1、Designation: C613 97 (Reapproved 2008)2C613 14Standard Test Method forConstituent Content of Composite Prepreg by SoxhletExtraction1This standard is issued under the fixed designation C613; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, the year of last revision. A number 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 U.S. Department of Defense.1 NOTEThis standard was c
3、orrected to a single-designation standard editorially in October 2013.2 NOTEThe designation of this standard was corrected editorially in November 2013.1. Scope1.1 This test method covers a Soxhlet extraction procedure to determine the matrix content, reinforcement content, and fillercontent of comp
4、osite material prepreg. Volatiles content, if appropriate, and required, is determined by means of Test MethodD3530/D3530MD3530.1.1.1 The reinforcement and filler must be substantially insoluble in the selected extraction reagent and any filler must becapable of being separated from the reinforcemen
5、t by filtering the extraction residue.1.1.2 Reinforcement and filler content test results are total reinforcement content and total filler content; hybrid material systemswith more than one type of either reinforcement or filler cannot be distinguished.1.2 This test method focuses on thermosetting m
6、atrix material systems for which the matrix may be extracted by an organicsolvent. However, other, unspecified, reagents may be used with this test method to extract other matrix material types for the samepurposes.1.3 Alternate techniques for determining matrix and reinforcement content include Tes
7、t Methods D3171 (matrix digestion),D2584 (matrix burn-off/ignition), and D3529/D3529MD3529M (matrix dissolution). dissolution and ignition loss). Test MethodD2584 is preferred for reinforcement materials, such as glass, quartz, or silica, that are unaffected by high-temperatureenvironments.1.4 The t
8、echnical content of this standard has been stable since 1997 without significant objection from its stakeholders.As thereis limited technical support for the maintenance of this standard, changes since that date have been limited to items required toretain consistency with other ASTM D30 Committee s
9、tandards. The standard therefore should not be considered to include anysignificant changes in approach and practice since 1997. Future maintenance of the standard will only be in response to specificrequests and performed only as technical support allows.1.5 The values stated in SI units are to be
10、regarded as standard. No other units of measurement are included in this standard.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and d
11、etermine the applicability of regulatorylimitations prior to use. Specific precautionary statements are given in Section 9 and 7.2.3 and 8.2.1.2. Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD2584 Test Method for Ignition Loss of Cured Reinforced ResinsD3171 Test Meth
12、ods for Constituent Content of Composite MaterialsD3529/D3529MD3529M Test MethodMethods for Matrix Solids Content and Matrix Content Constituent Content of CompositePrepreg1 This test method is under the jurisdiction of ASTM Committee D30 on Composite Materials and is the direct responsibility of Su
13、bcommittee D30.03 onConstituent/Precursor Properties.Current edition approved March 1, 2008Oct. 15, 2014. Published April 2008November 2014. Originally approved in 1967. Last previous edition approved in 2003 asC613 97(2003)1 2. DOI: 10.1520/C0613_C0613M-97R08E02.10.1520/C0613-14.2 For referencedAST
14、M standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user o
15、f an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as pu
16、blished by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D3530/D3530MD3530 Test Method for Volatiles Content of Composite Material PrepregD3878 Terminology for Composite MaterialsE122 P
17、ractice for Calculating Sample Size to Estimate, With Specified Precision, the Average for a Characteristic of a Lot orProcessE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE456 Terminology Relating to Quality and StatisticsE1309 Guide for Identification of Fiber-Reinforce
18、d Polymer-Matrix Composite Materials in DatabasesE1471 Guide for Identification of Fibers, Fillers, and Core Materials in Computerized Material Property Databases2.2 NFPA Standard:NFPA 86 Standard for Ovens and Furnaces33. Terminology3.1 DefinitionsTerminology D3878 defines terms relating to composi
19、te materials. Terminology D883 defines terms relatingto plastics. Terminology E456 and Practice E177 define terms relating to statistics. In the event of a conflict between terms,Terminology D3878 shall have precedence over the other documents.3.2 Definitions of Terms Specific to This Standard:Termi
