1、Designation: D3529M 10Standard Test Methods forConstituent Content of Composite Prepreg1This standard is issued under the fixed designation D3529M; 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 () 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 fiberconten
3、t, fiber areal weight, matrix solids content and matrixcontent of composite material prepregs. Optionally, the matrixsolids content can also be determined after a volatiles contenthas been established. Volatiles content, if appropriate andrequired, is determined by means of Test Method D3530/D3530M.
4、1.2 Procedure A of this test method applies to compositeprepreg of primarily thermosetting matrices that can be ex-tracted in organic solvent. The reinforcement and filler must besubstantially insoluble in the selected extraction reagent. Thisprocedure may also be used for the same purposes to extra
5、ctother matrix material types.1.3 Procedure B of this test method uses ignition loss of acomposite prepreg matrix and applies to organic matrix com-posite systems containing reinforcing fibers that do not changemass when exposed to the matrix combustion method.1.4 This test method assumes a two-part
6、 material system(plus volatiles) and does not distinguish between hybridreinforcements or matrices. Use with hybrid composites islimited to determination of total reinforcement or total matrixcontent.1.5 Matrix solids determination for Procedures A or B usesTest Method D3530/D3530M to determine vola
7、tiles content.1.6 Alternate techniques for determining constituent contentinclude Test Methods C613/C613M (resin content by Soxhletextraction) and D3171 (used principally for consolidatedlaminates).1.7 The values stated in SI units are to be regarded asstandard. No other units of measurement are inc
8、luded in thisstandard.1.8 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior
9、to use. Specific precau-tionary information is given in Notes 2-8 .2. Referenced Documents2.1 ASTM Standards:2C613/C613M Test Method for Constituent Content of Com-posite Prepreg by Soxhlet ExtractionD883 Terminology Relating to PlasticsD3171 Test Methods for Constituent Content of CompositeMaterial
10、sD3530/D3530M Test Method for Volatiles Content of Com-posite Material PrepregD3878 Terminology for Composite MaterialsE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE1309 Guide for Identification of Fiber-ReinforcedPolymer-Matrix Composite Materials in Databases2.2 NFPA St
11、andard:NFPA 86 Standard for Ovens and Furnaces33. Terminology3.1 DefinitionsTerminology D3878 defines terms relatingto composite materials. Terminology D883 defines termsrelating to plastics. Practice E177 defines terms relating tostatistics. In the event of a conflict between terms, TerminologyD387
12、8 shall have precedence over the other documents.3.1.1 fiber content, nthe amount of fiber present in acomposite or prepreg expressed either as percent by weight orpercent by volume. This is sometimes stated as a fraction, thatis, fiber volume fraction. See Terminology D3878.3.1.2 matrix content, nt
13、he amount of matrix present in acomposite or prepreg expressed either as percent by weight orpercent by volume. For polymer matrix composites this is resincontent. See Terminology D3878.3.1.3 prepreg, nthe admixture of fibrous reinforcementand polymeric matrix used to fabricate composite materials.
14、Itsform may be sheet, tape, or tow. For thermosetting resins, it has1This test method is under the jurisdiction of ASTM Committee D30 onComposite Materials and is the direct responsibility of Subcommittee D30.03 onConstituent/Precursor Properties.Current edition approved Nov. 1, 2010. Published Dece
15、mber 2010. Originallyapproved in 1976. Last previous edition approved in 2008 as D3529/D3529M 97(2008). DOI: 10.1520/D3529M-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information
16、, refer to the standards Document Summary page onthe ASTM website.3Available from National Fire Protection Association (NFPA), 1 BatterymarchPark, Quincy, MA 02269-9101.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.been partially c
17、ured to a controlled viscosity called “B stage”.See Terminology D3878.3.1.4 reinforcement content, nthe amount of reinforce-ment present in a composite or prepreg expressed either aspercent by weight or percent by volume.3.1.4.1 DiscussionIf fiber is the sole reinforcement, thenfiber content is equa
18、l to reinforcement content. See Terminol-ogy D3878.3.1.5 resin content, nsee matrix content. See TerminologyD3878.3.2 Definitions of Terms Specific to This Standard:3.2.1 dry resin content, na prepreg resin content calcu-lated by subtracting the average mass loss due to volatiles fromthe initial tes
