1、, A. E. C. M. A. STAN DAR D NORME A. E.C. M.A. A.E.C.M.A. NORM prEN 2559 Issue P 1 October 1988 EDITE PAR LASSOCIATION EUROPENNE DES CONSTRUCTEURS DE MATERIEL AROSPATIAL 88, boulevard Malesherbes, 76008 PARIS - TEL. 45-63-82-85 UDC : Key words : ENGLISH VERSION Aerospace series Carbon fibre preimpre
2、gnates Test method for the determination of the resin and fibre content and the mass of fibre per unit area Srie arospatiale Luft- und Raumfahrt Mthode dessai Prfverfahren pour la dtermination zur Bestimmung Primprgns de fibres de carbone Kohlenstoffaser-Prepreg de la teneur en rsine et en fibres et
3、 de la masse surfacique de la fibre des Harz -und Fasermasseanteiis und der flchenbezogenen Fasermasse This Aerospace Series pre-standard has been drawn up under the responsibility of AECMA (Association Europenne des Constructeurs de Matriel Arospatial), It is published on green paper for the needs
4、of AECMA-Members. It has been technically approved by the experts of the concerned AECMA Commission following comment by the Member countries. Subsequent to the publication of this pre-standard, the technical content shall not be changed to an extent that interchangeability is affected, physically o
5、r functionally, without re-identification of the standard. After examination and signature of the AECMA Standard Checking Centre (NPS) and formal agreement of the Official Services of the Member countries it will be submitted as a draft European Standard to CEN (European Committee for Standardizatio
6、n) for final vote. Nota - Extra copies can be supplied by B.N.A.E. - 8, rue Moreau-Vauthier - 92100 BOULOGNE-BILLANCOURT Edition approved for publication Comments should be sent within six months C7 Chairman after the date of publication decision 88, Bd. Malesherbes 17th October 1988 A.E.C.M.A. Mr.
7、BEZAUD 75008 PARIS - FRANCE aecma 1988 AECMA PREN2557 88 101Z3Ll 0003Lf85 T prEN 2559 Page 2 Contents 1 2 3 4 5 6 7 8 9 10 11 Scope and field of application References Definitions Principle of the method Designation of the method Apparatus Standard atmosphere for conditioning and testing Sampling an
8、d test specimens Procedure Calculation and expression of results Test report 0619XSP1387T5 AECMA PREN2559 88 LOL23LJ C10039p8b L prEN 2559 Page 3 1 Scope and field of application This ctcindard specifies a Iuettiod for determining the resin content (with or without volatiles) and fi.bre content and
9、mass of fibre per uni area of a carbon fibre preimpregnate, for aerospace use. 1.1 If the material to be tested contnfns only carbon and a resin which is completely combustible (urder the conditions of this test methcd) , the resiti content is equal to the loss on wet combustion (see note below). 1.
10、2 As an alternative to clause 1.1 , the resin cor,tent is equal to the loss or; sclvent extraction (see note below). Eiote : The carbon used as a reinforcement can be coated with 2 resin cLze and in this case, this will be eliminated during wet corfibuston or solvent extraction and thereiore include
11、d in the result. 1.3 This stardurd does not give any directions iiecessary to meet the health and safety requirements. It is the resyonsibilPty cf the use+ of this stnndard to cortsult nd establish appropriate health and safety precautlmo . 0 2 Referciices EN 2557 Aerospace series - Carbon fibre pre
12、impregnates - Test method for the determimtion of mass per unit area i EN 2558 Aerospace series - Carbon Eibre preimpregnates - Test method for the determination of the pezceiltage of olat ti le matter 1) EN 2743 Aerospace series -a Reinforced plastics - Standard atmospheres for conditioning and tes
13、ting 1) 3 l)eiiriitionc k cerbon fibre pxeimpregnate with a thermosettfng or thernoplastic resin is a material thuc can be purchased in the form o a synthetic resin impregnated carbon fibre ur.idirectioni sheet, tape or woven fabric aiid iised for the narturacturc of moulded conponents. 8 4 Principl
