1、Designation: D 3529/D 3529M 97 (Reapproved 2003)e1Standard Test Method forMatrix Solids Content and Matrix Content of CompositePrepreg1This standard is issued under the fixed designation D 3529/D 3529M; the number immediately following the designation indicates theyear of original adoption or, in th
2、e case of revision, the year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript 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.e1NOTEWarning/pr
3、ecaution notes were moved into text editorially in October 2003.1. Scope1.1 This test method covers the determination of the matrixsolids content and matrix content of composite materialprepregs. Volatiles content, if appropriate and required, isdetermined by means of Test Method D 3530/D 3530M.1.2
4、This test method focuses on thermosetting matrix ma-terial systems for which matrix may be extracted in organicsolvent. However, other, unspecified reagents may be used withthis test method to extract other matrix material types for thesame purposes.1.3 This test method does not distinguish between
5、hybridreinforcements or matrices. Its use with hybrids is limited to adetermination of total reinforcement or matrix, or the use of astandard factor to be used as the weight of a particularreinforcement or matrix constituent.1.4 Alternate techniques for determining matrix and rein-forcement content
6、include Test Methods C 613/C 613M(Soxhlet extraction) and D 3171 (meant typically for lami-nates; covering matrix digestion or combustion).1.5 The values stated in SI units are to be regarded asstandard.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with
7、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. Specific precau-tionary information is given in 8.2.4 and 8.2.52. Referenced Documents2.1 ASTM Standards:2C 613
8、/C 613M Test Method for Constituent Content ofComposite Prepreg by Soxhlet ExtractionD 883 Terminology Relating to PlasticsD 3171 Test Method for Constituent Content of CompositeMaterialsD 3530/D3530M Test Method for Volatiles Content ofComposite Material PrepregD 3878 Terminology of Composite Mater
9、ialsE 177 Practice for Use of Terms Precision and Bias inASTM Test MethodsE 1309 Guide for Identification of Composite Materials inComputerized Property Databases2.2 NFPA Standard:NFPA 86 Standard for Ovens and Furnaces33. Terminology3.1 DefinitionsTerminology D 3878 defines terms relatingto composi
10、te materials. Terminology D 883 defines termsrelating to plastics. Practice E 177 defines terms relating tostatistics. In the event of a conflict between terms, TerminologyD 3878 shall have precedence over the other documents.3.1.1 fiber content, nthe amount of fiber present in acomposite or prepreg
11、 expressed either as percent by weight orpercent by volume. See Terminology D 3878.3.1.2 matrix content, nthe 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 D 3878.3.1.3
12、prepreg, nthe admixture of fibrous reinforcementand polymeric matrix used to fabricate composite materials. Itsform may be sheet, tape, or tow. See Terminology D 3878.3.1.4 reinforcement content, nthe amount of reinforce-ment present in a composite or prepreg expressed either aspercent by weight or
13、percent by volume.3.1.4.1 DiscussionIf fiber is the sole reinforcement, thenfiber content is equal to reinforcement content. See Terminol-ogy D 3878.3.1.5 resin content, nsee matrix content.1This test method is under the jurisdiction of ASTM Committee D30 onComposite Materials and is the direct resp
14、onsibility of Subcommittee D30.03 onConstituent/Precursor Properties.Current edition approved Oct. 1, 2003. Published October 2003. Originallyapproved in 1976. Last previous edition approved in 1997 as D 3529/D 3529M 97.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact
15、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 BatterymarchPark, Quincy, MA 02269-9101.1Copyright ASTM International, 100 Bar
16、r Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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 test mass.3.2.2 matrix solids content, n
17、see dry resin content.3.2.3 wet resin content, na prepreg resin content that doesnot account for mass loss due to volatiles. This is usedinterchangeably with matrix content and resin content in thistest method.3.2.4 volatiles content, nthe amount of volatiles present ina prepreg expressed as percent
