This report has been prepared

for information and recordpurposes and is not to be referenced

-+B-afly publication,

NATIONAL BUREAU OF STANDARDS REPORT

9335

INTERLABORATORY COMPARISON OF

THE POTENTIAL HEAT METHOD

by

D. Gross

NBS

U.S. DEPARTMENT OF COMMERCE

NATIONAL BUREAU OF STANDARDS
THE NATIONAL BUREAU OF STANDARDS

The National Bureau of Standards is a principal focal point in the Federal Government for assurn,. maximum application of the physical and engineering sciences to the advancement of technology

in industry and commerce. Its responsibilities include development and maintenance of the national

standards of measurement, and the provisions of means for making measurements consistent with

those standards; determination of physical constants and properties of materials; development of methods for testing materials, mechanisms, and structures, and making such tests as may be necessary. narticularb for government agencies; cooperation in the establishment of standard practices

for incorporation in codes and specifications; advisory service to government agencies on scientific and technical problems; invention and development of devices to serve special needs of the Government, assistance to industry, business, and consumers in the development and acceptance of commercial standards and simplified trade practice recommendations; administration of programs in cooperation with L nited States business groups and standards organizations for the development

of international standards of practice; and maintenance of a clearinghouse for the collection and

dissemination of scientific, technical, and engineering information. The scope of the Bureau’s

activities is suggested in the following listing of its three Institutes and their organizational units. Institute for Basic Standards. Applied Mathematics. Electricity. Metrology. Mechanics. Heat. Atomic Physics. Physical Chemistry. Laboratory Astrophysics.* Radiation Physics. Radio Standards

Laboratory;* Radio Standards Physics; Radio Standards Engineering. Office of Standard Reference

Data. Institute for Materials Research. Analytical Chemistry. Polymers. Metallurgy. Inorganic Materials. Reactor Radiations. Cryogenics.* Materials Evaluation Laboratory. Office of Standard Refer- ence Materials. Institute for Applied Technology. Building Research. Information Technology. Performance

Test Development Electronic Instrumentation. Textile and Apparel Technology Center. Technical

Analysis. Office of Weights and Measures. Office of Engineering Standards. Office of Invention and

Innovation. Office of Technical Resources. Clearinghouse for Federal Scientific and Technical

Information.**

•Located <t Boulder, Colorado, 80301. ••Located at 5285 Port Royal Road, Springfield, Virginia, 22171.
NATIONAL

NBS PROJECT

421.02-12-4212127

NATIONAL BUREAU OF ST*

for use within the Government. I and review. For this reason, the whole or in part, is not authori Bureau of Standards, Washingto

the Report has been specifically

BUREAU OF STANDARDS REPORT

JUN2 218S6

NBS REPORT

9335

INTERLABORATORY COMPARISON OF

THE POTENTIAL HEAT METHOD

By

D. Gross

IMPORTANT NOTICE

Approved for public release by the

Director of the National Institute of

Standards and Technology (NIST)

on October 9, 2015.

s accounting documents Intended

tubjected to additional evaluation

listing of this Report, either in Office of the Director, National

the Government agency for which

iples for Its own use. <NBS>

U. S. DEPARTMENT OF COMMERCE

NATIONAL BUREAU OF STANDARDS
- *: i ; ' ' : •"' 7 g - « *n ! I
INTEFLABORATORY COMPARISON OF

THE POTENTIAL HEAT METHOD

By

D. Gross

ABSTRACT

Quantitative measurements of the total heat release from eight selected

building materials were made during an interlaboratory study of the Potential Heat Test Method. Statistical analysis of the results indicates that

a higher degree of variability existed among the nine participating laboratories than would be expected of a single laboratory performing standardized oxygen bomb calorimeter determinations of the heat of combustion. It was noted that the majority of laboratories tended to rank the materials

in the same order, or in an order which could be made the same by a ranking

change of a single material.

A discussion is presented of the effects of material sampling, of

the amount of combustion promoter used, and of specific details of the

experimental procedure. Suggestions are made for evaluating the causes

of interlaboratory differences and reducing their magnitude in a follow-up

study.
,

.

... ,.
INTERLABORATORY COMPARISON OF

THE POTENTIAL HEAT METHOD

By

D . Gross

Introduction

In March 1965, an interlaboratory comparison study of the potential

heat test method was initiated by a Task Group of Subcommittee V (Definitions and Nomenclature) of ASTM E-5 (Fire Tests of Materials and Constructions). One goal of the Task Group was to evaluate the suitability of

the test method for measuring and classifying materials according to their

degree of combustibility.

The test method had been developed several years earlier [l] to measure the total heat released under typical fire exposure conditions, but

without regard to the rate at which the heat was released. The method

makes use of standard calorimetric techniques in which the burning of

small quantities of combustible in an otherwise inert material is assured

by use of a combustion promoter which is added prior to test. By measuring

heat of combustion in an oxygen bomb calorimeter both before and after ex- posure to a "standardized fire" (2 hr in air at 750 C), the difference

may be considered as the potential heat of the material.

The Task Group consisted of the following members:

Mr. I. A. Benjamin, Granco Steel Products Co., Chairman

Mr. P. E. Baseler, Building Officials Conference of America

Mr. D. Gross, National Bureau of Standards

Dr. J. R. Jutras , National Research Council of Canada

Mr. J. A. Wilson, Factory Mutual Engineering Division.

The NBS Fire Research Section undertook the task of mailing specimens

to the participants in May 1965, and the test results were returned in the

period July to December 1965.

Participants

A total of nine laboratories, including the National Bureau of

Standards, participated in the study. These were:

Ohio State University

Underwriters Laboratories, Inc.

U. S. Forest Products Laboratory

Fire Research Section, National Research Council of Canada

Johns-Manville Fiber Glass Division

Owens-Corning Fiberglas Corporation

Factory Mutual Engineering Division

U. S. Bureau of Mines

- 1 -
Test Procedure

Details of the test procedure were described in a published article

[1]

and in a tentative test method standard (see Appendix A) distributed

to the participants. Prior to initiating the study, the ASTM Manual on interlaboratory studies [2] was consulted and advice was solicited from

the NBS Statistical Engineering Section.

To obtain a broad base of experience with a minimum of participation

time, it was suggested that the pilot study would provide satisfactory

estimates of precision without the need for duplicate determinations.

Except for preliminary experimentation for orientation in techniques of

bomb calorimetry, therefore, a single determination on each of eight

materials was requested, with additional testing (to provide duplicate

data) to be undertaken only if necessary.

The following were also distributed to the participating laboratories:

(1) a reference material (for practice and test method familiarization;

(2) a set of supplementary notes and instructions (see Appendix B);

(3) a summary data sheet;

(4) a questionnaire

(5) packages containing the samples, a specimen container and cap,

and a wire specimen holder.

