1 Standard Method of Test for FIBER CONTENT OF REINFORCED RESIN COMPOSITES' 1. Scope 1.1 This method covers the determination of the fiber content of resin matrix composites. “The technique wed is ase onthe digestion of the matrix resin by oxidizing rolent, hich Jo ot ailack the Ribers excessively 2 Applicable Documents ASTM Stondards 'D192 Test for Specific Gravity and Den- sity of Pastis by Displacement” 23. Summary of Method 3.1 The method consists of digest resin portion of weighed composite specimen ina hot digestion medivm,weualy an oxidizing Solion, The residue is ier, washed, died, fnd weighed. The weight percent of fiber can then be converted Lo 4 lume percent if the fiber density is known. A correction for the ‘eight loss of fiber maybe made 3.2 Two procedures are given A, for eesins Aigetble by concentrated iti ack, and 8 for resins digestible by an aqueous mixture of sulfuric acd and hydrogen peronide. As exar- ples of resin, epories come under Procedure A tnd polyimides under Procedure 4. Signiicane 4,1 The iter content fa composite must be determined to calculate the apparent strength land moduler ofthe riaforcing fibers inthe impose. may be Torther used 10 evaluate the quality ofa given specimen. 5. Apparaes S11 General 5.41 Medium porosity feted sintered Fike. S12 Ceucible holes 513 Anata balance. 5.14 Drying oven capable of attaining 100" 5.18 Borosiicate glass vacuum fier Mask 5.16 A vacuum source capable of 169 KPa (127 oH) presse 5.2 Procedure 4 55.2 Flask witha standaed-tape joints, 5.2.2 Water relox condensers with sland. ard-aper joins 5.23 Temperatue-repulted water or oll bath, 5.3 Procedure B 5.31 Disposable capillary Pasteur pipet. 5.32 Hot plo 6. Reagents 6.1 Procedure 4 6.11 Nitric sei, concentrated, greater than 10 % aqueous, ACS reagent grade, (62 Procedure Be 6.21 Hydrogen peroxide, 50% aqueous ep grate, "= Gini aprons March, 1973, Passed May PT gamal Book of ASTM Sunder, Par 3. iinaailiiicalleat6.22 Sulfrie ac, concent 4% aqueous, ACS rengent grade 7, Safty Precantions 7.1 Fity percent hydrogen peroxide should be stored in coat safety hood, inthe orginal container with a vented cap and beaker placed loosely over the top as a dust cover. Under ‘these conditions, the reagent Is quite stable Fifty peroent 110s should not be allowed to ome in contact with any organic: material Spills shouldbe flushed with copious quantities of water. The reagent will produce instant “white barat” on the skin, i essential that rubber gloves and eye protection be worn when the reagent i bing bandied. Any buras should be washed immediatly with water to prevent rial bistering, 7.2 All oxidations should be carried out bhind a safety shield, No atempt should ever be made to purify the 50% HDs by distil: tion. Explosive decomposition is su to occur with boing solution containing 65% Hs0y.” 18, Test Specimens 81 Preferably five or more specimens each weighing a east 030g ae cut from the sample Of interest. The specimen may be of any onvenient shape as fong as it will ato the beaker used in the tet 9. Procedures 9.1 Procedure A—Epoxy resin matrices (and others which can be digested by HINO.) B11 Weigh each specimen on an analytical balance to four significant Figures. 9.12 Determine the density of each spec amen by a Tiguid displacement technique, as described in Method D792 ifthe fiber content by volume i require. 19.1.3 Place each specimen in a separate Mask containing 30 ml of 10 % HNO, 9.14 FH the Masks with relox condensers and pace them ina constant temperature water ‘or oll ith held a 751°C. 9:15 Aller $'h or when the digestion is complete (Note 1, record the total digestion time forthe purposes of 10.1. Fite the con tents of each Matk onto tard sintered:pass Fier under a vacuum of 169 KPa (127 man Hg) for belle Wash the fiber with excess water Totloned by eetone, pai (Note ICeuin ten maces may rege ide af ining toch or de obs 9.16 Place the filer and specimen in an ‘vet at 100°C for 11a remove residual water tnd acetone. 