1、Designation: D2584 11Standard 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 number in
2、 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 Department of Defense.1. Scope1.1 This test method covers the determination of the ignitionloss o
3、f cured reinforced resins. This ignition loss can 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 thestandard.1.3 This standard is used to measure and describe theresponse of composite material to heat under controlledconditi
4、ons, but does not by itself incorporate all of the factorsrequired for fire hazard or fire assessments of the compositematerials under actual fire conditions.1.4 Fire testing is inherently hazardous. Adequate safe-guards for personnel and property shall be employed inconducting these tests.1.5 This
5、standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of whoever uses this standard to consult andestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to use.NOTE 1There i
6、s no known ISO equivalent to this standard.2. Referenced Documents2.1 ASTM Standards:2D618 Practice for Conditioning Plastics for TestingE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Summary of Test Method3.1 The specimen contained in a crucible i
7、s ignited andallowed to burn until only ash and carbon remain. Thecarbonaceous residue is reduced to an ash by heating in amuffle furnace at 565C (1050F), cooled in a desiccator, andweighed.4. Significance and Use4.1 This test method can be used to obtain the ignition lossof a cured reinforced resin
8、 sample. This test method can also beused to examine the fiber architecture of pultruded structuralshapes.4.2 If only glass fabric or filament is used as the reinforce-ment of an organic resin that is completely decomposed tovolatile materials under the conditions of this test and the smallamount of
9、 volatiles (water, residual solvent) that are potentiallypresent are ignored, the ignition loss can be considered to bethe resin content of the sample.4.2.1 This test method does not provide a measure of resincontent for samples containing reinforcing materials that loseweight under the conditions o
10、f the test or containing resins orfillers that do not decompose to volatile materials released byignition.5. Apparatus5.1 Crucible, platinum or porcelain, approximately 30-mLcapacity.5.2 Electric Muffle Furnace, capable of maintaining a tem-perature of 565 6 28C (1050 6 50F).6. Test Specimen6.1 A mi
11、nimum of three specimens shall be tested for eachsample.NOTE 2It is often convenient to use samples obtained from specimensthat have been tested for mechanical properties such as flexural or tensilestrength. Specimens obtained from these samples must be dry and thefractured areas removed, leaving sq
12、uare, unfrayed faces, before beingweighed and ignited.6.2 The specimen shall weigh approximately 5 g with amaximum size of 2.5 by 2.5 cm by thickness (1 by 1 in. bythickness).NOTE 3Materials that have gross differences in the ratio of resin toreinforcement within an area as small as 2.5 by 2.5 cm (1
13、 by 1 in.) mayrequire a larger specimen area than that listed in 6.2. If larger specimensare utilized, it will be necessary 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 thespecimen.1This test method is under the jurisdiction of ASTM
14、 Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.18 on Reinforced Thermoset-ting Plastics.Current edition approved Oct. 15, 2011. Published November 2011. Originallyapproved in 1967. Last previous edition approved in 2008 as D2584 - 08. DOI:10.1520/D2584-11.2For referen
15、ced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West C
16、onshohocken, PA 19428-2959, United States.7. Conditioning7.1 ConditioningCondition the test specimens at 236 2C(73.4 6 3.6F) and 50 6 10 % relative humidity for not lessthan 40 h prior to test in accordance with Procedure A ofPractice D618 for those tests where conditioning is required. Incases of d
17、isagreement, the tolerances shall be 61C (61.8F)and 65 % relative humidity. The conditioning is not required ifthe test is only performed to examine the fiber architecture.7.2 Test ConditionsConduct tests in the standard labora-tory atmosphere of 23 6 2C (73.4 6 3.6F) and 50 6 10 %relative humidity,
18、 unless otherwise specified in the test meth-ods or in the specification. In cases of disagreement, thetolerances shall be 61C (61.8F) and 610 % relative humid-ity.8. Procedure8.1 Heat a crucible at 500 to 600C for 10 min or more.Cool to room temperature in a desiccator and weigh to thenearest 1.0 m
19、g. The desiccator is not required if the test isperformed only to examine the fiber architecture.8.2 Place the specimen in the crucible and weigh to thenearest 1.0 mg. Heat the crucible and specimen in a bunsenflame until the contents ignite. Maintain such a temperaturethat the specimen burns at a u
20、niform and moderate rate untilonly ash and carbon remain when the burning ceases.NOTE 4It is not absolutely necessary to ignite the specimen in abunsen flame. Instead the crucible and contents can be placed in a mufflefurnace at a temperature lower than 565C and ignited. Care must be takenthat the i