Materials

A list of the eight materials selected is given in Table 1. These

were considered typical composite materials used in buildings at the

present time. The test materials were designated by code letter only,

and no producer identification was intended or implied. Asbestos millboard, designated M and conforming to Federal Specification HH-M-351 b, was the reference material. All samples were cut from larger sheets or blocks in a pre-arranged manner and a record kept of the sampling location.

Results

Table 2 is a summary of the replies to the questionnaire. There were

three requests for code letter identification of participating laboratories, and, by prior agreement, only one was necessary to carry. The code

letter S was given to this laboratory (NBS). As to whether the individual

labfe values and the ranking order of the materials was realistic, four

indicated yes and five were undecided. Comments on the basic theory and

application, difficulties encountered, and suggested revisions, are also

summarized. With regard to theory and application, several laboratories

commented that the method does not evaluate the rate at which heat is

released. As to experimental difficulties, several laboratories noted

instances of incomplete combustion, and there were questions as to preparation of representative samples.

2
Table 3 summarizes individual values of the heat of combustion of

the specimen (direct), the heat of combustion of the residue (after simulated fire exposure), and the potential heat. For these materials, the

heat of combustion of the residue was very significant in the determination of potential heat. Vacant spaces represent the absence of data.

In several instances, as noted, arithmetic or typographical errors were

found or assumed, and values adjusted.

Table 4 summarizes the percent residue values for all materials and

laboratories, and illustrates, with few exceptions, the good reproducibility of this determination. For materials C, D, and E, the percent

residue values agreed to within +0.5 % for all laboratories.

Table 5 lists, for each laboratory, average (or typical) values of

test parameters which affect the direct measurement of the heat of com- bustion. From this list, and the individual values on which they were

based, certain points may be noted:

1. It appeared that the incremental temperature readout varied

from 0.005 to 0.02 F. For an average calorimeter water equivalent of nearly 2500 Btu/deg F (g/lb)* a change of 0.02 F

corresponds to a change of 50 Btu/lb.

2. The fuse wire correction varied from 20 to 182 Btu-g/lb.* (The

latter value greatly exceeds the total calorific value of the

prescribed length, usually 10 cm, of No. 34 B & S gage Chromel

C or iron fuse wire).

3. The acid titration correction for material C varied from 0 to

94 Btu-g/lb. Since material C contained approximately 16% sulfur,

an appreciable correction was to be expected.

4. The temperature of the calorimeter water ranged from 3.1 F below

to nearly 12 F above the jacket at the start of the test.

5. The individual percentage values of combustion promoter used

varied from 0 to 91. However, only laboratory Z used a consistently different (higher) proportion of combustion promoter than

called for. This was done to prevent incomplete combustion of

specimens containing the prescribed amount (50%) of promoter.

One laboratory (V) separated composite materials C, E, and H into

their two layered components and tested each component separately. The

contributions of heat were then combined in proportion to their original

we igh t fr ac t ions

.

*For explanation of units, see footnote, Table 5

- 3 -
Statistical Analysis

Because the results were variable and the materials so different,

it was decided to present the results as deviations from the median value

for each material rather than in terms of a conventional analysis of

variance. The median value is the value such that half the results are smaller than, and half the results are larger than the median. The median was used rather than the arithmetic mean because it is less influenced by outlying values.

Table 6 summarizes the results of the direct and residue heat of

combustion measurements, showing the median value for each material and

the deviation of each laboratory from this median value. The first line

below the tabulated values gives the sum of such signed deviations for

each laboratory. This sum (or the equivalent average) is some measure

of the apparent bias of a particular laboratory - i.e., its sign and

its relative magnitude show the level of a laboratory with respect to

the rest of the group. The next line below the tabulation gives the sum of the absolute deviations for each laboratory, and is a comparative

measure of the spread of a laboratory's results.

The deviations listed in Table 6 are plotted in Figure 1 for each

material and laboratory. The materials have been arranged along the

horizontal axis in increasing order of the median value of the material.

It may be noted that the dispersion does not seem to depend upon the

magnitude of the median heat of combustion value.

The magnitudes of the interlaboratory deviations suggests that

differences between duplicate determinations by an individual laboratory

may be higher than 100 Btu/lb, the value derived from the initial test

method evaluation [1], A conventional heat of combustion measurement is

expected to duplicate within 0.3 percent within the same laboratory, and

within 0.5 percent at different laboratories [3]. For judging the ac- ceptability of test results obtained with a bomb calorimeter (95 percent

probability), the following limits are specified [4]:

"Repeatability - Duplicate results by the same operator shall be

considered suspect if they differ by more than 55 Btu/lb.

"Reproducibility - Results submitted by two or more laboratories

should be considered suspect if they differ by more than 175 Btu/lb."

Since this test method requires the mixing of a combustion promoter

with the specimen, as well as reporting the difference of direct and

residue bomb calorimeter measurements and accounting for weight changes

during the muffle furnace exposure, errors of somewhat greater magnitude

are to be expected. It appears highly desirable that duplicate determinations be included in the next phase of interlaboratory comparisons.

- 4 -
A simplified overall summary of the inter laboratory comparison may

be obtained by the comparison of material rankings listed in Table 7.

Three of the nine laboratories ranked the eight materials in exactly the same order, corresponding to the overall consensus. Considering materials

E and F to be "identical" for the purposes of the consensus (overall average values 1123 and 1093 Btu/lb) , a ranking change of a single material

would bring 3 more laboratories into agreement with the consensus.

Discussion

1. Sampling

Several laboratories expressed concern about the preparation of

representative samples from the heterogeneous engineering materials used

and the fact that the direct bomb calorimeter specimens weighed only one

gram. A measure of the extent of this problem might be gaged by (a)

variability in the direct bomb heat of combustion, and (b) variability

in the percent residue values for the muffle furnace specimens, since this

is a measure of the combustible and volatile content. For materials B (mineralized wood) and G (cinder aggregate concrete), there was considerable

variability in the direct bomb heats of combustion. For material B, five

of the laboratories cluster very close to the median value, while four

laboratories are extreme "outliers." This characteristic variability for

material B may possibly be associated with a differential separation of

the components during specimen preparation by some laboratories and suggests

that details of the specimen preparation need to be defined more closely.

For material B, 8 of 9 laboratories measured the residue within fairly

close limits, 44.2 to 46.4 percent. Only for material G was there an appreciable variation in the percent residue values, ranging from 58.7 to

82.4. For all other materials there was very good agreement in the weight

loss during the muffle furnace exposure (See Table 4).

It is also interesting and informative to note that the separation of

composite materials C, E, and H into their two (or three) layered components,

and their separate testing by laboratory V, yielded consistent and meaningful heat of combustion values, when their heat contributions were combined

in proportion to their original weight fractions.

With one exception, there did not appear to be any systematic cor- relation between the high (or low) heat of combustion values measured by

some laboratories and the location of the sample as cut from its original

large sheet or block. For material G (cinder aggregate concrete) , however

,

there was a significant difference between the direct heat of combustion

values as obtained from the two 6-5/8- by 16-in. blocks from which the

samples were cut. Figure 2 illustrates how the individual samples were distributed among the nine laboratories, and the resultant direct heat of

combustion values measured. The average for laboratories Q, R, S, T, and

U from one block was 1735 Btu/lb, compared to 2578 Btu per lb for laboratories V, X, Y and Z from the other block.