19、t mass.3.2.2 fiber areal weight, nthe mass per unit area of thefiberous reinforcement of a composite material.3.2.3 matrix solids content, nsee dry resin content.3.2.4 wet resin content, na prepreg resin content thatincludes any volatiles present in the uncured resin. This term isused interchangeabl
20、y with matrix content and resin content inthis test method.3.2.5 volatiles content, nthe amount of volatiles present ina prepreg expressed as percent by weight.3.3 Symbols:3.3.1 Aspecimen area, m2.3.3.2 FAWfiber areal weight; the fiber mass, Wf, dividedby the specimen area, A, in g/m2.3.3.3 FCfiber
21、content of specimen, weight percent.3.3.4 Mcmass of container, g.3.3.5 MCmatrix content of specimen, weight percent.3.3.6 Mffinal mass of specimen and container at end oftest, g.3.3.7 MIinitial mass of the specimen, g.3.3.8 MSmatrix solids content of specimen, weight per-cent.3.3.9 Vcaverage volatil
22、es content test result from TestMethod D3530/D3530M, weight percent.4. Summary of Test Methods4.1 Prepreg is sampled and specimens of a specific area areweighed and the matrix removed by appropriate procedure. ForProcedure A, the specimen is subjected to suitable solvent thataffects the matrix (but
23、not the reinforcement) until the matrix isdissolved and removed. The remaining reinforcement is thendried and weighed. For Procedure B, the specimen is placed ina muffle furnace for a specific time and at a specific tempera-ture (at which the reinforcement remains essentially un-changed) until the m
24、atrix can be entirely removed as ashresidue. The remaining reinforcement is weighed. For eitherprocedure the change in mass is expressed, both matrix contentand fiber content, as a percentage of the specimen initial mass.4.2 When matrix solids content is requested, adjacentsamples are tested for vol
25、atiles content according to TestMethod D3530. The average mass loss due to volatiles issubtracted from the average resin content result and the resultexpressed as a percentage of initial specimen mass as matrixsolids content. The matrix solids content is applicable mainlyto thermosetting matrices.5.
26、 Significance and Use5.1 This test method can be used to obtain the fiber content,fiber areal weight, matrix content or matrix solids content.Knowledge of these results is useful in specifying materialsystems and in developing optimum manufacturing processes.Where volatiles content is consistent and
27、 not critical to process,matrix content shall be used.5.2 This test method is limited to reinforcement constituentsthat do not change mass upon exposure to the matrix removalprocedure and limited to matrix constituents that are fullyremoved by the matrix removal procedure. In the event ofexperiencin
28、g either limitation, an agreement should be reachedwith the end-user as to how to proceed.6. Interferences6.1 Procedure A:6.1.1 Extent of Cure in Thermosetting SystemsIn Proce-dure A, the efficiency of matrix dissolution for thermosettingmatrix materials is directly related to the extent of cure of
29、theresin system. A resin that has started to cross link (such asB-staged resins) will be increasingly more difficult to extract asthe cure advances. If ProcedureAis ineffective in removing thematrix, and Procedure B is inappropriate for the fiber, thenanother test method, such as one of the methods
30、ofTest MethodD3171, should be consulted.6.1.2 Reagent SelectionThe proper reagent, in a suitablequantity, must be selected for the constituents under test. Thereagents listed in Section 8 are provided for consideration,particularly with regard to thermosetting materials, but cannotbe assured to perf
31、orm well on all material systems within thescope of this test method.6.1.3 Ability of Solvent to Reach MatrixSolvents are moreefficient if the material is spread as a film, rather than a solidmass. It is recommended that the sample be consolidated aslittle as possible before introduction into the so
32、lvent. A solventthat is satisfactory for a given form may not be adequate withthe same material of a different form.6.1.4 Solvent StrengthSolvent strength, or the ability torapidly dissolve the matrix, may be enhanced by increasing theamount of solvent, increasing agitation, increasing tempera-ture,
33、 or by placing the sample under vacuum. These are offeredas physical alternatives to use of more hazardous solvents, orcombined solvent systems.6.2 Procedure B:6.2.1 Applicability of Ignition Loss ApproachIn Proce-dure B a reinforced resin matrix composite specimen will beexposed to a temperature in
34、 excess of 500C in an airenvironment for up to 6 h. This test method does not providea measure of resin content for samples containing reinforcingmaterials that lose weight under the conditions of the test orcontain resins or fillers that do not decompose to volatilematerials released by ignition.6.