9.17 Cool the filter containing the fiber reside 1o room temperature ina desicator and ‘igh the sample accurately (four siniieant, Figures om an analytical balance 92 Procedure B—Polyimde or phenolic resin mateices (and thers which ean be dic ested by aqueous sulfur sid-hydrogen pe Toni mature) 9.2.1 Weigh each specimen on an analytics balance to four signifiaat figures, 19.22 Determine the density of each speci- rmen by a liquid displacement technique, as ‘described ig Method D792, ite iber content by volume i eauired, 9.23 Place each specimen into a suitable bear 9.24 Ad 20 10 28 ml of concentrated sulfuric acid 10 the specimen. (Caution: less than 20 mil must not be used.) Place the beaker wth the acid specimen mints on hotplate ‘nd het until the sulfuric acibegins to fue, 9.25 Aller the solution hat become dark, sud the 50% H,O, solution dropwise dawn the fide of the beaker. Wear rather gloves wile Aoing 50, Continue the aditin unit about 35 fmt have been added. Allow the solution to Continue 1 heat for 3 min, When he oxidation ofthe resin matie is compet, the fibers oat {o the top and the solution below the fibers becomes clear. Hater 5 min the solution snot lear, add some more H,O, “he (lal amount Of H.Os neaded to oxidize the resin matrix Completely variable and depends on the ype lof eesin and sample size (Note 9.2.6 When the oxidation scomplete, record the total digestion time forthe purposes of 10.1 Remote the beaker feom the hot plate and allow the solution t cool The cooling may be facitated by placing the beaker in ance bath 9.21 Filler the contents of sch beaker onto 4 tored sintered glass titer urder a vacuum of «ah {6 9Pa(127 mm Heo ster Waster wih excess water fod by atone 8 mice the fer an specimen a0 oven at LOD for 1 ho em seul war Saat 9129 Coal the fier consining the Mer cstv oom temperate na dsiceao and Sigh the sample cra) to Tow scant Mies ona unt! bloc 10, Correction for Fiber Weight Loss by Sol- 10.1 Weigh one blank consisting ofa bundle of fibers of ‘weight equal to the estimated mount present in the samples being digested fon an) analytical balance to four significant Figures 102 Repeat Procedute A @.1) or B (2.1) whichever ts applicable, with the blank (10.1) Gigested for an equal tngth of time as the 10.3 The fiber weightloss by solvent action csavals the combined weight ofthe iter andthe Sartng fiber minus the combined weight ofthe Fier and the eemsising ber. Only differences Tanger than 03 % should be considered sigs cet (Note 2). ‘Nore 2—Ceran fibers may, when i equiv sihthe hamid of he moore contin wet anl wishing a Snes name) Stvronment sould be yployed To iferetinte dine iter atck. by the soe! and mostre ‘lap em the atmosphere, 11, Catewatons Hct Weight of fiber in composite equals the ‘combined weight ofthe iter and the residue as fetermined in 9.1.7 of 929 plus the fiber ‘weigh tose {0 the rolrnt determined in 10:3 ‘ins the tate of the Miter. puta of i drt oti ae wth end tra St ee tn ee pai 1.2 Calelate weight percent fiber incom posite a fllows: ier at = (5 10 1.3 Calculate volume percent fiber in compos. ite a follows ber, vl = [HY] 100 whee: We weight of fiber in composite, ve = weight of inal eompaste specimen, P= ‘ber density, and composite density 12 Report 12.1 The report shall inclce the following 121 Complete identification of satel tested including type, source, form, principal dimensions, and previous history, 12.12 Number of species measured per 213 Average value and standard deviation of wight percent of fiber in composite, and [Bit Average vale and standard deviation of volume percent of ber in sompost 131 The following eritera should be used for judging the acceptability o results at 295% confidence leek TET Repeatabiliy—Two results (cach the average of duplicate determinations) obtained bythe same analyst. shoul be. conser stepect if they ilfer by more than LO, absote, T.L2 Reproducibiliy—Two results (seh the average of duplicate determinations) ob tained by diferent laboratories should be con sidered suspect they difer 9y more than 15 5 absolute ssn ofan ut es cma Fe elven batt ok a oo