Fire Research Information Service

National Bureau of Standards

sR^OOQOcS/

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NBS PROJECT NBS REPORT

1002-43-1029 February 6 , 1952 1434

COMBUSTIBILITY TESTS

OP

47 ASTM MATERIAL SAMPLES

by

Nicholas P. Setohkln

Ihia report ia iaaued

in any form, either in

from the Office of the

Approved for public release by the . . .

. n 1 XT • • tion, reprinting, or reproduction

Director or the NstlonQl Institute of penniaaion in writing is obtained

Standards and Technology (NIST) Waahington 25, D. C. on October 9, 2015.
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COMBUSTIBILITY TESTS OF 47 ASTM MATERIAL SAMPLES

toy

Nicholas P. Setchkin

ABSTRACT

Tests of 47 specimens of solid materials as requested by the advisory group to Subcommittee V,

ASTM Committee E-5 on Fire Tests of Materials and

Constructions were made at the National Bureau of

Standards for the purpose of evaluating a technique for determining the combustibility classifications of solid materials. Results of these

tests indicate that by using the technique proposed for adoption by ASTM, the specimens, except

for a few, could be readily classified as combustible or incombustible. The results for those fev;

were not conclusive and seem to require further

definition of the procedure and method of classification.

I. INTRODUCTION

The advisory group of Subcommittee V of ASTM E-5 has pro-

-posed the use of a small furnace type of combustibility tester

to evaluate the fire-hazard properties of various solid materials. This report presents the results of tests made with

this device on each of 47 solid materials which are being

tested independently by -seven laboratories.

II. OBJECT

The objective of the tests was to classify each of the 47

solid materials as to their combustibility characteristics for

the purpose of comparing experimental results with those obtained by workers in other laboratories.

- 1-

•III. TEST APPARATUS

The National Bureau of Standards ignition apparatus for

8oli<is, figure 1, was used for these tests.

a. Construction

The apparatus consists of a small cylindrical electrically heated furnace. A refractory tube 4 in. inside diameter

by S 3/4 in. long forms the cavity. A second refractory tube

3 in. inside diameter by S 3/4 in. long is supported v/lthln to

provide the combustion chamber of the furnace. The Incoming

air is preheated to furnace temperature in the annular space

between the two tubes. It enters the bottom of the combustion

chamber, rises around the specimen, and leaves through an opening in the furnace cover. This opening is also used for observation of the behavior of the specimen within the furnace. For

certain tests, a gas pilot flame burns above the opening in the

furnace cover. The plug at the bottom of the furnace facilitates removal of residue collecting during the tests.

b. Electric Power Supply

The furnace was normally operated from the laboratory

120-volt power supply lines through a variable ratio autotransformer. In some tests involving high air velocities, it

was necessary to use up to 220 volts. The auto-transformer was

adjusted to provide an output of 6o volts for the first five

minutes after which it was gradually increased during the next

30 minutes to about 90 volts, corresponding to a power consumption of about 500 wattfl. The power consumption of the furnace

varied with the rate of air flow and the operating temperature.

The maximum safe operating temperature of the furnace is 1000® C.

c. Air and Gas Supplies

The compressed air was reduced from the line pressure of

125 Ib/in.*^ to 30 lb/in.2 by means of a pressure regulator. A

needle valve and dry gas meter were used to control and measure

the air flow rate. Most tea^ts were run with an air velocity

past the specimen of about(7/to 15 ft/min under the temperature

conditions Involved. The rajte of flow required depended upon

the material under test and /the rate of its decomposition

reaction. ^ g' zs The velocities corresponded to volumetric rates of air

flow at 70® F of from about O.09 to O.17 ft3/min for the particular apparatus used during these tests. Air velocity has

been reported in the tables in preference to volumetric flow

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rate because it is believed that the velocity of the air past

the specimen is the critical variable. For a given volumetric

flow, this velocity i/ill depend upon the dimensions of the furnace and specimen. The rate at which air is supplied must be

a compromise between the need of oxygen for the reaction leading to ignition and the need for regulating heat losses from

the specimen resulting from a high rate of air flow.