5
For most engineering materials and products, the use of a prescribed

sampling procedure is probably not necessary provided the 1 gram (or 1/2 g)

direct bomb specimen is obtained from the intimately-mixed powder of a pulverized piece of minimum size 1/2 in. by 3 in. by nominal thickness.

For typical building materials with densities ranging up to 120 lb per cu

ft, this piece would weigh between 5 and 20 grams. A change in the

sampling procedure is therefore suggested (see Appendix C) to require this

minimum sample size to be pulverized for the direct heat of combustion

measurement. For grossly heterogeneous materials, e.g. cinder aggregate

concrete, bulk sampling procedures are obviously necessary if more con- sistent interlaboratory results are to be achieved.

2. Combustion Promoter

Several laboratories noted instances of incomplete combustion.

Laboratory Z used a higher proportion of combustion promoter than that

prescribed (50 percent) in order to avoid incomplete combustion. The use

of an equal weight of benzoic acid promoter was based on a prior investigation in which less than 30 percent benzoic acid mixed with aluminum

oxide was found to result in incomplete combustion [1],

In Figure 3 are plotted the specimen and residue heats of combustion

for the one material (E, protected steel) for which benzoic acid promoter

in a very wide range had been used. This data suggests the possibility

that 50 percent benzoic acid may not be quite sufficient to ensure com- plete combustion of some materials.

3. Experimental Procedures

It is evident from the comments provided, as well as from the sum- mary of typical test parameters shown in Table 5, that certain procedures

and measurements must be closely controlled, while others are of much less

importance.

In addition to representative sampling and the use of a minimum

of 507o of combustion promoter, the following items require particular

care and accuracy:

(a) mechanical or manual pulverization by grinding, filing, etc.

and intimate mixing, so as to avoid segregation or separation

of components (see Appendix C);

(b) accurate weighing and careful accounting for losses during the

preparation of pellets;

(c) temperature measurement to 0.005 F, or less;

(d) proper fuse wire and acid titration corrections.

6
The (plain) bomb calorimeter test procedure recommends that the

temperature of the water be initially 3 to 3.5 deg F below that of the

calorimeter jacket. Assuming the jacket to be at room temperature, the

initial water temperature ranged from 3.1 deg F below to nearly 12 deg F

above that of the jacket, but no systematic effect on the results could

be noted.

Only one laboratory (T) made allowance for the quantity of sulfur

(approx. 16 percent) in material C. However, since allowances of similar

magnitude occur for both the direct and residue, tests, the difference in

the potential heat was not significant.

Future Work

A second phase of the potential heat interlaboratory study, which

would incorporate the specified changes in the test procedure, is desirable. For 5 selected materials, and a minimum of 4 laboratories, a test

plan is listed in Table 8 which would permit evaluation of the percent

combustion promoter as well as repeatability within each laboratory and

reproducibility between laboratories. Each participant would be requested

to perform a total of 12 tests. In all such testing programs, comments

and feedback from the individual participants is very important.

Summary and Conclusions

Valuable experience has been gained from this initial interlaboratory

comparison of the Potential Heat Test Method. Of the 9 participating

laboratories, some were experienced in oxygen bomb calorimetry, while

others were novices. Major and minor variations were made by individual

laboratories in many aspects of the testing procedure. In addition, the

majority of the 8 test materials, selected as typical of composites used

in buildings at the present time, were of generally low potential heat

as a critical test of the method.

A higher degree of variability existed among the participating

laboratories than would be expected of a single laboratory performing

standardized oxygen bomb calorimeter determinations of the heat of combustion. However, the majority of laboratories tended to rank materials in

the same order, or in an order which could be made the same by a ranking

change of a single material.

Based on a study of the interlaboratory differences, and the comments

provided by the participating laboratories, it is suggested that more

specific test instructions and evaluations be provided in future test

programs. These include material sampling, the proportion of combustion

promoter, close control of pulverization, weighing and temperature

measurement, and the requirement for duplicate dterminations . Specific

suggestions were made in the "Discussion" and "Future Work" sections, and

by revisions in the Tentative Test Method (Appendix C).

7
Acknowledgments

This study was made possible through the excellent and prompt

cooperation of the laboratory and research workers in each of the

participating laboratories. The generous help of Mrs. M. G. Natrella

and Dr. W. J. Youden of the NBS Statistical Engineering Section in the

statistical analysis and experimental design aspects is gratefully

acknowledged

.

8
References

[1] Loftus, J. J. } Gross, D. , and Robertson, A. F., Potential Heat - A Method for Measuring the Heat Release of Materials in Building

Fires, ASTM Proc. 61, 1336-48 (1961).

[2] ASTM Manual for Conducting an Interlaboratory Study of a Test

Method, ASTM STP No. 335 (1963).

[3] Standard Methods of Laboratory Sampling and Analysis of Coal

and Coke, ASTM Designation D 271-64, 1966 Book of ASTM Standards,

Part 19.

[4] Standard Method of Test for Heat of Combustion of Liquid Hydrocarbon Fuels by Bomb Calorimeter, ASTM Designation D 240-64,

1966 Book of ASTM Standards, Part 17.

9
Appendix A. Tentative Method of Test For

POTENTIAL HEAT RELEASE OF MATERIALS

IN BUILDING FIRES

Scope

1. This method, of test provides a means of determining the potential release of heat of materials involved in building fires. The method

is applicable to a variety of materials including metals, and especially

materials of low combustible content. Determinations may be made on simple materials, or on composite assemblies of materials from which a representative sample can be taken and pulverized into a homogeneous

mixture.

Definition

2. Potential heat of a material is the difference between the heat

of combustion of a representative sample of the material and the heat of

combustion of any residue remaining after exposure to a simulated standard fire, using combustion calorimetric techniques.

Summary of Method*

3. One of two specimens removed from the material to be tested is

pulverized, pelleted, and burned in a high-pressure oxygen atmosphere.

The process is generally as described in ASTM D 271-58 (Laboratory Sampling and Analysis of Coal and Coke), but with certain modifications or permissible exceptions, to be noted in the test procedure. This determines the gross heat of combustion of the material. The second specimen

is heated in air for 2 hr at a temperature of 1382 F (750 C), conditions

adopted as representing a standard fire exposure. A portion of the

resulting residue of this specimen, if any, corresponding to a predetermined weight of original material, is ground or pulverized, mixed with a combustion promoter, and pelleted for burning as was the first specimen.

After correcting for the heat produced by the combustion promoter, the

difference in heating values of the two specimens is the potential heat,

as defined in par. 2. The test procedure is illustrated schematically

in Fig .1A .

Apparatus and Materials for Test

4. The apparatus and materials required for the test are listed

below.

(a) Oxygen bomb calorimeter, including firing circuit and

fuse wire.

