1、Designation: D 3530/D 3530M 97 (Reapproved 2008)Standard Test Method forVolatiles Content of Composite Material Prepreg1This standard is issued under the fixed designation D 3530/D 3530M; the number immediately following the designation indicates theyear of original adoption or, in the case of revis
2、ion, 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.1. Scope1.1 This test method co
3、vers the determination of the vola-tiles content, in weight percent of composite material prepregs.This standard focuses on composites with thermosetting resinsthat tend to lose a few percent of the matrix mass when heateddue to loss of both retained water and low molecular weightmatrix constituents
4、 that volatilize during heating.1.2 Use of this test method is limited to maximum tempera-ture of circulating air ovens (approximately 300C).1.3 Use of this test method is limited to temperatures belowwhich the matrix flows from the reinforcement.1.4 The values stated in SI units are to be regarded
5、asstandard.1.5 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. Spe
6、cific precau-tionary statements are given in Section 8.2. Referenced Documents2.1 ASTM Standards:2D 3878 Terminology for Composite MaterialsE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 1309 Guide for Identification of Fiber-ReinforcedPolymer-Matrix Composite Materials
7、in Databases2.2 NFPA Standard:NFPA 86 Standard for Ovens and Furnaces33. Terminology3.1 DefinitionsTerminology D 3878 defines terms relatingto composite materials. Terminology D 883 defines termsrelating to plastics. Practice E 177 defines terms relating tostatistics. In the event of a conflict betw
8、een terms, TerminologyD 3878 shall have precedence over other documents.3.1.1 prepreg, nthe admixture of fibrous reinforcementand polymeric matrix used to fabricate composite materials. Itsform may be sheet, tape, or tow. See Terminology D 3878.3.2 Definitions of Terms Specific to This Standard:3.2.
9、1 Volatiles Content, nthe amount of volatiles presentin a prepreg expressed as a weight percent.3.3 Symbols:3.3.1 Mithe initial mass of the sample.3.3.2 Mfthe mass of the sample after oven exposure.3.3.3 Vcthe weight percent volatiles content.4. Summary of Test Method4.1 Specimens of prepreg are wei
10、ghed and then exposed toelevated temperature, equal to the nominal cure or consolida-tion temperature of the material, in an air circulating oven toremove the volatiles. The exposed samples are reweighed andthe percent change in weight expressed as volatiles content.5. Significance and Use5.1 This t
11、est method is used to obtain the volatiles contentof composite material prepreg. Knowledge of the volatilescontent is useful in developing optimum manufacturing pro-cesses.5.2 The volatiles content is determined after exposure to thenominal cure or consolidation temperature.6. Interferences6.1 Airfl
12、owThe amount of measured volatiles may beincreased or decreased by changing the velocity of airflow.Since airflow in most ovens is not linear in each part, avelometer should be used to measure airflow where samplesare placed. Samples should be placed only in positions ofknown airflow so that results
13、 may be repeatable. Use of baffleshas been found to even airflow between samples.1This 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 March 1, 2008.