Variations of air velocity past the specimen are not likely to cause difficulty in the classification of specimens which

consist largely of combustible material. However, for materials

having very low combustible content the use of high air velocities past the specimen may obscure the flaming or self-heating

which would otherwise be noted. High air velocities also have

the disadvantage of requiring excessively high rate of power

consumption within the furnace as indicated on chart 20.

The gas pilot flame, when used, was adjusted to provide a

flame about 3/^ in. long. However, this pilot v/as not used

during most of the tests because the heat from the furnace wall

provided an adequate ignition source.

d. Thermocouples

Thermocouples were mounted as shown in figure 1. Thermocouple T]^ followed closely the heating coil temperatures; T2

indicated air temperatures below the specimen; T^ served as an

indication of surface temperature of the specimen while T3 was , used in measuring temperature within the specimen, 'V

During most of the tests, thermocouples formed from Ho, 26

B&3 gage chrorael and alumel wires were used because of their

quick response. In some tests conducted with treated wood it

was necessary to use thermocouples made from Ho. IS B&S gage

wires because of excessive corrosion of the finer wires. Calibration data for these wires are presented in table 1,

Table 1. Calibration of thermocouples of Hos. IS and 26

B&3 gage chromel and alumel v/lres

Temperature

‘ Electromotive force developed by

t Ho. IS gage wire ' Ho, 26 gage wire

op ' mv ‘ mv

200 ' 3oS0 ' 3.22

4oo ' S.30 ' S.27

600 ' 12, S5 ' 12.7s

SOO ' 17.55 ' 17.39

loOo ' 22.26 ' 22.15

1200 ’ 27.05 ' 26.90

1400 ' 31.70 ' 31.65

1600 ' 36.25 ' 36.20

ISOO • 40,63 ' 40.6s

2000 ! 1 45.00
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e. Size of Specimen

The size of the specimen tested varied with the type of

material but in most cases was cut 1.5 wide; 2 in. long,

and not over 1.5 in. thick. For thin sheet materials, a number

of sheets were assembled to provide a thickness of not less than

1/4 inch, boose materials, such as mineral v/ool, v;ere either

made into a bundle 1.5 x 1 x 2 in. or were Inserted in a wire

screen container having these dimensions.

IV. TEST PROCEDURE

After warming up the furnace and adjusting the rate of air

flow to that required for the test, the furnace temperature was

adjusted to 13^3 15° F as indicated by the thermocouple Tp.

The temperature of the heating coils was observed with the thermocouple T^. A specimen with attached thermocouples Tv and TJ4

. was fastened to a v;ire and lowered to the middle of the furnace

tube. Observations were then made of the behavior of the specimen with particular reference to flaming or glowing. The timetemperature data were also recorded for both the surface and

interior of the specimen. During these observations, the temperature of the furnace coils at Ti was maintained constant

regardless of changes of air temperature at T2 » Self-heating of the specimen was taken as another indication

of combustibility and was observed during the tests by a rise of.

the interior temperature of the specimen above the initial temperature of the air in the furnace.

The rate of rise of temperatures at the surface and in the

interior of the specimen at the beginning of the test were not

considered of great significance since these vary considerably

with test conditions such as air-supply rate, sample size, and

locations of the thermocouples in the specimen with respect to

the point of ignition or region of maximum self-heating.

The duration of the test varied with the characteristics of

the material tested. Definitely combustible materials usually

required only 3 to 5 minutes for classification. Incombustible

materials, on the other hand, usually required longer exposure

periods to permit observation of temperature changes within the

specimen. In most cases, the test period did not exceed I 5 to

20 minutes.