(b) Muffle furnace (having small opening or port for passage

of air supply tube). * See Reference [1],

10
(c) Hand mill (or ball mill),

(d) Pelleting press.

(e) Microbalance, weighing to 0.1 mg.

(f) Oxygen cylinder and accessory equipment.

(g) Compressed air supply.

(h) Standard alkali solution.

(i) Combustion promoter, National Bureau of Standards standard

material, sample 39 h, benzoic acid (calorimetric standard).

(j) Parts associated with muffle furnace firing (illustrated

in Fig. 2),

(1) Specimen container for use in the muffle furnace; a suitable part may consist of a fused silica or ceramic tube,

1-1/4 in. inside diameter by 4 in. long, closed at one end.

(2) Cap to fit open end of specimen container; cap to

be provided with an opening to pass an air supply tube with loose

fit.

(3) Air Supply tube; may be of porcelain, fused silica,

or corrosion-resistant metal; inside diameter 3/16 in. minimum;

length to extend beyond port of muffle furnace.

(4) Wire specimen holder; of corrosion-resistant metal;

formed to support the specimen away from the walls of the specimen container, for circulation of air about specimen.

(5) Support of fire brick or similar material shaped to

hold the specimen container and its cap in alignment with the

muffle furnace port, so that the air supply tube may be positioned

in the specimen container.

Test Specimens

5. Two air-dry test specimens representative of the material or assembly involved are required for each determination. A specimen is

considered "air-dry" when it has reached constant weight in an atmosphere maintained at. 73 + 2 F (23 + 1 C) and 50 + 5 percent relative

humidity. If the test subject is an assembly or composite material,

it is essential that the several elements of the subject are contained

in the test specimen in the same proportions that they occur in the subject. The two specimens are subjected to separate test procedures.

11
Procedure for Direct Bomb Test

6. (a)

(b)

Note 1:

Note 2:

(c)

Note 3:

(d)

(e)

(f)

(g)

The specimen shall be pulverized, using a hand mill or other means as may be necessary, into a form suitable to

pass a No. 60 sieve.

A pellet, weighing approximately 1 g., shall be prepared

from a representative sample of the powder, and then

weighed

.

All weight measurements shall be to the nearest 0.1 mg.

Pellets shall be made in accordance with the method for the

particular pelleting press in use and of a size convenient

for the specimen cup. The pellets shall be no harder than

necessary to prevent their disintegration when fired.

The prepared pellet is the test specimen for the procedure

for determination of the heat of combustion in accordance

with ASTM D271-58, par. 51-55 (oxygen bomb test). Also

see ASTM E-144, Recommended Practice for Safe Use of Oxygen Combustion Bombs.

Modifications and exceptions to the requirements of ASTM

D271-58 are listed in the Addendum.

If, after being fired in the oxygen bomb, the pellet is

found to have burned completely, or to have left no significant amount of residue or ash, the heat of combustion on an air-dry basis may be computed, and the following three

steps (e), (f), (g), shall be omitted.

If the pellet does not burn, or a residue remains after the

firing, another 1-g pellet is prepared, this time using an intimate mixture of the powdered sample and a standard

sample of benzoic acid combustion promoter, in equal weight

proportions

.

The pellet prepared with the added benzoic acid is used as the test specimen following the same procedures as for the

original specimen.

A correction for the heat of combustion of the benzoic

acid present in the pellet is applied to the measured heat

released by the specimen. The heat of combustion of the

sample material, on an air-dry basis, is then computed.

12
Procedure for Muffle Furnace and Bomb Test

7. (a) An air-dry specimen representative of the test material or assembly shall be cut in the form of a rectangular prism

1/2-by 3/4-by 3-in. Sheet materials may be folded or laminated to these dimensions.

(b) The muffle furnace is preheated to 1382 + 18 F (750 + 10 C).

The specimen is weighed, and placed on the wire support

4. (j) (4) in the specimen container 4. (j) (1). The con- tainer is closed with its cap 4. (j) (2), and placed in the

firebrick base 4. (j) (5) in the muffle furnace in such

position as to align the muffle furnace port and the opening in the specimen container cap. The external air supply

tube 4. (j) (3) is passed through the port into the container

in proximity to the specimen. Firing is continued for 2 hr

with a regulated air flow of 0.1 ft per min, referred to

60 F and 30.0 in. Hg, supplied to the specimen. If ignition

should occur immediately upon placing the specimen in the

furnace, application of air shall be delayed until the

initial flaming has stopped.

(c) The container with the specimen shall be cooled in a desiccator, after which the weight of the residue is determined.

(d) If the residue from the muffle firing procedure is less than

5 percent of the initial weight of the specimen, the following steps (e) and (f) are omitted, and the heat of combustion

previously determined under the direct bomb test, par. 6 (d),

shall be reported as the potential heat of the material.

(e) If the residue after the muffle firing is in excess of 5 percent of the original specimen weight, the residue shall be

pulverized, mixed with an equal weight of benzoic acid and

treated as specified in the procedure for direct bomb test

to determine the heat of combustion (of the residue).

(f) To determine the heat of combustion of the residue per unit

weight of original specimen, multiply the heat of combustion

determined in par. 7. (e) above by the ratio of residue

weight, 7. (c) to the original specimen weight 7. (b).

Potential Heat

8. The potential heat of a material is determined by subtracting the

heat of combustion of the residue remaining from the muffle fur- nace firing, par. 7. (f), from the heat of combustion of the

material established in the direct bomb test, par. 6 (g). The

potential heat is thus a measure of the heat released by a material in the muffle furnace firing, the conditions of which are considered to simulate a standard fire. For most materials.

13
potential heat may be reported in heat units per unit weight,

or where appropriate to the material and its use, it may be

expressed on the basis of volume or surface area of the material.

For materials such as metals where the combustion process is

relatively slow, and is a function of surface area, potential

heat should appropriately be reported on a surface area basis

only.

ADDENDUM

Modifications and exceptions to the requirements of ASTM D 271-58

are as follows:

(paragraph references apply to the standard as presented in the

1961 Book of ASTM Standards).

par. 52 (3) Fuse wire may be that provided for the bomb in use;

a suitable correction factor for the wire shall be

applied

.

par. 53 (b) Benzoic acid is a suitable substance for standardization procedures (see 4. (i) of this standard).

par. 54 (a) Alternate method of Note 32 for materials of high

ash content not used; in cases of incomplete burning,

a combustion promoter is added (see 6.(e)).

par. 54 (f) An ignition system supplied for the bomb may be

substituted

.

par. 54 (h) Where materials leave a residue, remove the cup con- taining the residue, then proceed to rinse out the bomb

and titrate as described in this paragraph.

par. 55

(Note 40) The method of this test for potential heat release of

materials gives the gross heat of combustion of a material in an air-dry condition; net calorific value

(net heat of combustion) calculations are not normally

a part of this procedure, (see footnote*).

