1、Designation: D3529 16Standard Test Methods forConstituent Content of Composite Prepreg1This standard is issued under the fixed designation D3529; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number i
2、n 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 fibercon
3、tent, 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 D3530.1.2
4、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 extractot
5、her 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 mat
6、erial 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 to determine volatiles conte
7、nt.1.6 Alternate techniques for determining constituent contentinclude Test Methods C613 (resin content by Soxhlet extrac-tion) and D3171 (used principally for consolidated laminates).1.7 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thiss
8、tandard.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 to use. Specif
9、ic precau-tionary information is given in Sections 8 and 9.2. Referenced Documents2.1 ASTM Standards:2C613 Test Method for Constituent Content of CompositePrepreg by Soxhlet ExtractionD883 Terminology Relating to PlasticsD3171 Test Methods for Constituent Content of CompositeMaterialsD3530 Test Meth
10、od for Volatiles Content of CompositeMaterial PrepregD3878 Terminology for Composite MaterialsE177 Practice for Use of the Terms Precision and Bias inASTM Test Methods2.2 NFPA Standard:NFPA 86 Standard for Ovens and Furnaces33. Terminology3.1 DefinitionsTerminology D3878 defines terms relatingto com
11、posite materials. Terminology D883 defines termsrelating to plastics. Practice E177 defines terms relating tostatistics. In the event of a conflict between terms, TerminologyD3878 shall have precedence over the other documents.3.1.1 fiber content, nthe amount of fiber present in acomposite or prepre
12、g 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, nthe amount of matrix present in acomposite or prepreg expressed either as percent by weight orpercent by volume. For polyme
13、r matrix composites this is resincontent. See Terminology D3878.3.1.3 prepreg, nthe admixture of fibrous reinforcementand polymeric matrix used to fabricate composite materials. Itsform may be sheet, tape, or tow. For thermosetting resins, it has1This test method is under the jurisdiction of ASTM Co
14、mmittee D30 onComposite Materials and is the direct responsibility of Subcommittee D30.03 onConstituent/Precursor Properties.Current edition approved Nov. 1, 2016. Published November 2016. Originallyapproved in 1976. Last previous edition approved in 2010 as D3529M 10. DOI:10.1520/D3529-16.2For refe
15、renced 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.3Available from National Fire Protection Association (NFPA), 1 Battery
16、marchPark, Quincy, MA 02269-9101.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1been partially cured to a controlled viscosity called “B stage”.See Terminology D3878.3.1.4 reinforcement content, nthe amount of reinforce-ment present
17、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 equal to reinforcement content. See Terminol-ogy D3878.3.1.5 resin content, nsee matrix content. See TerminologyD3878.3.2 Definitions of Term
18、s 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 test 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
19、, 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 interchangeably with matrix content and resin content inthis test method.3.2.5 volatiles content, nthe amount of volatiles present ina prepreg expresse
20、d 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,ing/m2.3.3.3 FCfiber 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 s
21、pecimen 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 volatiles content test result from TestMethod D3530, weight percent.4. Summary of Test Methods4.1 Prepreg is sampled and specimens of a specific a
22、rea areweighed and the matrix removed by appropriate procedure. ForProcedure A, the specimen is subjected to suitable solvent thataffects the matrix (but not the reinforcement) until the matrix isdissolved and removed. The remaining reinforcement is thendried and weighed. For Procedure B, the specim
23、en 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 matrix can be entirely removed as ashresidue. The remaining reinforcement is weighed. For eitherprocedure the change in mass is expressed, both mat
24、rix contentand fiber content, as a percentage of the specimen initial mass.4.2 When matrix solids content is requested, adjacentsamples are tested for volatiles content according to TestMethod D3530. The average mass loss due to volatiles issubtracted from the average resin content result and the re
25、sultexpressed as a percentage of initial specimen mass as matrixsolids content. The matrix solids content is applicable mainlyto thermosetting matrices.5. Significance and Use5.1 This test method can be used to obtain the fiber content,fiber areal weight, matrix content or matrix solids content.Know
26、ledge of these results is useful in specifying materialsystems and in developing optimum manufacturing processes.Where volatiles content is consistent and not critical to process,matrix content shall be used.5.2 This test method is limited to reinforcement constituentsthat do not change mass upon ex
27、posure to the matrix removalprocedure and limited to matrix constituents that are fullyremoved by the matrix removal procedure. In the event ofexperiencing 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
28、Thermosetting SystemsIn Proce-dure A, the efficiency of matrix dissolution for thermosettingmatrix materials is directly related to the extent of cure of theresin system. A resin that has started to cross link (such asB-staged resins) will be increasingly more difficult to extract asthe cure advance
29、s. If ProcedureAis ineffective in removing thematrix, and Procedure B is inappropriate for the fiber, thenanother test method, such as one of the methods ofTest MethodD3171, should be consulted.6.1.2 Reagent SelectionThe proper reagent, in a suitablequantity, must be selected for the constituents un