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V. TEST RESULTS

The results obtained from tests on the samples of the 47

materials are prese?ited in tables 2, , and 4 . Time-temperature data, together with some notes on observations of the

specimens during test, are presented in the charts included

in this report.

Table 2 lists materials which can definitely be classified as combustible, as evidenced by flame, self-sustained

glow, emd/or pronounced self-heating.

Table 2. OEnNiYELV combustible materials

Code chart MATERIAL

Ev 1 DENCE

Flame or glow ' self1 OURA- 1 „0N LCNQTH TlQisJ SUR— ' ' FACE

•HEATING

. IN .CENTER

4 AIR 1 VELOC-i

ITY .1

Remarks

USL. tiSL. IMi. 'hlh S£C' 2L OF

i-i 1 asphalt CANVAS (2 SHEETS) 3 • 0 25 • 75 235 15 ' Very dense smoke

1-1 1 DO (l sheet) 2 0 20 t — 267 15 ' Do

i-i 1 Do DO 2 • 0 2? 1 — 207 15 ' Do

1-2 1 asphalt paper (2 sheets) 4 •

1 45 • 97 t 145 15 ' Do

1-2 1 Do ( 1 sheet) 2 • 0 55 •

l 57 — 15 ' Do

1-3 2 DO (2 sheets) 6 •

1 45 1 21 7 -

15 ’ Do

1-3 2 DO (

1 sheet) 3 ' 0 55 1

1 1 7 — 15 ' Do

1-4 2 RED asphalt board 4

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1 45 1 160 • — 15 ' Do

1-5 2 ASPHALT PAPER (2 SHEETS) , 6 • 0 55 1 167 — 15 ' Do

1-6 3 Do DO 8 • 2 40 1 240 • — 15 ' DO

1-7 3 1 /2- INCH asphalt board 8 ' 3 20 1 297 9 23 7 12 ' Violent burning

1-0 4 1 /I 6 -IN. CARDBOARD (2 SHEETS) 5

' 0 25 t 257 1 — 15 ' Dense smoke

1-13 6 ASBESTOS asphalt (2 SHEETS) ^2 '1 07 ' 272 1 — 15 • glow, light smoke

1 1-i 6 DOUGLAS riR (treated)

'

' 2 t p BLUE 2 00 1 387 t 287 18 ' Intense glow

11-2 7 DO DO -^2 *3 45 1 270 1 287 18 ' Do

1 1-3 7 Do Do ^2 *4 50 t 367 • 24 7 18 ' Do

1 1-3 7 DO DO 2 • 7 00 • 92 1 157 130 ' INTENSE BURNING

Vl-1 9 Eagle insulation satt FLASH' 0 25 t — » 167 12 ' Dull glow

VI -2 1 0 ROCK WOOL (loose) FL&GL' 0 20 1 — f 237 12 ' held by wire

Vl-2 1 0 Do do FL&Gl' 0 30 — t 297 13 ' held in wire SCREEN

VI -2 10 DO DO No FLAME — 1 137 143 ' Do

IX-l 12 GLASS WOOL PAD (h|GH DENSITY) ~2 *0 25 — 1 175 8

' DULL GLOW

lX-4 1 3 DO DO 2 • 3 30 67 1 157 10 ' DO .

' lX-5 13 Do Do 2*1 15 202 1 67 10 ' Do

XI-1 1 4 Douglas pir 6 • 5 53 ' 437 1 317 10 ' below

XI-2 14 Yellow pine 6 ' 6 30 407 I 387 8 &l 1 ' Do

Xl-3 IS Poplar 8 ' S 20 525 1 372 16& 8

' Do

XI-4 1 5 Douglas fir (treated) 2 ' 6 1 0 342 1 257 10 ' Do

XI-5 1 6 Do Do 5 '10 00 377 1 292 10 ' • Do

XIV-I 1 7 Oak Do ~ 2 '12 30 432 f 357 9

' Do ! ^ XIV-2 1 8 Poplar do ^2 '12 00 t — 1 (147) 10 ' Fall to bottom

XlV-2 1 6 Do DO (i size) <^2 '7 00 1 '24 7

' 267 10 ' DO

XlV-3 1 6 Birch Do '12 30 1 277 1 347 10 ' Burning gas below >

1 1 • 1 SPECIMEN

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Table presents a tabulation of materials which are definitely classified as incombustible by the test. These

samples produced no flame or evidence of self-heating.