14
Appendix B. Supplementary Notes and Instructions

1. To permit statistical interpretation of variations in test results,

the samples have been cut from the larger sheets in a pre-arranged

manner. It is requested that the following directions be followed:

For the Muffle Furnace Test, cut a test specimen from the

end opposite to the label location. Remove sufficient

material from the newly exposed edge for the Direct Bomb

Test. This may be done using a clean file, rasp or other

device and the filings pulverised, if necessary, using a mortar and pestle, ball mill, etc. Use the edge closest

to the label for trial runs, if desired. The remaining

sample should be retained for possible future comparisons

or for use as reference materials.

2. Please note the following change in test procedure [Par. 7(a)]:

The specimen for the Muffle Furnace Test should be 1/2" wide,

3" long and the thickness as supplied , but not greater than

1 in. Sheet materials should be folded (or laminated) to

these dimensions (1/2" by 1" by 3").

3. Standard grade benzoic acid for use as a combustion promoter and for

standardizing the oxygen bomb calorimeter is available for purchase

from the oxygen bomb manufacturers or from chemical supply companies.

A primary standard benzoic acid powder may be purchased from the

Standard Materials Unit, Attn: Mrs. Pauline Michael, National Bureau

of Standards, Washington, D. C. 20234. This is currently identified

as Calorimetric Standard Sample No. 39i, and is priced at $6.00 for

a 30 gram sample.

4. Caution should be observed when performing a direct bomb calorimeter

test on a specimen which is predominantly metallic (One material in

this series). It is possible that high reaction temperatures will

occur which could involve portions of the capsule and bomb, or that an electrical short in the ignition system may occur through the

conventional steel capsule. For such tests, the use of a silica

combustion capsule is recommended (c.f. A.H. Thomas Co., Cat. No.

3879-C)

.

5. A suitable air supply tube could be one of the following:

(a) Vycor 7mm i.d. standard tubing (Corning No. 743172, or equivalent)

(b) Porcelain 7mm o.d. protection tubing (McDanel No. PT5M, or " )

15
6. Please use the accompanying data sheet, which was designed to

facilitate the recording of data. It is desirable, in addition,

that each participant make a personal, permanent record of all

the data and calculations, properly dated and labeled for future

reference. A spare data sheet is included.

7. If a Fahrenheit thermometer is used, compute heats of combustion

directly in Btu/lb, using a calorimeter water equivalent expressed

in Btu/*F (g/lb), and the heat of combustion of benzoic acid as 11,373 Btu/lb.

If a Centigrade thermometer is used, compute heats of combustion

in cal/g using a water equivalent expressed in cal/®C, and the

heat of combustion of benzoic acid as 6318 cal/g. Multiply by

1.80 to convert heats of combustion to Btu/lb.

8. The appropriate oxygen bomb instruction manual, e.g. Parr Manual

No. 130, Oxygen Bomb Calorimetry and Combustion Methods, should

be studied.

16
Appendix C. Test Method Revisions

Replace existing sections in Tentative Test Method (Appendix A) with

the following:

6. (a) The specimen shall be pulverized into a form suitable to pass a No. 60 sieve. Grinding, filing or milling operations, whether

manual or mechanical, should be effected on the cross-section

which is normal to the grain, fiber or other process- induced

orientation. Particular care should be taken to avoid segregation

or separation of components. The representative specimen shall

not be smaller than 1/2 in. by 3 in. by the thickness as supplied, nor shall the resultant powder weigh less than 10 grams.

Note: While many materials may be suitably reduced using a clean

carbide double bastard file and/or mortar and pestle, it may

sometimes be useful to (dry- ice) freeze materials containing

asphaltic, mas tic or plastic components prior to filing, or to use mechanical blendors , ball or hammer mills, grinders, milling

or lathe cutters, etc. For laminated materials, it may be preferable to separate into component layers and to grind, file or pulverize each component separately. The powdered components

may then be intimately mixed in proportion to their original

weight fractions and the mixture tested, or, alternately, each

component may be tested separately and the contributions of

heat combined in proportion to their original weight fractions.

6. (b) A pellet, weighing approximately 1 g, shall be prepared from an intimate mixture of the powder, and then weighed.

6. (e) If the pellet does not burn, or a residue remains after the

firing, another 1-g pellet shall be prepared using approximately

1/2-g portions of the powdered sample and a standard sample of

benzoic acid combustion promoter. Weigh each portion accurately

to 0.1 mg, mix together thoroughly and pelletize. Record the

weight of the pellet to 0.1 mg. Any loss in weight after mixing

and pelletizing should be subtracted from the sample and the

combustion promoter in proportion to their original weight

fractions, and the corrected weights used in the heat of com- bustion calculations.

Add the following after Note 3, Section 6.(c)

Note 4: For tests on specimens which are predominantly metallic, the use

of a silica combustion capsule is recommended. The water equivalent of the calorimeter using the silica capsule should be measured

and used.

17

Figure 1a. Schematic Diagram of Test Procedure

for Potential Heat Measurements
- , - •

-
TABLE 1. LIST OF MATERIALS

Nominal Measured

Designation Material Thickness Density

in

.

lb per cu

A Asbestos-cement board 1/4 121

B Mineralized wood 7/8 24

C Gypsum board 3/8 49

D Mineral acoustic tile 3/4 24

E Protected steel 1/16 281

F Glass fiber insulation 1 2.2

G Cinder aggregate concrete 1 5/8 120

H Aluminum sandwich panel 1 28

M Asbestos millboard 1/2 55
TABLE 2.

SUMMARY

OF

REPLIES

TO

QUEST

IOMAIRE

d 05

X . o 05 44 0) 1 05

•r4 > O 54

d mh 44 •H 0 • 05 •r4 d pd AJ 60

03 AJ

O

a CD CO ca 0) d

05 05

d CD 54 o 44 54

r-4 •r-4 44 44 X) r-4 CL +1 54 d 54 •H ,—| 05 0 d CD 0 05 CL •r4 O 03 05 i-4 d

05 54 o 54 44 CO \ 05 Pm pd 05 0 d o O X r. 0 X X CD d 0 o o 03 d •H o o u 44 r-4 d 54 ,—| 0) CD 44 « 54 o o d CD o CD o CL CD pd O d CD i o 0 t4 CL •H AJ 05 o > 05 u *t4 d AJ 03 03 CD 54 X d 44 •r4 0 0) AJ *r4 CD *H 05 44 AJ 05 *t4