30、der test. Thereagents listed in Section 8 are provided for consideration,particularly with regard to thermosetting materials, but cannotbe assured to perform well on all material systems within thescope of this test method.6.1.3 Ability of Solvent to Reach MatrixSolvents are moreefficient if the mat
31、erial is spread as a film, rather than a solidmass. It is recommended that the sample be consolidated aslittle as possible before introduction into the solvent. A solventthat is satisfactory for a given form may not be adequate withthe same material of a different form.6.1.4 Solvent StrengthSolvent
32、strength, or the ability torapidly dissolve the matrix, may be enhanced by increasing theamount of solvent, increasing agitation, increasingtemperature, or by placing the sample under vacuum. These areoffered as physical alternatives to use of more hazardoussolvents, or combined solvent systems.6.2
33、Procedure B:6.2.1 Applicability of Ignition Loss ApproachIn ProcedureB a reinforced resin matrix composite specimen will beexposed to a temperature in excess of 500C in an airenvironment for up to 6 h. This test method does not providea measure of resin content for samples containing reinforcingmate
34、rials that lose weight under the conditions of the test orcontain resins or fillers that do not decompose to volatilematerials released by ignition.D3529 1626.2.2 Length of TestThe sample type and configurationwill determine the length of test exposure. The products ofmatrix combustion will disappea
35、r more readily in configura-tions having a large surface area of resin matrix exposure to theoxidizing atmosphere.6.2.3 Pre-IgnitionProvision is made in this standard forpre-ignition of the specimen and crucible using a Bunsenflame. This step may be helpful to flash-off volatiles andinitiation of th
36、e burning process, but care should be taken toprevent mechanical loss of sample residue.6.2.4 Residual Resin Combustion ProductsFiber residueshould be carefully examined for the presence of adherent resincombustion product before determining the final fiber mass(Wf). If significant amounts of resin
37、product remain on fiber(“producing a false indication of fiber content”) surfaces, thetest method should be repeated. Care should be taken duringthis process to assure that no physical loss in fiber contentoccurs.7. Apparatus7.1 Cutting (Grooved) Template or DieThe specimen areashall be produced wit
38、h either a cutting templates or a cuttingdie. The cutting template or die shall be designed to producethe nominal specimen area and shall be capable 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 ave
39、rage 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 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 minut
40、e.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 container shall beof a suitable volume for the sample and solvent (a minimum of250 mLis suggested). Other sizes of container may be requireddepending on s
41、ample size, and amount of solvent needed tocomplete the dissolution process.7.4.3 Fritted Glass Crucibles or Sample HolderThe frit-ted glass crucible filter shall be of a suitable porosity to allowdissolved matrix to pass while retaining reinforcement.7.4.4 AgitatorMechanical shaker or ultrasonic ba
42、th. Mini-mum shaker speed recommended is 100 agitations orrevolutions/minute. Minimum frequency for ultrasonic bathrecommended is 40 kHz.7.4.5 Hot PlateThe hot plate shall have adjustable con-trols suitable for heating the solvent to its boiling point and becapable of controlling the temperature to
43、within 615C.7.4.6 Vacuum PumpCapable of delivering vacuum of atleast 50 kPa.7.5 Procedure B:7.5.1 CruciblePorcelain, or equivalent properties, with acapacity sufficient to completely contain the specimen.7.5.2 Electric FurnaceMuffle design capable of maintain-ing 565C +/- 30C for burn-out of the res
44、in matrix.7.5.3 Laboratory DesiccatorDesign for pre- and post-testconditioning of the specimen and crucible.7.5.4 Bunsen FlameA source of a controlled heat flamefor pre-ignition of the specimen.7.5.5 Laboratory Safety EquipmentHeatproof gloves andprotective eyewear are specifically recommended. Labo
45、ratoryexhaust fan and/or ventilation system should be available foruse.8. Reagents8.1 Purity of ReagentsAs a minimum, a technical-gradereagent is required to provide accurate results. A reagent-gradereagent will be used when resolving disputes or performingsubsequent analysis of extract or residue.
46、Unless otherwiseindicated, the reagent shall conform to the specifications of theCommittee on Analytical Reagents of the American ChemicalSociety, where such specifications are available.48.2 Matrix Dissolution SolventsAsuitable solvent shall beselected that is compatible with the material system un
47、der testand the apparatus. Read and understand the precautions listedin Section 9 before selecting a matrix dissolution solvent.Matrix dissolution 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
48、), CH3NOC3H6.8.2.3 Methyl Ethyl Ketone (MEK, 2-Butanone),CH3COC2H5.8.2.4 Dimethylformamide (DMF), (CH3)2NCHO.(WarningAs of the approval date of this standard, DMF waslisted by the International Agency for Research on Cancer inGroup 3 as “not classifiable as to its carcinogenicity tohumans” and is co
49、nsidered a reproductive toxin by the NationalToxicology Program. See a recent DMF safety data sheet formore information.)8.2.5 Dichloromethane (MECL, methylene chloride),CH2Cl2. (WarningAs of the approval date of this standard,MECL was listed by the International Agency for Research onCancer in Group 2B as a “possible human carcinogen.”)8.2.6 Methyl Isobutyl Ketone (MIBK, 4-Methyl-2-pentanone), (CH3)2CHCH2COCH3.9. Hazards9.1 This test method should be used only by laboratoryworkers with general training in the safe handling of chemi-
