Designation: D2584 − 11

Standard Test Method for

Ignition Loss of Cured Reinforced Resins1
This standard is issued under the fixed designation D2584; 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 (´) 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 carbonaceous residue is reduced to an ash by heating in a

1.1 This test method covers the determination of the ignition muffle furnace at 565°C (1050°F), cooled in a desiccator, and
loss of cured reinforced resins. This ignition loss can be weighed.
considered to be the resin content within the limitations of 4.2.
4. Significance and Use
1.2 The values stated in SI units are to be regarded as the
standard. 4.1 This test method can be used to obtain the ignition loss
of a cured reinforced resin sample. This test method can also be
1.3 This standard is used to measure and describe the used to examine the fiber architecture of pultruded structural
response of composite material to heat under controlled shapes.
conditions, but does not by itself incorporate all of the factors
required for fire hazard or fire assessments of the composite 4.2 If only glass fabric or filament is used as the reinforce-
materials under actual fire conditions. ment of an organic resin that is completely decomposed to
volatile materials under the conditions of this test and the small
1.4 Fire testing is inherently hazardous. Adequate safe- amount of volatiles (water, residual solvent) that are potentially
guards for personnel and property shall be employed in present are ignored, the ignition loss can be considered to be
conducting these tests. the resin content of the sample.
1.5 This standard does not purport to address all of the 4.2.1 This test method does not provide a measure of resin
safety concerns, if any, associated with its use. It is the content for samples containing reinforcing materials that lose
responsibility of whoever uses this standard to consult and weight under the conditions of the test or containing resins or
establish appropriate safety and health practices and deter- fillers that do not decompose to volatile materials released by
mine the applicability of regulatory limitations prior to use. ignition.
NOTE 1—There is no known ISO equivalent to this standard.
5. Apparatus
2. Referenced Documents 5.1 Crucible, platinum or porcelain, approximately 30-mL
2.1 ASTM Standards:2 capacity.
D618 Practice for Conditioning Plastics for Testing 5.2 Electric Muffle Furnace, capable of maintaining a tem-
E691 Practice for Conducting an Interlaboratory Study to perature of 565 6 28°C (1050 6 50°F).
Determine the Precision of a Test Method
6. Test Specimen
3. Summary of Test Method
6.1 A minimum of three specimens shall be tested for each
3.1 The specimen contained in a crucible is ignited and sample.
allowed to burn until only ash and carbon remain. The
NOTE 2—It is often convenient to use samples obtained from specimens
that have been tested for mechanical properties such as flexural or tensile
strength. Specimens obtained from these samples must be dry and the
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics fractured areas removed, leaving square, unfrayed faces, before being
and is the direct responsibility of Subcommittee D20.18 on Reinforced Thermoset- weighed and ignited.
ting Plastics.
Current edition approved Oct. 15, 2011. Published November 2011. Originally
6.2 The specimen shall weigh approximately 5 g with a
approved in 1967. Last previous edition approved in 2008 as D2584 - 08. DOI: maximum size of 2.5 by 2.5 cm by thickness (1 by 1 in. by
10.1520/D2584-11. thickness).
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM NOTE 3—Materials that have gross differences in the ratio of resin to
Standards volume information, refer to the standard’s Document Summary page on reinforcement within an area as small as 2.5 by 2.5 cm (1 by 1 in.) may
the ASTM website. require a larger specimen area than that listed in 6.2. If larger specimens

*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
 D2584 − 11
are utilized, it will be necessary to cut into approximately 2.5 by 2.5-cm where:
(1 by 1-in.) pieces and place in a crucible of sufficient size to contain the
specimen.
s = estimated standard deviation,
X = value of a single observation,
n = number of observations,
7. Conditioning
X̄ = arithmetic mean of the set of observations.
7.1 Conditioning—Condition the test specimens at 236 2°C 9.3 Subtract the lowest specimen ignition loss from the
(73.4 6 3.6°F) and 50 6 10 % relative humidity for not less highest specimen ignition loss for the sample and report as the
than 40 h prior to test in accordance with Procedure A of ignition loss range.
Practice D618 for those tests where conditioning is required. In
cases of disagreement, the tolerances shall be 61°C (61.8°F) 10. Report
and 65 % relative humidity. The conditioning is not required if 10.1 Report the following information:
the test is only performed to examine the fiber architecture. 10.1.1 Complete identification of the material.
7.2 Test Conditions—Conduct tests in the standard labora- 10.1.2 The ignition loss, weight percent of the sample, and
tory atmosphere of 23 6 2°C (73.4 6 3.6°F) and 50 6 10 % standard deviation. If only glass reinforcement and organic
relative humidity, unless otherwise specified in the test meth- resin were present, the ignition loss can be considered to be the
ods or in the specification. In cases of disagreement, the resin content.
tolerances shall be 61°C (61.8°F) and 610 % relative humid- 10.1.3 Observations in regard to any irregularities noted in
ity. the physical properties of the residue, such as melting.