20、nology3.2.1 dry resin content, nprepreg resin content calculated by subtracting the average mass loss due to volatiles from the initialtest specimen mass.3.2.2 filler content, nthe amount of filler present in a prepreg or composite expressed either as percent by weight or percentby volume.3.2.2.1 Di
21、scussionIn this test method the reinforcement is separated from the remainder of the material, which includes the matrix and the filler. Ifthe filler is not then separated from the matrix to determine the proportion of each, then the filler content is included in the matrixcontent.D3878 defines term
22、s relating to composite materials. Terminology D883 defines terms relating to plastics. TerminologyE456 and Practice E177 define terms relating to statistics. In the event of a conflict between terms, Terminology D3878 shall haveprecedence over the other documents.3.2.3 matrix content, nthe amount o
23、f matrix present in a composite or prepreg expressed either as percent by weight or percentby volume. For polymer matrix composites this is resin content. D38783.2.4 prepreg, reinforcement content, nthe admixtureamount of fibrous reinforcement and polymeric matrix used to fabricatecomposite material
24、s. Its form may be sheet, tape, or tow. For thermosetting matrices it has been partially cured to a controlledviscosity called “B stage”.reinforcement present in a composite or prepreg expressed either as percent by weight or percent byvolume. This is sometimes stated as a fraction, that is, reinfor
25、cement volume fraction. D38783.2.5 resin content, replicate, nsee matrix content.a test specimen tested under nominally identical conditions as other testspecimens from the same sample. D38783.1.4 sample, na small part or portion of a material or product intended to be representative of the whole. D
26、8833.2.6 test result, nthe value obtained for a given property from one test unit.43.2.6.1 DiscussionA test result may be a single observation or a combination of a number of observations when two or more test specimens aremeasured for each test.3.2.7 test specimen, na test unit or portion of a test
27、 unit upon which a single or multiple observation is to be made.43.2.8 test unit, na unit or portion of a material that is sufficient to obtain a test result(s) for the property or properties to bemeasured.3.2.8.1 DiscussionA test unit may be a subunit of a primary (first stage) sampling unit or it
28、may be a subunit of a composite of primary samplingunits or of increments from these primary sampling units.3 Available from National Fire Protection Association (NFPA), 1 Batterymarch Park, Quincy, MA 02269-9101.4 See Form and Style for ASTM Standards.C613 1423.2.9 volatiles content, nthe amount of
29、 volatiles present in a prepreg expressed as percent by weight.3.2.10 wet resin content, nprepreg resin content determined by considering volatiles as part of the resin mass.3.2 Definitions of Terms Specific to This Standard:3.2.1 dry resin content, nprepreg resin content calculated by subtracting t
30、he average mass loss due to volatiles from the initialtest specimen mass.3.2.2 filler content, nthe amount of filler present in a prepreg or composite expressed either as percent by weight or percentby volume.3.2.2.1 DiscussionIn this test method the reinforcement is separated from the remainder of
31、the material, which includes the matrix and the filler. Ifthe filler is not then separated from the matrix to determine the proportion of each, then the filler content is included in the matrixcontent.3.2.3 reinforcement content, nthe amount of reinforcement present in a composite or prepreg express
32、ed either as percent byweight or percent by volume. This is sometimes stated as a fraction, that is, reinforcement volume fraction.3.2.4 replicate, na test specimen tested under nominally identical conditions as other test specimens from the same sample.3.2.5 volatiles content, nthe amount of volati
33、les present in a prepreg expressed as percent by weight.3.2.6 wet resin content, nprepreg resin content determined by considering volatiles as part of the resin mass.3.3 Symbols:3.3.1 Ainitial mass of dry reinforcement during a reagent exposure evaluation.3.3.2 Bfinal mass of dry reinforcement durin
34、g a reagent exposure evaluation.3.3.3 cpercent reinforcement mass change due to reagent exposure.3.3.4 CVcoefficient of variation statistic of a sample population for a given property.3.3.5 Maadditional mass of filler in the test specimen.3.3.6 Memass of the test specimen extraction residue.3.3.7 Mi