-d 05 CD 05 03a 05 AJ

d 0 05 05 pd 44

AJ

d AJ -d •r4 05 AJ CD

O 0 d o rg £ 54 d 0 pd o 03 pd

O

O 44 05 04 05 05O *»4 0 CDO

O

X 0 0) pd

O 0 AJ

03

u

O

d 05 AJ

O 44 44 o

05 AJ 44 AJ 54 54 •r4 •HO

d 60

•H 05

d t4 05d 05 44 o 05

O

d

44 44 AJ 05

d AJ CO

O CD

C 44 44 •»4 •i4

i-< 00 a)

r-4 0 P0 O CD

a 54 o 05 44

r

—1 d d r-4 d 05 CD 0 05 0 r, i—i

CO f-l

aa o 54 0 o 0 o 44 CO o CL 5m 44

*-4 0 *i4 d 54 o pd

d *r4 0 CD 44 CL o 44 TO d CL AJ 05 00 r-4 44 CU o CL

X

44 0 o 44 CD 05 CD

d 54 •H

O 05

d o 05

d

•H CD

d *H 05 x: o 05 o o 05

C 05 o d 5m CD

Q CQ

M

Q 0 44 ,d P4 ^ M 00 53

M CL

X

05 1 CD

u

44 44 54 i •r4 o d pd d o o X 54 44 o 05

05 CL

C AJ

X • *H 0) 0 d o 0) X 44 0 0) 05 o 54 bo 54 05 o CD > d •H a) 5m d CL CD pd 54 o o o AJ r-4 05 •H CL 05 44 CD vO u •r4 54 f-4 44 CO CD r—1 05 CL

CL 05O CDO

d 05 0 05 0 •H 05 CL 0 0 05 54 05 05 a) 54

X

M > d 03

O > d

d

d

X CL 05

05 o 54 54 o •r4 44 o o o 05

X

X 02 z 05 * CL •H 00 CD !3 & > 44 05

05 00

d 44 05 o 05 05 44 54 5a 05 44 CD o ,d u r-4 d

05

O CO 0 O 54 AJ CL ,-4

QJ

r-4 r—l 0 05 00 o d AJ /-V CD w CL

00 05 05 o CO

d

d * PS

d 03 CL •i4 d

d cr

CO

p 05 AJ 54 05 1—1 r-4

03 CD i-4 d - X

AJ

X t4

03 CD

d > 0 r-4 • 0 CD •4

rl

X

X

u o AJ 0) 05

X

d

03

p •H CD

X 44 05 •i4

CD 44 AJ 0 r-4 *t4 AJ u t-4 O o 03 CD

X

d Xl 0) 05 05 05d 05 44 44

O 54 0) x 051 d d d d 03 54 05 CL CD AJ

05 03 o o o n 54 05 AJ 0 CL 03 a d> 2 o O -d O O 05 05 o z O CQ d o 03 44

54 Pm 60 1 0 o i d

•H 1 X 05 44 AJ •r4 •H

54 05 05 54 54 o CO 00 1 pi2 O 54 54 05 0) 0) Ps o 05 d 5m o

03 i CO- 05 > rd AJ pd

r-4 44

O o 05 CD CD d o CO AJ « X 05 44 CO r-4 O d 05 44 r-4 •H 05 d > CD 05 •H 03 o 05 o AJ 44 •r4 54 X O

44 54 a) 05 05 -d 44

O o AJ 05 •t4 05 CD 05

03

O *r4 AJ 44

X2 CO c O

d 05

a CD 44 03 54 03

05 AJ 44 CL

O CD o O o 05 PS 54 05 Psd CD CD 44 05 44 ,d o AJ d 0) •i4 X 0) d pd 05 CD CD o AJ O CL . X > X > •r4 0) o r-4

54 AJ

X CD AJ 05r-4 rH *r4 T-t

X 05 •r4 ,d 05 di o CD O 05 05 0) 05 o 54 r-4 r-4 03 AJ X 05 d AJ X 54 54 0 1

44

X 44 rC 44 CD

dd CDd 05 CD 05 pd

X •H 05

X 05

O *t4 - CD 00 05 0 44 54 00 54 54 •H 03 03 i-4 pd 44 •H 44 >> MH C 54 od o o 03 05 05 d O 03 O CD d 44 CO 03 CD 1 »4 O O 54 O X o CL CO X d 05 05 05 CL 05 0 o 05

CD o o -r-l

O 44d 44

X

O 05X CO pd 54

r-4 pd pd

CQ 44 05 AJ AJ CO 05 05O

O CD

d 0) cOd 05 05 pd

i-4 1 O 03

d o 0) 54 AJa 05 0 44 05 54 44 44

d CL CD

d £ . CD

X 05X PS 05

d

O 03O pd AJ •i4 O o o 44 o 44 CD 44 14 O 0) 05 44 3 d cd CO 3 AJ CD Cl 03 AJ U t4 03 0 CD I—1 A4 CD N o 3 54 o 05 05

03 *r4 d 44 AJ *t4 s o -H

d •t4 54

X i-4 •« *H AJ ps

d pd

d AJ

AJ X) 1 4J -d

d 05 AJd 03 54 54 05 o 0) COd 44 AJ pd

d o CD c Cl CD o *t4 CD o 44 05 d 44 03 03 a o 05 CD d o 44 r-4 v4 02

05 CO 05 - o r-4 03 •H

O

d > 44

d

O

dr-4 *t4 d 05 05 *r4 CD CD 44 0 X CD AJ •r4 05 05 CD CD 00 AJ pd pd 44 05 *H o 0 W 0) 05 05 O d 05 05 0 44 X *t4 O CO 0 O 05 -d 44 d 05 O 54 1 54 d 44 54 54 05 o 0) r-4 *|4 05 o 54 r-4 d O 05 AJ d d d O o 01 o 14 ca O 54 t4 CO 05 44 o *H -d 0) pd O O pd 05 05 T~) •H

<ul ai 44

a AJ 05 54 AJ CD

U 44 0) AJ AJ AJ AJ 0 d

r-4 0 *t4 d 44

J^ 1 fi 05 -»4

O rd

O CD 05 *r4 d Cl CD 05 CD

O 0 44 •>4 CD

O ,d

O o 05 Hi H X X d H O N r-4 44 £ CQ CQ g 0 o O 03 O a 44 Pm o 1 t1 ol

1-4 05 05

CD 44 C-* 05 c*-* C'- 05 05 03 >*

Pd •Hi d i o

•H •H

AJ 44 o O

O CO 05 03

d CD z 53 0) 05 05 0) o >-• >-< >* XM1 CD54O 54 CQ

-d

O O' o2 CQ

H >

CO 44 Z o

clou

cl o d n

OO-w iJ C ro nj • •h aj 54 05 C d f*

*H *H AJ

CD £. *H

U "0 00

w

doo

05 4J ^

a> o 0 *h

O 05 AJ 05 44 4-1 O *H »—(

-O to c

a> aj *h ^ - a> T) w E C

05 CD <D *H

5-1 *4 M 44 O CD

cx4 e

*h

p

UO 0) S 4Ji eo

4-1 4-1 O X d 0) o n

*H 0) 05 X

05 £

*H

O 0 CL

-d3 d

U AJ

a; cd U *H u u O CD O >

42O

C -r-4 O J2

*r4 £

AJ

CD 5m

cl - oa- 05 <2 r-4 44

'O 0 a o o o u -h « 00 O U 41 44 O 5m

CD *t4 5m AJ 05 44 o a u 0) 0)

05

u • CD 05 a. a»