8. Procedure 11. Precision and Bias

11.1 Table 1 is based on a round robin conducted in 2001 in
8.1 Heat a crucible at 500 to 600°C for 10 min or more.
accordance with Practice E691, involving two materials tested
Cool to room temperature in a desiccator and weigh to the
by seven laboratories (six for pultruded rod). For each material,
nearest 1.0 mg. The desiccator is not required if the test is
all the samples were prepared at one source, but the individual
performed only to examine the fiber architecture.
specimens were prepared at the laboratories which tested them.
8.2 Place the specimen in the crucible and weigh to the Each test result was the average of three individual determi-
nearest 1.0 mg. Heat the crucible and specimen in a bunsen nations. Each laboratory obtained two test results for each
flame until the contents ignite. Maintain such a temperature material. (Warning—The explanation of “r” and “R” in 11.2
that the specimen burns at a uniform and moderate rate until and 11.3 are only intended to present a meaningful way of
only ash and carbon remain when the burning ceases. considering the approximate precision of this test method. The
data in Table 1 should not be applied to acceptance or rejection
NOTE 4—It is not absolutely necessary to ignite the specimen in a
bunsen flame. Instead the crucible and contents can be placed in a muffle of materials, as these data apply only to the materials tested in
furnace at a temperature lower than 565°C and ignited. Care must be taken the round robin and are unlikely to be rigorously representative
that the ignition does not proceed so rapidly that there will be a of other lots, formulations, conditions, materials, or laborato-
mechanical loss of the noncombustible residue. ries. Users of this test method should apply the principles
8.3 Heat the crucible and residue in the muffle furnace at outlined in Practice E691 to generate data specific to their
565 6 28°C (1050 6 50°F) until all carbonaceous material has materials and laboratory (or between specific laboratories). The
disappeared (Note 5). Cool the crucible to room temperature in principles of 11.2-11.2.3 would then be valid for such data.)
a desiccator and weight to the nearest 1.0 mg. 11.2 Concept of “r” and “R” in Table 1—If Sr and SR have
NOTE 5—The time for the carbonaceous residue to disappear is
been calculated from a large enough body of data, and for test
dependent largely on the specimen geometry. It can be up to 6 h but is results that were averages from testing two specimens for each
usually much less. test result, then:
8.4 Bring the crucible and residue to constant weight within
TABLE 1 Ignition Loss of Cured Reinforced Resin
1.0 mg.
Values expressed in % loss
Material
Average SrA SrB RC RD
9. Calculations Glass Reinforced 36.30 2.57 2.57 7.21 7.21
Laminate
9.1 Calculate the ignition loss of the specimen in weight Pultruded Rod 21.36 0.289 0.940 0.0808 0.2632
percent as follows: A
Sr = within laboratory standard deviation for the indicated material. It is obtained
Ignition loss, weight % 5 @ ~ W 1 2 W 2 ! /W 1 # 3 100 (1) by pooling the within-laboratory standard deviations of the test results for all of the
participating laboratories:
where: 1
S r 5 f f s S 1 d 2 1 s S 2 d 2 ….1 s S n d 2 g /n g 2
W1 = weight of specimen, g, and B
SR = between-laboratories reproducibility, expressed as standard deviation:
W2 = weight of residue, g. 1
S R 5 f S r 2 1S L 2 g 2
9.2 Average the 3 specimen values to obtain the sample
where SL = standard deviation of laboratory means.
average. C
r = within-laboratory critical interval between tow test results = 2.8 × Sr.
D
R = between-laboratories critical interval between tow test results = 2.8 × SR.
s5 =@ ( X 2
2 n ~ X̄ !
2
#/~n 2 1! (2)

2
 D2584 − 11
11.2.1 Repeatability: Two results obtained within one labo- representing the critical difference between two test results for
ratory shall be judged not equivalent if they differ by more than the same material, obtained by different operators using differ-
the “r” value for that material. “r” is the interval representing ent equipment in different laboratories.
the critical difference between two test results for the same 11.2.3 Any judgement in accordance with 11.2.1 or 11.2.2
material, obtained by the same operator using the same would have an approximate 95% (0.95) probability of being
equipment on the same day in the same laboratory. correct.
11.2.2 Reproducibility: Two test results obtained by differ-
ent laboratories shall be judged not equivalent if they differ by 11.3 There are no recognized standards by which to estimate
more than the “R” value for that material. “R” is the interval bias of this method.

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