Table 3. oef»nitely incombustible materials

Code •chart*

1 1

f-.'. tr«i Ai. 1

1

EVIDENCE AIR

VELOCITY

t FUSION

Flame or glow self-heating’ TEMPERATURE Time

tiSL.

'J- £l/{llN ££1 lilli 1-3 4

1 l/8-IN. ASBESTOS CEMENT board’ None None f 15 1 —

l-l 0 4

t l/8-IN. ASBESTOS CEMENT6HINQLE' DO DO 15 1 —

l-l 1 5

1 1/4-IN. ASBESTOS CEMENT PLATE' 00 OO 15 1 —

1-12 5

1 l/4-lN. OO 1 00 00 15 t — —

: 1 1-2 8

« 3/4 -IN. KaVLO MAGNESIUM BLOCK ' 00 DO 10 t - .. IV-1 8

1 5/8-1 N. Do • DO DO 10 1 — —

VI l-l 10 1 ROCK WOOL (loose) DO DO t 12 1 — —

VII-2 10 1 ROCK WOOL BATT I DO 00 12 • —

VII l-l 1 1 1 ALUMINUM ALLOY SHEET 1 — 00 8

1 1300 4 20

VII 1-2 1

f 00 1 — DO 8

1 1285 8 00

VII 1-3 1 1

1 Do 1 — DO 8

t 1300 3 40

VII 1-4 1 1

1 Do — DO 8

1 1310 4 30

VII 1-5 t 12 t Do 1 — Do 8

1 1232 4 00

VIII-5 12 1 Do 1 — Do 6

1 1270 4 20

IX-3 13 1 Glass wool pad •

• lo.'ii: Do 10 1 —

IX-5 13 1 00 • DO 00 130 1 - —

X-l 13 • magnesium alloy BLOCK t Oo Do t 10 1 - -. --

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Table 4 lists materials of minor combustible content.

These materials exhibited brief flaming and little or no selfheating. They usually consisted of incombustible material

with either a covering or admixture of a small amount of combustible material. The final classification of materials of

this group should be made in accordance with adopted definition

of combustible and incombustible materials.

Table Materials of uncertain classification

1 t

1

1 Evidence

«

• AIR

velocity Code 'Chart* Material f Flame or glow ' self-heat 1 NO •

1 1

• t

1

1 1 NTENS 1 TY ; DURAT 1 ON | SURFACE i CENTER'

jLta. •nui I 2L

• OF • ft/m IN

1 i l-l 6 ' asbestos paper (5 sheets) f flash • 0 05 1 None * NONE ' 10 V-l 9

' Painted steel plate ~ 2 ' 0 20 1 DO * DO ' 12 Vl-I 3

' Eagle insulation batt Flash ' 0 10 1 DO * DO ' I2e

lX-2 12 • GLASS wool pad • Flash • 0 10 I Do * Do ' 10 XI l-t 16 • i/2-iN. plasterboard 2 •

1 20 « DO * DO • 10

XI 1-2 16 ’ i/2-in. plasterboard t 2 * 1 25 DO * DO ' 10

XI 1 l-i 1 7 ' l/2-IN. PLASTERBOARD 3

•

1 25 — • 35 • 10

VI. DISCUSSION

a. Evidence of Combustibility

The combustibility of materials with respect to their

fire hazards was Indicated during the tests by flame, sustained

glow, and/or self-heating.