35、initial mass of the test specimen.3.3.8 Mrmass of reinforcement in the test specimen.3.3.9 nnumber of replicates in the sample population.3.3.10 sn1standard deviation statistic of a sample population for a given property.3.3.11 Wfweight percent of filler in prepreg.3.3.12 Wmweight percent of matrix
36、in prepreg.3.3.13 Wrweight percent of reinforcement in prepreg.3.3.14 xitest result for an individual test specimen from the sample population for a given property.3.3.15 xaverage value of a sample population for a given property.4. Summary of Test Method4.1 The exposed surface area of the prepreg m
37、aterial test specimen is increased by cutting the test specimen into smaller pieces.The test specimen is weighed and the matrix material removed by means of Soxhlet extraction. The extracted residue is dried andweighed. If a filler is present in the residue, in addition to reinforcement, the two com
38、ponents are separated by filtering the residue.From mass measurements of the initial test specimen, and of the residue taken at various stages in the process, the matrix content,reinforcement content, and filler content are calculated and reported in weight percent.4.1.1 Soxhlet ProcessWhile describ
39、ed in detail in common quantitative chemical analysis textbooks, the Soxhlet process issummarized as follows. The test specimen is loaded into a filtering extraction thimble, which is placed into the extraction chamberof a Soxhlet extraction assembly (see Fig. 1) containing an appropriate extraction
40、 reagent. The porous thimble allows the liquidextraction reagent to pass while retaining the test specimen. Freshly distilled liquid reagent enters from the top of the extractionchamber, filling it until the liquid reaches the highest level of the reagent-return tube.At this moment the tube operates
41、 as a siphon,draining the extraction chamber completely as it returns the liquid reagent and any extracted material to a reservoir beneath theextraction chamber. The heated reservoir boils the reagent, the vapor of which is led to a condenser placed above the extractionchamber. The distilled condens
42、ate then drips down into the thimble, starting once again the process of filling the extractionchamber. The Soxhlet operation is not a continuous operation, but rather a sequence of fillings and siphonings, each cycle of whichC613 143is called a reflux change. The heat input and reagent volume are a
43、djusted to cause the boiling reagent to return to the extractionflask from the condenser at 3 to 10 reflux changes per hour, with the extraction continuing for a minimum of 4 h or 20 refluxchanges, whichever comes first.4.1.2 Volatiles ContentVolatiles content is primarily applicable to thermosettin
44、g materials, and, if required, is determined byTest Method D3530/D3530MD3530. Volatiles content determination requires different test specimens than those used in theextraction process, since the process of determining volatiles content renders thermosetting material specimens unsuitable forsubseque
45、nt organic solvent extraction.5. Significance and Use5.1 The prepreg volatiles content, matrix content, reinforcement content, and filler content of composite prepreg materials areused to control material manufacture and subsequent fabrication processes, and are key parameters in the specification a
46、ndproduction of such materials, as well as in the fabrication of products made with such materials.5.2 The extraction products resulting from this test method (the extract, the residue, or both) can be analyzed to assess chemicalcomposition and degree of purity.6. Interferences6.1 Extent of Cure in
47、Thermosetting SystemsThe efficiency of extraction for thermosetting matrix materials is directly relatedto the extent of cure of the resin system. Resins that have started to cross-link (such as B-staged resins) will be increasingly moredifficult to extract as the cure advances. This test method may
48、 not be appropriate for such materials; Test Methods D3171 or D2584may be better test method choices.6.2 Reagent SelectionThe proper reagent, in a suitable quantity, must be selected for the constituents under test. The reagentslisted in Section 8 are provided for consideration, particularly with re
49、gard to thermosetting materials, but cannot be assured toperform well on all material systems within the scope of this test method.6.3 Thimble ContaminationIf the extract is to undergo further analysis, the thimble must be clean to avoid a significant sourceof contamination.6.4 Reinforcement Mass Change As a Result of ReagentThe calculations of this test method assume that the reinforcementmass (or filler, if filler content is being determined) is not significantly affected (whether mass increase or mass loss) by exposureto th