35、2.2 Length of TestThe sample type and configurationwill determine the length of test exposure. The products ofmatrix combustion will disappear more readily in configura-tions having a large surface area of resin matrix exposure to theoxidizing atmosphere.D3529M 1026.2.3 Pre-IgnitionProvision is made
36、 in this standard forpre-ignition of the specimen and crucible using a Bunsenflame. This step may be helpful to flash-off volatiles andinitiation of the burning process, but care should be taken toprevent mechanical loss of sample residue.6.2.4 Residual Resin Combustion ProductsFiber residueshould b
37、e carefully examined for the presence of adherent resincombustion product before determining the final fiber mass(Wf). If significant amounts of resin product remain on fiber(“producing a false indication of fiber content”) surfaces, thetest method should be repeated. Care should be taken duringthis
38、 process to assure that no physical loss in fiber contentoccurs.7. Apparatus7.1 Cutting (Grooved) Template or DieThe specimen areashall be produced with either a cutting templates or a cuttingdie. The cutting template or die shall be designed to producethe nominal specimen area and shall be capable
39、of limiting theerror in area to no more than 62%.NOTE 1Attainment of 2 % area accuracy with a cutting template anda single-edge blade requires that average cut be made within 0.4 mm ofthe nominal line. A cutting die is preferred over a cutting template and istypically capable of providing a cut area
40、 error of less than 0.05 %.7.2 Analytical BalanceThe analytical balance shall becapable of reading to within 61 mg.7.3 Timer, accurate to nearest minute.7.4 Procedure A:7.4.1 Fume Exhaust Hood,7.4.2 Containers (Beakers, Flasks)borosilicate or suitableplastic that is not dissolved by solvent. The con
41、tainer shall beof a suitable volume for the sample and solvent (a minimum of250 mLis suggested). Other sizes of container may be requireddepending on sample size, and amount of solvent needed tocomplete the dissolution process.7.4.3 Fritted Glass Crucibles or Sample HolderThe frit-ted glass crucible
42、 filter shall be of a suitable porosity to allowdissolved matrix to pass while retaining reinforcement.7.4.4 AgitatorMechanical shaker or ultrasonic bath. Mini-mum shaker speed recommended is 100 agitations orrevolutions/minute. Minimum frequency for ultrasonic bathrecommended is 40 kHz.7.4.5 Hot Pl
43、ateThe hot plate shall have adjustable con-trols suitable for heating the solvent to its boiling point and becapable of controlling the temperature to within 615C.7.4.6 Vacuum PumpCapable of delivering vacuum of atleast 50 kPa.7.5 Procedure B:7.5.1 Crucible Porcelain, or equivalent properties, with
44、acapacity sufficient to completely contain the specimen.7.5.2 Electric FurnaceMuffle design capable of maintain-ing 565C +/- 30C for burn-out of the resin matrix.7.5.3 Laboratory DesiccatorDesign for pre- and post-testconditioning of the specimen and crucible.7.5.4 Bunsen Flame A source of a control
45、led heat flamefor pre-ignition of the specimen.7.5.5 Laboratory Safety EquipmentHeatproof gloves andprotective eyewear are specifically recommended. Laboratoryexhaust fan and/or ventilation system should be available foruse.8. Reagents8.1 Purity of ReagentsAs a minimum, a technical-gradereagent is r
46、equired to provide accurate results. A reagent-gradereagent will be used when resolving disputes or performingsubsequent analysis of extract or residue. Unless otherwiseindicated, the reagent shall conform to the specifications of theCommittee on Analytical Reagents of the American ChemicalSociety,
47、where such specifications are available.48.2 Matrix Dissolution SolventsAsuitable solvent shall beselected that is compatible with the material system under testand the apparatus. Read and understand the precautions listedin Section 9 before selecting a matrix dissolution solvent.Matrix dissolution
48、solvents found effective for many thermo-setting matrices include the following:8.2.1 Acetone (2-Propanone), CH3COCH3.8.2.2 1,2 Methyl Pyrrolidinone (NMP), CH3NOC3H6.8.2.3 Methyl Ethyl Ketone (MEK, 2-Butanone),CH3COC2H5.8.2.4 Dimethylformamide (DMF), (CH3)2NCHO.NOTE 2Warning: As of the approval date
49、 of this standard, DMF waslisted by the InternationalAgency for Research on Cancer in Group 2B asa “possible human carcinogen” and is considered a reproductive toxin bythe National Toxicology Program. See a recent DMF material safety datasheet for more information.8.2.5 Dichloromethane (MECL, methylene chloride),CH2Cl2.NOTE 3Warning: As of the approval date of this standard, MECLwas listed by the International Agency for Research on Cancer in Group2A and 2B as a “probable human carcinogen.”8.2.6 Methyl Isobutyl Ketone (MIBK, 4-Methyl