The flame was characterized by color, intensity, and duration. The color of the flame, orange, blue, and light purple

(clear), seemed to indicate about the same degree of fire hazard. However, the intensity combined with duration of flaming

may indicate different degrees of fire hazard, intense flames

or those of long duration naturally represent hazards of higher

degree than the weak ones or those of only a few seconds duration. The latter types of flame were observed in the tests with

asbestos paper (sample III-l)’^ glass-wool pad (sample IX-2),

painted-steel plates, and other materials of minor combustible

content, listed in table 4 as "uncertain".

'^Numerals in parenthesis indicate the Code numbers in tables.

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Theoretically, the materials of the "uncertain" group are

also combustible. However, from a practical point of view,

this classification should probably be modified to "minor combustible content" if the effect of the combustible component

can be considered negligible in comparison with the large proportion of incombustible basic material.

Glow and self-heating may be considered as evidences of

different degrees of the same ignition characteristic. Temperature conditions in the specimen in which a bright red or

yellow color was visible, that is 1550® ^ above, were produced by the process of self-heating. They are commonly referred to as "glow" whereas, temperature conditions below

1550® indicated by the thermocouple measurements, have

been called "self-heating". Slow self-sustaining combustion

is distinguished from both rapid combustion with flaming and

self-heating (which may include glow) sustained only by the

high temperature of the surroundings. The glov/ which continues

after the material has been removed from the furnace is defined

as "sustained glow" and shows definite evidence of combustibility

Self-heating without sustained glow or flaming is not

necessarily evidence of combustibility of the material as a

whole. However, self-heating of materials to high temperatures

would present a definite fire hazard to materials of low-ignition

temperatures stored nearby or in contact with the self-heating

material. For example, asbestos Insulation containing over

5 percent of combustible components when heated to 500® F

(260® C) has further self-heated to 1110® F ( 6OO® C). This

would almost certainly cause the ignition of paper, wood, or

other low-ignition temperature materials stored nearby. Therefore, evidence of appreciable self-heating must be considered

as- a characteristic of combustible materials.

The extent of self-heating that should be permitted before

a material is reclassified from minor combustible content to

combustible is uncertain. U. 3. Coast Guard Specification

W164.009, which uses a similar test method to the one mentioned

here, allows a temperature rise of IS® F (lO® C). Experience

with materials being evaluated for compliance with this specification indicates that this is a very conservative limit and

that a temperature r^se of 5^® F (30® C) would be more practical.

Previous experiments'^ involving the fire hazard of asbestos

chimney insulations, acoustical tile, and other materials have

shown that the carbon content of the material in question was

well correlated with the combustibility characteristics. In

order to establish Justifiable limits for the self-heating,

''^N. P, Setchkin and 3. H. Ingberg, Test Criterion for an

Incombustible Material, A3TM Proc. V. ^5, pp. S66-S77 (19^5)-

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flashes, and short flaming, it seems desirable to conduce largescale experiments with materials of the uncertain group or those

of minor combustible pontent.

b. Time-Temperature Curves

The rising temperature in the specimen was observed at

convenient times and recorded in millivolts on cross-section

paper; the paper was also graduated in degrees F or C. This

procedure was found to be more suitable than recording in a

table at specified intervals because the trend of the timetemperature curves and accidental errors can be noticed at

once and correctly judged in respect to other data. Moreover,

any kind of observation can be recorded on the same sheet in

respect to observed time.

The time-temperature curves, obtained with the thermocouples placed on the surface and in the mass of specimens,

have only relative value for the indication of maximum selfheating occurring on the surface or within the material. The

shape and relative position of the curves, with respect to

observed time, vary with location of the thermocouples, air

velocity, and distance from the locus of ignition. Therefore,

these curves should not be treated as precise characteristics

of the material.