05 r—I

14

a

Pm 0

CD AJ 44 AJc H (D dJ CL D 05 0 -O - O *H w O 05 Q- d 05 05 H 5m 5m

05 ^ c a s o u

44 o • •h x: <D d 05 b p *h

73 AJ

05

C

L CD

C o o B 05 «H C 44

<D 0) CD , ^ E L j •H 4 (D I > U P- O 0) 0) *4 CL *4 CL 05 0- I 0)

05 CD CD CD O 05 CD c 05 S

O) 05 & q P *H ^

44

OO

5m

0) 00 AJ

AJ

C <D

CD -H CD

(D

X

X

W 4 H 03

05 44

44 ^ 3 44 X 0 *HO CO

Li 0) o a ^

fip 05

x

00 o

44 Jj 44 O O 44 44 C *H0 00

44

OC

d *h pd

•»

d

CD • a 03 *H r4 0 CD

d -d c 2 05 44 CD B

CD 03 »4 CD J4

O

•H CD

OC <D

J4 44 J4 00

C 0) 05 d 5m o X O CL 44 44

ZD 44 05

B 4J

54 05 O d

CL £1 O 0 U O a o

54 05

05 00 ,-4 44 c 05 CD

05 *H r-4 *i4 0 54 ^ 54 r4 d -H 05 L 03 44 AJ O CD 05 CO r-4 05 d 0

CD 0 X U 0 00 U O d C O O -H O 44 x

•H i—I

44 05 £ v-l

05 CQ

d

M

03 05 03 d c

05 05

O

•H

DQ

03

O 05

cd o x:

PQ 00 44 C/3 0

4J

a

CD CD

05 05 54

“* x:
TABLE

3.

SUMMARY

VALUES

OF

HEAT

OF

COMBUSTION

AND

POTENTIAL

HEAT

(Btu

per

lb)

Potential

Heat=

Direct

Heat

.of C

ombu

stionResidue.

.Heat

of

Combustion x

Percent

Residue

U J3

U -O

Changed

from

671

(Typographical

or

arithmetic

error)

Changed

from

789

(Assumed

error

in

percent

residue,

see

Table

4)

Changed

from

187

(Arithmetic

error).

Potential

heat

value

also

changed.

Changed

from

531

(Arithmetic

error).
TABLE 4. SUMMARY OF VALUES OF PERCENT RESIDUE

Material Q R NBS T U V X Y Z A b Av^

A 77.6 78.5 78.6 77.8 77.2 79.9 (90.1) 79.1 78.1 78.4

B 46.1 46.2 46.4 44.2 (87.5) 45.9 45.9 46.0 45.9 45.8

C 73.1 72.9 73.2 73.0 72.4 73.0 72.8 73.2 72.7 72.9

D 85.5 85.6 85.7 85.

4

a 85.6 85.8 85.5 85.6 85.8 85.6

E 89.9 88.8 89.6 89.7 89.2 89.7 89.3 89.5 89.8 89.5

F 87.0 86.7 87.0 - 86.3 87.1 84.4 85.8 86.1 86.3

G 61.0 82.4 78.7 78.0 58.7 72.0 59.5 75.8 58.7 69.4

H 30.1 (35.7) 29.8 30.1 29.5 30.1 30.2 29.9 29.3 29.9

M 82.4 82.5 82.5 - 82.4 - 82.2 - 82.6 82.4

a. Changed from 99.3 (residue weight taken to be 6.1517g instead of 7 .1517g)

b. Values in parenthesis not included in averages.
TABLE 5. SELECTED AVERAGE VALUES

_Q_. -A

Temp. Readout, °F, assumed .005 .005

Weight Readout, g .0001 .0001

Percent Combustion Promoter 50 47

Fuse Wire Correction, Btu-g/lb* 22 28

Acid Titration Corr. Exc."C" 4 17

Acid Titration Corr., Mat'l "C" 17 94

Temp. Diff., Direct Tests, °F -0.5 1.4

"Water Equivalent "of

Calorimeter

Btu

( _a * °F VI b J

2449

Btu (_i\

°C VlhV

cal

~F

1351

cal

°C

"^F (jiD Equivalent 2449 2432

Laboratory

NBS T U V X Y Z

.005 .005 .02 .005 .005 .01

.0001 .0001 . 0001 .0001 .0001 .0001 .0001

52 50 38 50 50 50 85

24 24 182 20 28 30 - 9 8 3 8 8 10 17

64 44 0 30 50 60 44

1.6 -6.5 1.1 -2.3 2.2 -

2443 2419 2448 2418

4532

1357

2534

2443 2419 2534 2443 2448 2418 2518

*These units result from the convenient arrangement employed with many calorimeters

which permits calculation of the heat of combustion in Btu per lb using samples

weighed in grams.
o n it CM 00 CM fi- CM it CM NO NO o it NO CM it 00

u cn

m it

m li- 1 NOm o 00 cn 1—1 it v£> i—i cn CM 00 CM

4) CM i i CM en ON

m

r

—1

CM o cn r—1 o i—i i—l

m 00

a CM CM 1—1 ‘ i—i r—1 3pm on 00 O i—i

in it cn it

O

m cn On

m cn NOO i—i i—1 s_x it ON it i r—i o ON i—1 o r—i cn n- m CM it NO ri ON

ON o i NO cn

n 1—1r-l o CN CM

m I—l cn cn $ 1 i 1 CM 1 i 1 i—i W

Cdw CM it 00 ON cn CM NO 00 o CM

m i—i r-l i—i

VsO NO ri ON 00 NO

H

m 00 00 00

m NO <t o 00 ri <t

m o CO NO in CM ON

m <! X CM 00 it i m r-l NO it i i—i i cn <t It 00 CM cn 2 1 1 1 CM • i 1 1 i CM CM

Ed 1 o

<3 cn it in l—l1cnn 00 r—1

r-l ON ONm Ci

m cn cn it ON in

w X) o ii CM o cn ON

m o i—l 00 i—i

ON r—i <t CM in o m > i-t !—1 o i r-l CM cn i

i 1—1 i 1 i—i cn i it 00

cd i 1 r-l i i 1 O

Pmw P it 00 CM cn cn NO o 00 CM it cn NO it cn o i—i

cn CM o

EEO i—i cn cn cn CO 1—1

CM <t CO 00 r-i cn ON NO 00 cn o CM CM

J

p t3 cn

m ON cn ON i cn r-l i—i

CM in it O' it

m i ON cn

<c to i 1—1 | CM it r-l i r—1 i i cn

n > p 1 1 1 8 i o

13 X) o to 00 cn o ON CM 00 CM cn it o in cn CM CM

m ON

H

J o ON -t cn

n in

m CM

m t—i i—i i CMm

m NO

H

H CM ON CM o r—1 i m o <t r-l i—i r-i cn i m i—i

CM cn

CO I | i i—i

CM i i i—i

E3 i co2OO it it i—i

ON ON in CM CM n. 00 CM CM

m ON ON cn

CO CM On ON CM it 00 r-i

n

m o t—1

cn ri CM CM

n

Pm PE o CM CM i—1 o 00 NO NO i 1—1 i o i—i o 1 cn cn o <3 r-l 1—1 1 i i §w

Ed

m it cn

m cn

n CM

m 1—1 in CM On <t cn 00 i—i

i—i i—i

00 it NO CM CM i—1 n ri NO i—l i—i

ON 00

nd z fd i O i 1—1

<r NO cn CM o o r-l T—1 n cn

n ri 1 i r—1

i—i i—i

wow2 it

m 1—1 cn CM ONm CM cn r-l cn in 00 ri o in <t On ON i—i CO r-- 1 NO O |—1 it <t i—l cn CM cn O CM cn i—I 00 CM 2 O' o 1 00 CM cn m O i—l r-i CM it rH NO i 00 o it 9 r—1 1 1 1 i i cn cn 1 i 1—1 CM

