100 • 38 50 20 0 Percent positive effects 40 40 0 — 63 50 80 100

Number minimum effects 2 3 9 _ 1 3 1 0 Number maximum effects 2 3 0 - 3 4 3 4

Percent minimum effects 40 30 90 13 30 20 0 Percent maximum effects 40 30 0 38 40 60 67

fFor legend, see Table 28
NBS-H4A (rev. ?-{'OI U.S. DEPT. OF COMM.

/

U.S. DEPT. BIBLIOGRAPHIC DATA

SHEET (See instructions)

1. PUBLICATION OR

REPORT NO.

NBSIR 83-2678

2. Performing Organ. Report No. 3. Publication Date April 1983

4. TITLE AND SUBTITLE

AN INTERLABORATORY EVALUATION OF THE 1980 VERSION OF THE NATIONAL BUREAU OF STANDARDS

TEST METHOD FOR ASSESSING THE ACUTE INHALATION TOXICITY OF COMBUSTION PRODUCTS

5. AUTHOR(S)

Barbara C. Levin, Maya Paabo and Merritt M. Birky

6. PERFORMING ORGANIZATION (If joint or other than NBS, see instructions) 7. Contract/Grant No. national bureau of standards

DEPARTMENT OF COMMERCE

WASHINGTON, D.C. 20234

8

.

Type of Report & Period Covered

Final Report

9.

SPONSORING ORGANIZATION NAME AND COMPLETE ADDRESS (Street. City. State, ZIP)

10.

SUPPLEMENTARY NOTES

| | Document describes a computer program; SF-185, FIPS Software Summary, is attached.

11. ABSTRACT (A 200-word or less factual summary of most significant information. If document includes a significant

bi bliography or literature survey, mention it here) Seven laboratories selected from academia, industry, and government evaluated the 1980

version of the NBS test method for assessing the toxicity of combustion products to

determine the operability of the procedure and the reproducibility of results across laboratories. The experimental design specified that each laboratory was responsible

for testing Douglas fir and three other materials from a total of twelve natural and

synthetic materials. All laboratories were required to use similar exposure and com- bustion systems, to measure the autoignition temperatures of their materials, to

determine the toxicity of the gaseous products released by the materials under both

flaming and non-flaming conditions, to monitor chamber environmental conditions

(temperatures, and oxygen, carbon monoxide, and carbon dioxide concentrations), and to

measure blood carboxyhemoglobin in the test animals (rats). In addition, a few laboratories measured hydrogen cyanide generated from nitrogen—containing materials.

Toxicity was evaluated on the basis of incapacitation (hind- leg flexion beharioral

avoidance response) during the 30 minute exposure and of lethality during the exposure

and 14 day post-exposure observation period. The results of this interlaboratory

evaluation were statistically analyzed and, in most cases, demonstrated reproducible

results across laboratories. Possible reasons for any inconsistencies are discussed.

Sensitive, experimental factors are identified and modifications to the test method

which resulted from the experimental data collected during the interlaboratory

evaluation are described.

12. KEY WORDS (Six to twelve entries; alphabetical order; capitalize only proper names; and separate key words by semicolons)

Carbon monoxide; carboxyhemoglobin; combustion; combustion products; hydrogen cyanide;

inhalation; interlaboratory evaluation; LC^; test methcds; toxicity.

13. AVAILABILITY 14. NO. OF

PRINTED PAGES

|~X~1 Unlimited

| | For Official Distribution. Do Not Release to NTIS 88

| | Order From Superintendent of Documents, U.S. Government Printing Office, Washington, D.C.

20402. 15. Price

[32 Order From National Technical Information Service (NTIS), Springfield, VA. 22161 $11.50

U S COMM- DC 6043-P80


i

1

i,