Designation: D 2584 – 02

Standard Test Method for

Ignition Loss of Cured Reinforced Resins1
This standard is issued under the fixed designation D 2584; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.

1. Scope* present is ignored, the ignition loss can be considered to be the

1.1 This test method covers the determination of the ignition resin content of the sample.
loss of cured reinforced resins. This ignition loss can be 4.2.1 This test method does not provide a measure of resin
considered to be the resin content within the limitations of 4.2. content for samples containing reinforcing materials that lose
1.2 The values stated in SI units are to be regarded as the weight under the conditions of the test or containing resins that
standard. do not decompose to volatile materials released by ignition.
1.3 This standard does not purport to address all of the 5. Apparatus
safety concerns, if any, associated with its use. It is the
responsibility of whoever uses this standard to consult and 5.1 Crucible, platinum or porcelain, approximately 30-mL
establish appropriate safety and health practices and deter- capacity.
mine the applicability of regulatory limitations prior to use. 5.2 Electric Muffle Furnace, capable of maintaining a tem-
perature of 565 6 28°C (10506 50°F).
2. Referenced Documents
6. Test Specimen
2.1 ASTM Standards: 2
D 618 Practice for Conditioning Plastics for Testing 6.1 A minimum of three specimens shall be tested for each
E 691 Practice for Conducting an Interlaboratory Study to sample.
Determine the Precision of a Test Method NOTE 1—It is often convenient to use samples obtained from specimens
that have been tested for mechanical properties such as flexural or tensile
3. Summary of Test Method strength. Specimens obtained from these samples must be dry and the
3.1 The specimen contained in a crucible is ignited and fractured areas removed, leaving square, unfrayed faces, before being
allowed to burn until only ash and carbon remain. The weighed and ignited.
carbonaceous residue is reduced to an ash by heating in a 6.2 The specimen shall weigh approximately 5 g with a
muffle furnace at 565°C (1050°F), cooled in a desiccator, and maximum size of 2.5 by 2.5 cm by thickness (1 by 1 in. by
weighed. thickness).

4. Significance and Use NOTE 2—Materials that have gross differences in the ratio of resin to
reinforcement within an area as small as 2.5 by 2.5 cm (1 by 1 in.) may
4.1 This test method can be used to obtain the ignition loss require a larger specimen area than that listed in 6.2. If larger specimens
of a cured reinforced resin sample. are utilized, it will be necessary to cut into approximately 2.5 by 2.5-cm
4.2 If only glass fabric or filament is used as the reinforce- (1 by 1-in.) pieces and place in a crucible of sufficient size to contain the
ment of an organic resin that is completely decomposed to specimen.
volatile materials under the conditions of this test and the small 7. Conditioning
amount of volatiles (water, residual solvent) that may be
7.1 Conditioning—Condition the test specimens at 236 2°C
(73.4 6 3.6°F) and 50 6 5 % relative humidity for not less
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics than 40 h prior to test in accordance with Procedure A of
and is the direct responsibility of Subcommittee D20.18 on Reinforced Thermoset- Practice D 618 for those tests where conditioning is required.
ting Plastics.
Current edition approved March 10, 2002. Published May 2002. Originally
In cases of disagreement, the tolerances shall be 61°C
published as D 2584 – 67 T. Last previous edition D 2584 – 94. (61.8°F) and 62 % relative humidity.
2
For referenced ASTM standards, visit the ASTM website, [Link], or
contact ASTM Customer Service at service@[Link]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.