MH

Pm 1 1 3OM =4 m CM NO cn ri CM cn 00

m it i—i o rH NO ON CM

H to 0) r-i NO cn <t it r-l o ON

B

B ON o 00 it CO cn ON o B

B

<3 1-1 3 i cn i—i

ON CM cn r—1NO 3 3 i 1—1 m 1—1 CO i—i 1—1

m 3 3 M T3 t-H CM cn i—i

CN ON CO CO i CsJ i—i CO co

!> 4) cd r-l W 2 > <U 41 Q P P 3 3 *—i

i—l i—i • tO O O

NO •rl CO co P X> jq w 4) <3 PE a Q w Pm O Ed <2 <3 PQ o Q W Em O Ed <3 4 P c e C X-N o 41 o

4)

p •r-l 3 •rl

B o p P TE

p P

•ri a; to <p to •rl Ct) ip CO u p 4) o 3 CO 4) o 3

41 -rl Ed •3 41 td rO

CX

Q CO I-' § ai g o a
TABLE 7 . COMPARISON BY MATERIAL RANKINGS

Potential Heat

Ranking Order

(Lowest = 1)

(Highest = 8)

Laboratory QRSTUVXYZ

1

2

3

4

5

6

78

AAAACAAAA ECCCACCCF FFDDEDDDC CDE DEEFD def g gffbe BGGEFGGEB GBBBBBBGG

H H H H (H) H H H H

Consensus

E

<

oq

*o

wa
TABLE 8, PROPOSED TEST PLAN FOR SECOND PHASE

MATERIAL

A B C

j B

i

|

E

50% Combustion Promoter X

X

XXX X

X

75% Combustion Promoter X

i X
POTENTIAL

HEAT

SUMMARY

DATA

SHEET

44d

CD r—

<

ft>

P3

5-( <D 44

ft !3

d

CDB

•1-4 CDo&

co!

oo|

M

<n!

re3u

to

mi

u. <r|

|

f.

i

|

i

oo|

Cvj|

<o 60 60 60 O

60

<-< 3

ct 44

cd «

60 60 60 60 60

JO

60 '

1

fu

CD

3

44PC PC

*3 Ire C I CO O' (e

T5 T3 re re re *0 re II 14 14 14 u

CO cure °r4 <4-4 cu CM re T3 <4-4 CM CO CU 14 1-4 CM e B B 4J 44 O' O' O' *0

IX B e B B & -U U

4<N d O' - o iT3 C

•H •r4 o

4J 4-1 CM •r4

1 CD o 44

4-N T5 c CD 1 'O

CO

4-1 4-1 14 <44 4J o 14 3 4-1 44 4J U

, , .

.

,c J3 14 4J re •H 14 cu JO CO rd M

. 60 60 O 14 a> 4-1 O o B 0) 44 60 00 O

o 44 1-4 •H <J 14 13 -d o cd 1 O H CO ®M •H U

CO « 0) CD o II 0) T3 CD 44 CD • 44 ai 0) ^ M

<11 eu jc 5 S o re 14 14 c 7

CD rd J-l H CU JC 5 £ O

re H B 60 . W O' 0) 14 o <4-4 O CD 60 JZ B 60 • O

c a) iH re 0) CU 4-1 o •H •re o re N •M 00 rd Qj *M re 0) P.V

u ft -9 4-1 QJ B . f< O o 44 C d i-4 a> •H e •u cu •M p 4 £ P o a. Ol a. 4-J B re O' 4-1 14 C/1 !> 0) o

*> o CU CJ CU

<u O S re B 4J B CO o 0) 14 r\ re 3

L> PC B re E 4-4 e

CU cu PC o c re CD 0) 14 14 44 44 o Pu C c o c re 0) •M o a) o CO r-4 4J CU i-4 •r4 re -d CD (U OJ CD O CD CD CO r-4 •M o H 44 ll B

4 H re 5 44 CD a> B g 3 3 >H B •r4 re •M o *H o r—

1

•r4 r—

4

• -d CO r-4 •M -O re •M o r-4 *r4 M

-U JC 0) • o N re 4-1 re -d CD ret CO <44 u o *M •M » CD M ft 44 CT3 U g 14 60 Cl) a 4J •r4 c 4J B CO •H 44 o <44 01 CD CO CA 60 CD d 44 i4 C

c: O °H > CU <D O c •r4 o o 3 O CD 14 3 Cu CU CD 0) > CU CD o c •M

CU PC Q < CO PC H M Pu H o Pu < IS O 1*44 CO CO (X C ca PC H M PM

u ; s-j C ; CO O' IB

Total

heat,

Q

r

=W(t

f

r

~

tir)

Comb,

promoter

heat

Qp

r

Fuse

wire

correction

Qfr

Acid

titration

correction

Q

ar

Net

heat,

Q

nr

=Qr

-Qpr"Qfr"Qar

DEI//

AT/OR

3TU

Pee

L8

DBL//AJ/0/V

S>T U

PEP

LS ® ©

9

& £ R

(23 U) (32*1/ (%9Q)

/200

RESIDUE

O

e f d

(/o4) 03&) (m)

e o

• (*

In a - 8

> m

£>

e

i ©|-/980l | G E H

Ott) (2350 O'50Z)

F/G /. DEI//ATfCN PROM MED/AN HEAR OF COMBUST/ON

l/ALUE POP EACH MATERSA L

LAB Q.RSFO/XYZ

symbol
Q

i 1728

1 R

j

i 2130

i

1

_ _ J

NBS

] 2103

j

T

1

i

1

1531

t

j

| 1183

!

i

i U

Average0 1735

ET ^ Sg ’-j

)

V

— —

1866

X

! 2669

1

i

1 Y

i

j

270?

i

i Z

1

1

3070

f * 3"

V

V

Average 2578

Figure 2. Distribution of Material G Samples

(Cinder Aggregate Concrete)

Letters designate laboratories

Numbers designate direct heat of combustion, Btu per lb
HEAT

OF

COMBUSTION

BTU

FBR

LB

HO. 3 SPECIMEN MP RESIDUE HEATS OF COMBUST!OH FOR MATERIAL E