14、Published April 2008. Originallyapproved in 1976. Last previous edition approved in 2003 as D 3530/D 3530M 97(2003).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
15、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.6.2 Sample ExposureThe geom
16、etric shape and position-ing of the sample have an effect on the measured volatilescontent. Samples placed horizontally in a rack will not beexposed to the same amount of airflow as samples hungvertically. A ribbon wound in a 150 mm diameter hoop maygive slightly different results than the same ribb
17、on wound in a50 mm diameter hoop. A thinner sample will be exposed tomore airflow at its surface than a thicker sample.6.3 Time of ExposureFor any given temperature, sampleplacement, and airflow, the sample will lose volatiles at a setinitial rate, that decreases over time. After some time period,vo
18、latiles lost in the test will approach the true volatiles contentof the sample. If the time period is not sufficient to show a truevolatiles content of the material, the volatiles content isrepresentative of only the condition of the test.6.4 Time of Ambient ExposureVolatiles content varies dueto pr
19、olonged exposure of temperatures exceeding prepreg glasstransition temperature or exposure to humidity. This change isassociated with matrix crosslinking and change in tack.7. Apparatus7.1 Cutting BladeDie cutter that provides fixed specimenarea to within a tolerance of 0.5 % is recommended. Singlee
20、dge blade is acceptable.7.2 Cutting TemplateWhen a die cutter is not used, acutting template is required. The cutting template shall havegrooves within a tolerance of 0.4 mm parallel true positionfrom center line. This allows a 2 % area error.7.3 Analytical BalanceThe analytical balance shall becapa
21、ble of reading to within 60.1 mg.7.4 Circulating Air Oven, capable of tolerance within 63C.Removable baffles should be placed in the oven so that airflowis not directly aimed at the specimen.7.5 Rack, that allows air circulation and from which hooksmay be suspended.7.6 Timer, capable of reading 20 6
22、 1 min.7.7 Desiccator.8. Hazards8.1 Some materials contain flammable or toxic solvents aspart of the matrix. These materials could build up to dangerousconcentrations of vapor in the oven. NFPA 86 provides guide-lines on amount of flammable materials that may be safelyplaced in an oven.9. Test Speci
23、mens9.1 A minimum of three specimens shall be tested for eachsample.9.2 The specimen size shall be a minimum of 1600 mm2bymaterial thickness. Ribbon, braid, and fabric forms that do notdrip resin shall be suspended from the rack. Ribbon shall belooped in close proximity so that individual strands ar
24、e notclumped together. Other forms may be placed horizontally onthe rack.10. Calibration and Standardization10.1 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.11. Conditi
25、oning11.1 Store carbon fiber-epoxy prepreg at low temperaturesas recommended by the manufacturer (typicallyapproximately 18C). Allow sealed packages of material towarm as recommended by manufacturer or controlling speci-fication before seal is opened to ensure that the material doesnot absorb moistu
26、re from the atmosphere.12. Procedure12.1 Weigh each of the three specimens on an analyticalbalance to 0.1 mg. Record the mass of each specimen as Mi.12.2 Coat any surfaces of the rack or clip that may contactthe specimen with a suitable release agent to prevent loss ofspecimen weight due to resin ad
27、herence.12.3 Place the samples on the rack or suspended from therack (braids, ribbons, and fabric) as quickly as possible, placethe rack into a preheated oven, and set at the nominal cure orconsolidation temperature as recommended by the manufac-turer or controlling specification. The specimens shou
28、ld beplaced so that the maximum surface area is exposed to thecirculating heat.12.4 Set the timer for 15 min.NOTE 1Other times may be used, but a timed study shall beperformed showing that at least 90 % of the maximum volatiles content isobtained at the recommended time.12.5 Remove the specimens fro
29、m the rack and place them ina desiccator.12.6 Remove the specimens from the desiccator after theyhave cooled to ambient (a minimum of 5 min). Weighspecimens within 1 min of removal from desiccator. Recordthis mass as Mf.13. Calculation13.1 Calculate the volatiles content Vc, weight percent, ofeach s
30、pecimen as follows:Vc5Mi2 MfMi3 100 (1)where:Mi= initial weight of prepreg specimen, g, andMf= weight of specimen after removed from oven, g.14. Report14.1 Report the following information or references point-ing to other documents containing the information to themaximum extent applicable:14.1.1 Re
31、porting of items that are beyond the control of agiven test laboratory, such as material details shall be theresponsibility of the requestor,14.1.2 Complete identification of the material according toGuide E 1309 including fiber type, surface treatment, fibermanufacturer, resin system, resin manufac
32、turer, prepreg manu-facturer, prepreg form, prepreg areal weight, and prepregmatrix content,14.1.3 The time and temperature to remove the volatiles,14.1.4 Specific ambient exposure conditions and time ateach condition, and14.1.5 The volatiles content for each of the three specimensexpressed as weigh
33、t percent, the average volatiles content.D 3530/D 3530M 97 (2008)215. Precision and Bias15.1 PrecisionThe data required for the development of aprecision statement is not available for this test method.Committee D30 is currently planning a round-robin test for thistest method in order to determine p
34、recision.15.2 BiasBias cannot be determined for this test methodas no acceptable reference standard exists.16. Keywords16.1 composite materials; prepreg; volatiles contentASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedi
35、n 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 revision at any time by the responsible technical committee and mu
36、st 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. Your comments will receive careful consideration at a meeting of th
37、eresponsible 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 copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C70
38、0, 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).D 3530/D 3530M 97 (2008)3