*A Summary of Changes section appears at the end of this standard.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 2584 – 02
7.2 Test Conditions—Conduct tests in the standard labora- 10.1.3 Observations in regard to any irregularities noted in
tory atmosphere of 23 6 2°C (73.4 6 3.6°F) and 50 6 5 % the physical properties of the residue, such as melting.
relative humidity, unless otherwise specified in the test meth-
ods or in the specification. In cases of disagreement, the 11. Precision and Bias
tolerances shall be 61°C (61.8°F) and 62 % relative humid- 11.1 Table 1 is based on a round robin conducted in 2001 in
ity. accordance with Practice E 691, involving two materials tested
by seven laboratories (six for pultruded rod). For each material,
8. Procedure
all the samples were prepared at one source, but the individual
8.1 Heat a crucible at 500 to 600°C for 10 min or more. specimens were prepared at the laboratories which tested them.
Cool to room temperature in a desiccator and weigh to the Each test result was the average of three individual determi-
nearest 1.0 mg. nations. Each laboratory obtained two test results for each
8.2 Place the specimen in the crucible and weigh to the material.
nearest 1.0 mg. Heat the crucible and specimen in a bunsen
flame until the contents ignite. Maintain such a temperature NOTE 5—Caution: The explanation of 9r9 and 9R9 in 11.2 and 11.3 are
only intended to present a meaningful way of considering the approximate
that the specimen burns at a uniform and moderate rate until precision of this test method. The data in Table 1 should not be applied to
only ash and carbon remain when the burning ceases. acceptance or rejection of materials, as these data apply only to the
NOTE 3—It is not absolutely necessary to ignite the specimen in a materials tested in the round robin and are unlikely to be rigorously
bunsen flame. Instead the crucible and contents can be placed in a muffle representative of other lots, formulations, conditions, materials, or labo-
furnace at a temperature lower than 565°C and ignited. Care must be taken ratories. Users of this test method should apply the principles outlined in
that the ignition does not proceed so rapidly that there will be a Practice E 691 to generate data specific to their materials and laboratory
mechanical loss of the noncombustible residue. (or between specific laboratories). The principles of 11.2-11.2.3 would
then be valid for such data.
8.3 Heat the crucible and residue in the muffle furnace at
11.2 Concept of 9r9 and 9R9 in Table 1—If Sr and SR have
565 6 28°C (1050 6 50°F) until all carbonaceous material has
been calculated from a large enough body of data, and for test
disappeared (Note 4). Cool the crucible to room temperature in
results that were averages from testing two specimens for each
a desiccator and weight to the nearest 1.0 mg.
test result, then:
NOTE 4—The time for the carbonaceous residue to disappear is depen- 11.2.1 Repeatability:
dent largely on the specimen geometry. It can be up to 6 h but is usually Two results obtained within one laboratory shall be judged
much less.
not equivalent if they differ by more than the 9r9 value for that
8.4 Bring the crucible and residue to constant weight within material. 9r9 is the interval representing the critical difference
1.0 mg. between two test results for the same material, obtained by the
9. Calculations same operator using the same equipment on the same day in the
same laboratory.
9.1 Calculate the ignition loss of the specimen in weight 11.2.2 Reproducibility:
percent as follows: Two test results obtained by different laboratories shall be
Ignition loss, weight % 5 [~W1 2 W2!/W1 # 3 100 (1) judged not equivalent if they differ by more than the 9R9 value
for that material. 9R9 is the interval representing the critical
where: difference between two test results for the same material,
W1 = weight of specimen, g, and obtained by different operators using different equipment in
W2 = weight of residue, g.
different laboratories.
9.2 Average the 3 specimen values to obtain the sample
11.2.3 Any judgement in accordance with 11.2.1 or 11.2.2
average.
would have an approximate 95% (0.95) probability of being
s 5 =@ (X 2 2 n~X̄! 2 #/~n 2 1! (2) correct.
11.3 There are no recognized standards by which to estimate
where: bias of this method.
s = estimated standard deviation,
X = value of a single observation,
TABLE 1 Ignition Loss of Cured Reinforced Resin
n = number of observations,
X̄ = arithmetic mean of the set of observations. Values expressed in % loss
Material
9.3 Subtract the lowest specimen ignition loss from the Average SrA SrB RC RD
highest specimen ignition loss for the sample and report as the Glass Reinforced Laminate 36.30 2.57 2.57 7.21 7.21
ignition loss range. Pultruded Rod 21.36 0.289 0.940 0.0808 0.2632
A
Sr = within laboratory standard deviation for the indicated material. It is
10. Report obtained by pooling the within-laboratory standard deviations of the test results for
all of the participating laboratories:
10.1 Report the following information: 1
10.1.1 Complete identification of the material. Sr 5 [ [ ~S1 !2 1 ~S2 !2 .... 1 ~Sn !2 ] / n ] 2
B
SR = between-laboratories reproducibility, expressed as standard deviation:
10.1.2 The ignition loss, weight percent of the sample, and 1

standard deviation. If only glass reinforcement and organic SR 5 [Sr2 1 SL2 # 2

where SL = standard deviation of laboratory means.
resin were present, the ignition loss can be considered to be the C
r = within-laboratory critical interval between tow test results = 2.8 3 Sr.
resin content. D
R = between-laboratories critical interval between tow test results = 2.8 3 SR.

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 D 2584 – 02

SUMMARY OF CHANGES

This section identifies the location of selected changes to this test method. For the convenience of the user,
Committee D20 has highlighted those changes that may impact the use of this test method. This section may also
include descriptions of the changes or reasons for the changes, or both.

D 2584 – 02: (1) A new precision and bias statement was prepared following
a round robin in 2001.

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