1、Designation: D 2584 02Standard Test Method forIgnition Loss of Cured Reinforced Resins1This standard is issued under the fixed designation D 2584; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、in parentheses indicates the year of last reapproval. Asuperscript 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*1.1 This test method covers the determination of the ignitionlo
3、ss of 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 does not purport to address all of thesafety concerns, if any, associated with its use. It is
4、 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.2. Referenced Documents2.1 ASTM Standards:2D 618 Practice for Conditioning Plastics for TestingE 691 Practice for C
5、onducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Summary of Test Method3.1 The specimen contained in a crucible is 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), c
6、ooled in a desiccator, andweighed.4. Significance and Use4.1 This test method can be used to obtain the ignition lossof a cured reinforced resin sample.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
7、conditions of this test and the smallamount of volatiles (water, residual solvent) that may bepresent is ignored, the ignition loss can be considered to be theresin content of the sample.4.2.1 This test method does not provide a measure of resincontent for samples containing reinforcing materials th
8、at loseweight under the conditions of the test or containing resins thatdo not decompose to volatile materials released by ignition.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 (10506 50F)
9、.6. Test Specimen6.1 A minimum of three specimens shall be tested for eachsample.NOTE 1It 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
10、areas removed, leaving square, 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 2Materials that have gross differences in the ratio of resin toreinforcement within an area as
11、small as 2.5 by 2.5 cm (1 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.7. Conditioning7.1 Conditi
12、oningCondition the test specimens at 236 2C(73.4 6 3.6F) and 50 6 5 % relative humidity for not lessthan 40 h prior to test in accordance with Procedure A ofPractice D 618 for those tests where conditioning is required.In cases of disagreement, the tolerances shall be 61C(61.8F) and 62 % relative hu
13、midity.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.18 on Reinforced Thermoset-ting Plastics.Current edition approved March 10, 2002. Published May 2002. Originallypublished as D 2584 67 T. Last previous edition D 2
14、584 94.2For referenced 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.1*A Summary of Changes section appears at the end of t
15、his standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.2 Test ConditionsConduct tests in the standard labora-tory atmosphere of 23 6 2C (73.4 6 3.6F) and 50 6 5%relative humidity, unless otherwise specified in the test meth-od
16、s or in the specification. In cases of disagreement, thetolerances shall be 61C (61.8F) and 62 % 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 mg.8.2 Place the specimen in the crucible and wei
17、gh 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 uniform and moderate rate untilonly ash and carbon remain when the burning ceases.NOTE 3It is not absolutely necessary to ignite the specimen in
18、 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 ignition does not proceed so rapidly that there will be amechanical loss of the noncombustible residue.8.3 Heat the crucible and residue in the
19、muffle furnace at565 6 28C (1050 6 50F) until all carbonaceous material hasdisappeared (Note 4). Cool the crucible to room temperature ina desiccator and weight to the nearest 1.0 mg.NOTE 4The time for the carbonaceous residue to disappear is depen-dent largely on the specimen geometry. It can be up
20、 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 specimen 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.
21、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 observation,n = number of observations,X= arithmetic mean of the set of observations.9.3 Subtract the lowest specimen ignition loss from thehighest speci
22、men 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 material.10.1.2 The ignition loss, weight percent of the sample, andstandard deviation. If only glass reinforcement and organicresin were presen
23、t, 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 residue, such as melting.11. Precision and Bias11.1 Table 1 is based on a round robin conducted in 2001 inaccordance with Practice E 691, involving
24、 two materials testedby seven 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 determi-nations. Each laboratory obt
25、ained two test results for eachmaterial.NOTE 5Caution: The explanation of 9r9 and 9R9 in 11.2 and 11.3 areonly intended to present a meaningful way of considering the approximateprecision of this test method. The data in Table 1 should not be applied toacceptance or rejection of materials, as these
26、data apply only to thematerials tested in the round robin and are unlikely to be rigorouslyrepresentative of other lots, formulations, conditions, materials, or labo-ratories. Users of this test method should apply the principles outlined inPractice E 691 to generate data specific to their materials
27、 and laboratory(or between specific laboratories). The principles of 11.2-11.2.3 wouldthen be valid for such data.11.2 Concept of 9r9 and 9R9 in Table 1If Srand SRhavebeen calculated from a large enough body of data, and for testresults that were averages from testing two specimens for eachtest resu
28、lt, then:11.2.1 Repeatability:Two results obtained within one laboratory shall be judgednot equivalent if they differ by more than the 9r9 value for thatmaterial. 9r9 is the interval representing the critical differencebetween two test results for the same material, obtained by thesame operator usin
29、g the same equipment on the same day in thesame laboratory.11.2.2 Reproducibility:Two test results obtained by different laboratories shall bejudged not equivalent if they differ by more than the 9R9 valuefor that material. 9R9 is the interval representing the criticaldifference between two test res
30、ults for the same material,obtained by different 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 th
31、is method.TABLE 1 Ignition Loss of Cured Reinforced ResinMaterialValues expressed in % lossAverage SrASrBRCRDGlass Reinforced 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
32、the within-laboratory standard deviations of the test results forall of the participating laboratories:Sr5 S1!21 S2!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 i
33、nterval between tow test results = 2.8 3 Sr.DR = between-laboratories critical interval between tow test results = 2.8 3 SR.D2584022SUMMARY OF CHANGESThis section identifies the location of selected changes to this test method. For the convenience of the user,Committee D20 has highlighted those chan
34、ges that may impact the use of this test method. This section may alsoinclude descriptions of the changes or reasons for the changes, or both.D 2584 02: (1) A new precision and bias statement was prepared followinga round robin in 2001.ASTM International takes no position respecting the validity of
35、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 responsibility.This standard is subject to r
36、evision 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 ASTM International Headquarters. Yo
37、ur 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 shown below.This standard is cop
38、yrighted 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).D2584023