18、 by weight.3.3 Symbols:3.3.1 Mcmass of container.3.3.2 Miinitial mass of the specimen.3.3.3 Mffinal mass of specimen and container at end oftest.3.3.4 Wmmatrix content of specimen in weight percent.3.3.5 Wmsmatrix solids content of specimen in weightpercent.4. Summary of Test Method4.1 Specimens of
19、the prepreg are weighed and subjected tosolvent, that may be heated, until the matrix is dissolved. Thedissolved matrix is rinsed from the reinforcement residuewhich is then dried and weighed. The loss in mass is expressedas matrix content, a percentage of the specimen mass.4.2 Where applicable, adj
20、acent samples are tested for vola-tiles content according to D 3530/D 3530M. A calculation ofamount of resin in the sample after volatiles content issubtracted is expressed as matrix solids content, a percentageof specimen mass. The matrix solids content is applicablemainly to thermosetting matrices
21、.5. Significance and Use5.1 This test method can be used to obtain the matrixcontent or matrix solids content. Knowledge of the matrixcontent or matrix solids content is useful in developingoptimum manufacturing processes. Where volatiles content isconsistent and not critical to process, matrix cont
22、ent shall beused.5.2 This test method is limited to reinforcement constituentsthat do not lose or gain weight upon exposure to solvent andmatrix constituents that do not dissolve in the solvent. Alter-native methods or solvents should be used or an agreementshould be made with the end user for how t
23、o consider the effectof incomplete matrix dissolution or reinforcement weightchange for reporting purposes.6. Interferences6.1 Extent of Cure in Thermosetting SystemsThe effi-ciency of matrix dissolution for thermosetting matrix materialsis directly related to the extent of cure of the resin system.
24、Resins that have started to cross link (such as B-staged resins)will be increasingly more difficult to extract as the cureadvances. This test method may not be appropriate for suchmaterials; one of the methods of Test Method D 3171 is thenrecommended.6.2 Reagent SelectionThe proper reagent, in a sui
25、tablequantity, 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 perform well on all material systems within thescope of this test method.6.3 Ability of Solvent
26、 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 solvent. A solventthat is satisfactory for a given form may not be adequate withthe same materi
27、al of a different form.6.4 Solvent StrengthSolvent strength, or the ability torapidly dissolve the matrix, may be enhanced by increasing theamount of solvent, increasing agitation, increasing tempera-ture, or by placing the sample under vacuum. These are offeredas physical alternatives to use of mor
28、e hazardous solvents, orcombined solvent systems.7. Apparatus7.1 Cutting (Grooved) TemplateCutting templates shallvary no more than 0.4 mm from center line when used. Thisgives a maximum error of 2 %. This is not required if a cuttingdie is used.7.2 Cutting BladeDie cutting blades are recommended to
29、provide a consistent cut area error from sample to sample of nogreater than 0.05 % of the target area. If a die is not available,a single edged blade will be used.7.3 Analytical BalanceThe analytical balance shall becapable of reading to within 61 mg.7.4 Timer, accurate to nearest minute.7.5 Fume Ex
30、haust Hood.7.6 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 mL is suggested). Other sizes of container may be requireddepending on sample size, and amount of solv
31、ent needed tocomplete the dissolution process.7.7 Fritted Glass Crucibles or Sample HolderThe frittedglass crucible filter shall be of a suitable porosity to allowdissolved matrix to pass while retaining reinforcement.7.8 AgitatorMechanical shaker or ultrasonic bath. Mini-mum shaker speed recommende
32、d is 100 agitations orrevolutions/minute. Minimum frequency for ultrasonic bathrecommended is 40 kHz.7.9 Hot PlateThe hot plate shall have adjustable controlssuitable for heating the solvent to its boiling point and becapable of controlling the temperature to 615C.7.10 Vacuum PumpCapable of deliveri
33、ng vacuum of atleast 50 kPa.8. Reagents8.1 Purity of ReagentsAs a minimum, a technical-gradereagent is required to provide accurate results. However, whenresolving disputes or performing subsequent analysis of extractor residue, a reagent-grade reagent shall be used. Unlessotherwise indicated, it is
