1、Designation: D2584 11D2584 18Standard Test Method forIgnition Loss of Cured Reinforced Resins1This standard is issued under the fixed designation D2584; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A n
2、umber in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 This test method covers the determination of the i
3、gnition loss of cured reinforced resins. This ignition loss canshall beconsidered to be the resin content within the limitations of 4.2.1.2 The values stated in SI units are to be regarded as the standard.1.3 This standard is used to measure and describe the response of composite material to heat un
4、der controlled conditions, butdoes not by itself incorporate all of the factors required for fire hazard or fire assessments of the composite materials under actualfire conditions.1.4 Fire testing is inherently hazardous. Adequate safeguards for personnel and property shall be employed in conducting
5、 thesetests.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof whoever uses the user of this standard to consult and establish appropriate safety safety, health, and healthenvironmentalpractices and determine the appl
6、icability of regulatory limitations prior to use.NOTE 1There is no known ISO equivalent to this standard.1.6 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of Internati
7、onal Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D618 Practice for Conditioning Plastics for TestingE691 Practice for Conducting an Interlaboratory Study to Determine the Precision
8、of a Test MethodE2935 Practice for Conducting Equivalence Testing in Laboratory Applications3. Summary of Test Method3.1 The specimen contained in a crucible is ignited and allowed to burn until only ash and carbon remain. The carbonaceousresidue is reduced to an ash by heating in a muffle furnace a
9、t 565C (1050F), cooled in a desiccator, and weighed.4. Significance and Use4.1 This test method can be is used to obtain the ignition loss of a cured reinforced resin sample. This test method can also beused to examine the fiber architecture of pultruded structural shapes.NOTE 2The basic concept of
10、burning off of the organic matrix of a reinforced polymer composite has also been shown to be a useful method forenabling a visual examination of the fiber architecture or laminate structure of some reinforcements.4.2 If only glass fabric or filament is used as the reinforcement of an organic resin
11、that is completely decomposed to volatilematerials under the conditions of this test and the small amount of volatiles (water, residual solvent) that are potentially presentare ignored, the ignition loss canshall be considered to be the resin content of the sample.1 This test method is under the jur
12、isdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.18 on Reinforced ThermosettingPlastics.Current edition approved Oct. 15, 2011Sept. 15, 2018. Published November 2011October 2018. Originally approved in 1967. Last previous edition approved in 20082011as
13、 D2584 - 08.D2584 - 11. DOI: 10.1520/D2584-11.10.1520/D2584-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM websit
14、e.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior e
15、ditions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2
16、959. United States14.2.1 This test method does not provide a measure of resin content for samples containing reinforcing materials that lose weightunder the conditions of the test or containing resins or fillers that do not decompose to volatile materials released by ignition.5. Apparatus5.1 Crucibl
17、e, platinum or porcelain, approximately 30-mL capacity.5.2 Electric Muffle Furnace, capable of maintaining a temperature of 565 6 28C (1050 6 50F).6. Test Specimen6.1 A minimum of three specimens shall be tested for each sample.NOTE 3It is often convenient to use samples obtained from specimens that
18、 have been tested for mechanical properties such as flexural or tensilestrength. Specimens obtained from these samples must be dry and the fractured areas removed, leaving square, unfrayed faces, before being weighed andignited.6.2 The specimen shall weigh approximately 5 g with a maximum size of 2.
19、5 by 2.5 cm by thickness (1 by 1 in. by thickness).NOTE 4Materials 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 requirea larger specimen area than that listed in 6.2. If larger specimens are utilized, it will be necessar
20、y to cut into approximately 2.5 by 2.5-cm (1 by 1-in.)pieces and place in a crucible of sufficient size to contain the specimen.7. Conditioning7.1 ConditioningCondition the test specimens at 236 2C (73.4 6 3.6F) and 50 6 10 % relative humidity for not less than40 h prior to test in accordance with P
21、rocedure A of Practice D618 for those tests where conditioning is required. In cases ofdisagreement, the tolerances shall be 61C (61.8F) and 65 % relative humidity. The conditioning is not required if the test isonly performed to examine the fiber architecture.7.2 Test ConditionsConduct tests in the
22、 standard laboratory atmosphere of 23 6 2C (73.4 6 3.6F) and 50 6 10 % relativehumidity, unless otherwise specified in the test methods or in the specification. In cases of disagreement, the tolerances shall be61C (61.8F) and 610 % relative humidity.8. Procedure8.1 Heat a crucible at 500 to 600C for
23、 10 min or more. Cool to room temperature in a desiccator and weigh to the nearest 1.0mg. The desiccator is not required if the test is performed only to examine the fiber architecture.8.2 Place the specimen in the crucible and weigh to the nearest 1.0 mg. Heat the crucible and specimen in a bunsen