21、gnition does not proceed so rapidly that there will be amechanical loss of the noncombustible residue.8.3 Heat the crucible and residue in the muffle furnace at565 6 28C (1050 6 50F) until all carbonaceous material hasdisappeared (Note 5). Cool the crucible to room temperature ina desiccator and wei
22、ght to the nearest 1.0 mg.NOTE 5The time for the carbonaceous residue to disappear is depen-dent largely on the specimen geometry. It can be up to 6 h but is usuallymuch less.8.4 Bring the crucible and residue to constant weight within1.0 mg.9. Calculations9.1 Calculate the ignition loss of the spec
23、imen in weightpercent as follows:Ignition loss, weight % 5 W12 W2!/W1# 3 100 (1)where:W1= weight of specimen, g, andW2= weight of residue, g.9.2 Average the 3 specimen values to obtain the sampleaverage.s 5 =(X22 nX!2#/n 2 1! (2)where:s = estimated standard deviation,X = value of a single observatio
24、n,n = number of observations,X= arithmetic mean of the set of observations.9.3 Subtract the lowest specimen ignition loss from thehighest specimen ignition loss for the sample and report as theignition loss range.10. Report10.1 Report the following information:10.1.1 Complete identification of the m
25、aterial.10.1.2 The ignition loss, weight percent of the sample, andstandard deviation. If only glass reinforcement and organicresin were present, the ignition loss can be considered to be theresin content.10.1.3 Observations in regard to any irregularities noted inthe physical properties of the resi
26、due, such as melting.11. Precision and Bias11.1 Table 1 is based on a round robin conducted in 2001 inaccordance with Practice E691, involving two materials testedby seven laboratories (six for pultruded rod). For each material,all the samples were prepared at one source, but the individualspecimens
27、 were prepared at the laboratories which tested them.Each test result was the average of three individual determi-nations. Each laboratory obtained two test results for eachmaterial. (WarningThe explanation of “r” and “R” in 11.2and 11.3 are only intended to present a meaningful way ofconsidering th
28、e approximate precision of this test method. Thedata in Table 1 should not be applied to acceptance or rejectionof materials, as these data apply only to the materials tested inthe round robin and are unlikely to be rigorously representativeof other lots, formulations, conditions, materials, or labo
29、rato-ries. Users of this test method should apply the principlesoutlined in Practice E691 to generate data specific to theirmaterials and laboratory (or between specific laboratories). Theprinciples of 11.2-11.2.3 would then be valid for such data.)11.2 Concept of “r” and “R” in Table 1If Srand SRha
30、vebeen calculated from a large enough body of data, and for testresults that were averages from testing two specimens for eachtest result, then:11.2.1 Repeatability:Two results obtained within one laboratory shall be judgednot equivalent if they differ by more than the “r” value for thatmaterial. “r
31、” is the interval representing the critical differencebetween two test results for the same material, obtained by thesame operator using the same equipment on the same day in thesame laboratory.TABLE 1 Ignition Loss of Cured Reinforced ResinMaterialValues expressed in % lossAverage SrASrBRCRDGlass R
32、einforced Laminate 36.30 2.57 2.57 7.21 7.21Pultruded Rod 21.36 0.289 0.940 0.0808 0.2632ASr= within laboratory standard deviation for the indicated material. It isobtained by pooling the within-laboratory standard deviations of the test results forall of the participating laboratories:Sr5 S1!21 S2!
33、21 Sn!2/n 12BSR= between-laboratories reproducibility, expressed as standard deviation:SR5 Sr21 SL2#12where SL= standard deviation of laboratory means.Cr = within-laboratory critical interval between tow test results = 2.8 3 Sr.DR = between-laboratories critical interval between tow test results = 2
34、.8 3 SR.D2584 11211.2.2 Reproducibility:Two test results obtained by different laboratories shall bejudged not equivalent if they differ by more than the “R” valuefor that material. “R” is the interval representing the criticaldifference between two test results for the same material,obtained by dif
35、ferent operators using different equipment indifferent laboratories.11.2.3 Any judgement in accordance with 11.2.1 or 11.2.2would have an approximate 95% (0.95) probability of beingcorrect.11.3 There are no recognized standards by which to estimatebias of this method.ASTM International takes no posi
36、tion 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 rights, and the riskof infringement of such rights, are entirely their own responsibili
37、ty.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to AST
38、M International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address
39、shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D2584 113