34、 intended that the reagent conform toD 3529/D 3529M 97 (2003)e12the specifications of the Committee on Analytical Reagents ofthe American Chemical Society, where such specifications areavailable.48.2 Matrix Dissolution SolventsA suitable solvent shall beselected that is compatible with the material
35、system under 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 Pyrrolidi
36、none (NMP), 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 2B as a “possible human carcinogen” and is considereda repr
37、oductive toxin by the National Toxicology Program. Seea recent DMF material safety data sheet for more 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 2A a
38、nd 2B as a “probable human carcino-gen.”)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-cals. A source of useful information is given in Footnote 8
39、.5(PrecautionIn addition to other precautions, consult theappropriate material safety data sheet for each material used,including reagent materials and test specimen materials, forspecific recommendations on safety and handling.)(PrecautionIn addition to other precautions, the extractionand filterin
40、g processes should be performed under a suitablevented chemical fume hood.) (PrecautionIn addition toother precautions, materials that have been exposed to poten-tially toxic or flammable reagents should be air-dried under ahood before being subsequently oven-dried to eliminate abuildup of a potenti
41、ally dangerous concentration of vapor inthe drying oven. NFPA 86 provides guidelines on amount offlammable materials that may be safely placed in an oven.)9.2 Use of mixed matrix dissolution solvents with differentboiling points are not covered by this test method.(PrecautionIn addition to other pre
42、cautions, do not usemixed solvents without knowing how the mixed solvent willreact under test conditions, which includes drying.)10. Test Specimens10.1 A minimum of three specimens shall be tested for eachsample.10.2 The specimen size shall be a minimum of 6400 mm2.Minimum mass of the specimen shall
43、 be 1 g.11. Calibration and Standardization11.1 All measuring equipment shall have certified calibra-tions that are current at the time of use of the equipment. Thecalibration documentation shall be available for inspection.12. Conditioning12.1 Store composite prepreg with thermosetting resins atlow
44、 temperatures as recommended by the manufacturer (typi-cally approximately 18C (0F). Allow sealed packages ofmaterial to warm as recommended by manufacturer or control-ling specification before seal is opened to ensure that thematerial does not absorb moisture from the atmosphere.12.2 Do not expose
45、the material, that usually has somevolatile content, at ambient temperature for long periods oftime before testing is begun. The material may stage (see 6.1)or lose volatiles, that gives a false indication of matrix solidscontent.13. Procedure13.1 Matrix Content:13.1.1 Weigh each specimen on an anal
46、ytical balance to 0.1mg. Record the mass of each specimen as W1.13.1.2 Place each specimen in a separate container using aminimum of 100 mL of solvent.13.1.3 Sample shall be in the solvent at the steady statecondition of the test for a minimum of three min. The steadystate condition may be one or mo
47、re of the following:13.1.3.1 AgitationMay be used to speed dissolution ofresin into the solvent. Minimum shaker agitation of 60 cycles/minute. Recommended minimum ultrasonic frequency 40 kHz.13.1.3.2 PressureVacuum may be used to lower solventpressure and initiate boiling at lower temperatures. This
48、 isuseful for solvents with high vapor pressure such as MEK orMECL. Recommended vacuum is below 50 kPa.13.1.3.3 TemperatureA raised temperature may be used toincrease solvent efficiency and reduce resin dissolution times.Recommended temperatures are in the range above roomtemperature up to the boili
49、ng point of the solvent.13.1.4 Decant solution.13.1.5 Repeat 13.1.3 and 13.1.4 at least one additional time.NOTE 1A change of solvents or conditions may be made. Also a rinsesolvent may be used to make the sample easier to dry. When changingsolvents, be sure to assess solvent compatibility and also additionalhazards when drying the material.13.1.6 Place the sample in a weighed, fritted glass crucibleor other suitable container of recorded mass, W2. Dry thesample in a circulating oven at a temperature and timesatisfactory to remove the solv