The magnitude of the self-heating should always be measured as an increase above the temperature indicated by the

air thermocouple To prior to inserting the specimen within the

furnace, but not above the actually observed air temperature

at the time of test. The reading of thermocouple T2 was often

affected by radiation from the specimen or combustion of gases

below.

c. Effect of Air Velocity

Changes in air velocity around the specimen produce various effects depending upon the material tested. The intensity

of the flaming of highly combustible materials ordinarily increases with the increase of air velocity (sample II-3), but

for materials of lower combustibility this flaming may be reduced so much that a material of an uncertain group can be rated

as combustible with low air velocity and as incombustible with

high air velocity (samples VI- 1 , IX-5 ). Moreover, the magnitude

of the self-heating of the material decreases with increased air

velocity as shown in chart 7 (sample II-3), chart 9 (sample VI-l)

chart 10 (sample VI-2) and chart I3 (sample IX-5).

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The supplemental tests conducted with mineral wool and

glass wool of high densities (samples A and B, chart 19) also

Indicated different -effects, of high and low air velocities.

The combustibility of mineral wool (sample A) in air of

12oS-ft/min velocity was indicated by a bright orange flame

during a period, and in air of 12S-ft/min velocity by

a short blue flame for only 40 seconds, with substantially the

same self-heating of the material. The behavior of the glass

wool sample B with velocities of 13.7 133 ft/rain were about

the same. A short flame was observed for 40 and 30 seconds, respectively, but self-heating of the material was not observed.

d. Size of Specimen

The most favorable size of specimens for this furnace

appears to be about 1 1/2 in. wide, 2 in. long, and from 1/2 to

1 in. thick. G-reater thicknesses* would tend to restrict the

free passage of air between the furnace wall and the specimen,

thus making observation of the flame difficult. Very thin

sheets or plates of material also are not favorable for observation of the self-heating of materials. Therefore, a few

sheets should be assembled into one specimen in order to

Increase the total thickness of a test specimen to not less

than 1/4 inch.

e„ Electric Current Supply

A current of 120- or 220-volt potential was used for heating the apparatus, depending upon selected air flow. The current input and temperature of the heating colls was Increased

rapidly with the air flow as shown on chart 20. The maximum

temperature for the refractory tube and coll protection was

not allowed to exceed IS32® F (lOOO® C). Therefore, for long

service of the apparatus and its economical operation, it would

be advisable to keep the temperature below this limit.

VII. CONCLUSION AND RECOMMENDATIONS

The above test results and discussion indicate that the

Ignition and combustion characteristics of materials are usually

well defined by the method tentatively adopted by Subcommittee V

for the classification of combustible and Incombustible materials

The uncertainty of classification for a few materials can probably be resolved by further refinement and definition of the

test conditions.

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One teat condition which should be modified for uniformity

of results is the rate of air flow. This rate should be so

adjusted that air velocity around the specimen (about 7

15 ft/min) would be favorable to the development of ignition

reaction in the material subjected to test and at the same time

avoid excessive heat losses. A second item is related to procedure in the observation of major evidences of ignition that

Involve the intensity and duration of flaming or sustained glow.

The attention of an observer should not be diverted to the observation of the initial portions of the time- temperature

curves, which have no practical value until they approach the

maximum. The main significance of the time-temperature curve

is that it indicates the maximum self-heating of the specimen

or that no self-heating has occurred.

Difficulties in defining a few materials with properties

placing them in the boundary zone between combustible and incombustible types wbre to be expected, and complications arose

as to their classification particularly in view of practical

applications. Therefore, the fire-hazard characteristics of

materials of uncertain classification should be determined in

large-scale tests, and the results correlated with the above

data and the limited percentage of combustible components

components permitted in the material.

On the basis of already available data, the following

recommendations are suggested:

The limit for combustible components in incombustible materials should not exceed 3 percent.

Duration of flame at 13 ^3

° F should not be more

than 30 seconds. Self-heating should not exceed 5^® F (30® C) above the initial temperature

in the apparatus.

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