24、flame untilthe contents ignite. Maintain such a temperature that the specimen burns at a uniform and moderate rate until only ash and carbonremain when the burning ceases.NOTE 5It is not absolutely necessary to ignite the specimen in a bunsen flame. Instead the crucible and contents can be placed in
25、 a muffle furnaceat a temperature lower than 565C and ignited. Care must be taken that the ignition does not proceed so rapidly that there will be a mechanical loss ofthe noncombustible residue.8.3 Heat the crucible and residue in the muffle furnace at 565 6 28C (1050 6 50F) until all carbonaceous m
26、aterial hasdisappeared (Note 56). Cool the crucible to room temperature in a desiccator and weight to the nearest 1.0 mg.NOTE 6The time for the carbonaceous residue to disappear is dependent largely on the specimen geometry. It can be up to 6 h but is usually muchless.8.4 Bring the crucible and resi
27、due to constant weight within 1.0 mg.9. Calculations9.1 Calculate the ignition loss of the specimen in weight percent as follows:Ignition loss,weight%5W1 2W2!/W1 #3100 (1)where:W1 = weight of specimen, g, andW2 = weight of residue, g.9.2 Average the 3 specimen values to obtain the sample average.s 5
28、=(X 2 2nX! 2#/n 21! (2)s 5=(X 2 2nX! 2#/n 21! (2)where:s = estimated standard deviation,D2584 182X = value of a single observation,n = number of observations,X = arithmetic mean of the set of observations.9.3 Subtract the lowest specimen ignition loss from the highest specimen ignition loss for the
29、sample and report as the ignitionloss range.10. Report10.1 Report the following information:10.1.1 Complete identification of the material.10.1.2 The ignition loss, weight percent of the sample, and standard deviation. If only glass reinforcement and organic resinwere present, the ignition loss cans
30、hall be considered to be the resin content.10.1.3 Observations in regard to any irregularities noted in the physical properties of the residue, such as melting.11. Precision and Bias11.1 Table 1 is based on a round robin conducted in 2001 in accordance with Practice E691, involving two materials tes
31、ted byseven laboratories (six for pultruded rod). For each material, all the samples were prepared at one source, but the individualspecimens were prepared at the laboratories which tested them. Each test result was the average of three individual determinations.Each laboratory obtained two test res
32、ults for each material. (WarningThe explanation of “r” and “R” in 11.2 and 11.3 are onlyintended to present a meaningful way of considering the approximate precision of this test method. The data in Table 1 should notbe applied to acceptance or rejection of materials, as these data apply only to the
33、 materials tested in the round robin and are unlikelyto be rigorously representative of other lots, formulations, conditions, materials, or laboratories. Users of this test method shouldapply the principles outlined in Practice E691 to generate data specific to their materials and laboratory (or bet
34、ween specificlaboratories). The principles of 11.2 11.2.3 would then be are valid for such data.)11.2 Concept of “r” and “R” in Table 1If Sr and SR have been calculated from a large enough body of data, and for test resultsthat were averages from testing two specimens for each test result, then:11.2
35、.1 Repeatability: Repeatability Limit (r)Two results obtained within one laboratory shall be judged not equivalent if theydiffer by more than the “r” value for that material. “r” is the interval representing the critical The value below which the absolutedifference between two individual test result
36、s for the same material, obtained by the same operator using the same equipment onthe same day in the same laboratory.obtained under repeatability conditions is likely to occur with a probability of approximately0.95 (95 %).11.2.2 Reproducibility: Reproducibility Limit (R)Two test results obtained b
37、y different laboratories shall be judged notequivalent if they differ by more than the “R” value for that material. “R” is the interval representing the critical The value belowwhich the absolute difference between two individual test results for the same material, obtained by different operators us
38、ingdifferent equipment in different laboratories.obtained under reproducibility conditions is likely to occur with a probability ofapproximately 0.95 (95 %).11.2.3 Any judgement Conduct equivalence testing on numerical data from two sources in accordance with 11.2.1PracticeE2935 or 11.2.2 would have
39、 an approximate 95% (0.95) probability of being correct.any known method for judging theequivalence of two means, for example a t-test.11.3 There are no recognized standards by which to estimate bias of this method.TABLE 1 Ignition Loss of Cured Reinforced ResinMaterial Values expressed in % lossAve
40、rage SrA SrB RC RDGlass ReinforcedLaminate36.30 2.57 2.57 7.21 7.21Pultruded Rod 21.36 0.289 0.940 0.0808 0.2632A Sr = within laboratory standard deviation for the indicated material. It is obtainedby pooling the within-laboratory standard deviations of the test results for all of theparticipating l
41、aboratories:Sr5f f sS1 d21sS2 d2 .1sSn d2 g/n g 12B SR = between-laboratories reproducibility, expressed as standard deviation:SR5fSr21SL2 g12where SL = standard deviation of laboratory means.C r = within-laboratory critical interval between tow test results = 2.8 Sr.D R = between-laboratories criti
42、cal interval between tow test results = 2.8 SR.D2584 183ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent
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