14、e of the metlics 4.1 Vet: coinbustLon method DetermLiiation of the difference in Ioass by mzns of weighing Sefore 2nd after removal of the resin by it wet combustion method, employing coricentraied auiphuric aclci md hydrogeiz peroxide solution, to constant nass. i) In preperatior, AECMA PREN2557 88
15、 m LOL231L 0003487 3 m prEN 2559 Page 4 4.3 Solvent extraction nethod. Determination of the. difference in muss by means cf weighir,g before aiid nfter extraction of the resin with methyl ethyl ketone or other suitable solvent, as agreed between the purchoser and the supplier, to constant mass. Two
16、variants are possible : 4.2.1 A standard method of extraction using a Soxhlet. 4.2.2- A fsster method of extraction by soakiiig and decantution. 5 Designation of the method Carbon fibre preimpregnates Test method for the determinstion of the resin and fibre content and the mass of fibre per unit are
17、a EN 2559 - A Title description Standard number Method of test procedure (see table 1) Table 1 Principle Procedure Wet combustion (see clause 4.1) See clause 9.1 Solvent extraction using Soxhlet (see clause 4.2.1) See clause 9.7 Solvent extraction by soaking and decantation See clause 3.3 (see claus
18、e 4.2.2) 6 Apparat u s Gal 6.2 Template of standrd specimen 6.3 Accillary items such as sharp cutting knife and tweezers 6.4 Wet combustion method 6.4.1 250 ml double necked pear shaped flask with : 6.4.1.1 6.4.1.2 a water pump coiinected to the other. Ealance with an accuracy of 0,l mg 50 nil dropp
19、ing funnel to one neck and 0619XSP1267T5 AECMA PREN2557 8 LOL23LL 0003488 5-a I prEN ?559 Page 5 O 1 0619XSP1387T5 6.4.3 Heat source with suitable temperature control 6.4.3 400 ml beaker 6.4.4 20 ml sintered glass crucible (11 3 porosity) 6.4.5 Desiccator containing a suitable drying agent (for exam
20、ple silica gel, calcium chloride or phosphorus pentoxide) 6.4.G Concentrated sulfuric acid (specific gravity 1,84) 6.4.7 Hydrogen peroxide solution (30% to 50% w/v) 6.4.8 Acetone (propanone) 6.4.9 Distilled water 6.4.10 Suitable protective clothing, including rubber gloves, for haridling hydrogen pe
21、roxide and sulphuric acid solutions and a safety screen for eye protection. 6.5 Solvent extraction using a Sohxlet 6.5.1 Single thickness extraction thimble, nominal diameter 30 to 31 mm, nominal length 60 to 80 mm. 6.5.2 Electric oven capable of maintaining a tempereture of 105C with an accuracy of
22、 4, 5C 6.5.3 A suitable extraction apparatus of the Sohxlet t:ype, comprising a condenser, siphon tube and flask and provided with an electric heating mantle 6 -5.4 Vacuum desiccator 6.5.5 Methyl ethyl ketone (MEK; butan-?-one) - analytical grade - or other suitable solvent, as agreed between the pu
23、rchaser and the supplier. 6.6 6.6.1 Erlenmeyer flask or beaker 6.6.: Drying cabinet capable of maintaining a temperature of 105OC with an accuacy of 5 5C 6.6.3 Vacuum desiccator 6.6.4 Li suitable solvent for extraction, as agreed between purchaser and supplier 6.6.5 Acetone (propanone). Extraction b
24、y soaking and decantation AECMA PREN2559 88 W LOL23Ll 0003Ll87 7 M prKi 2559 Page 6 7 Starrard atnosphere for co1;ditioning d conditioned i.n the stsndard testint nvicture pick-upp shall be allowed to reach anbieiic temperature over n ptiriod of time accord.ng to the mass of the package. This tine s
25、hall not be less tlian 8 h and the nctual tiiae shall be recorded in thr report. Q k?hei the ma Leril has reached the arnbietit temperature, the aimxir,t required for testhg shall be sampled and conditioned in the standard tesfirig atmosphere (see clause 7.2.1) for a minimum of 2 h, unless otherwise
26、 specFLred. 7.2.1 Standard atnosphere for testing The CWKS shall be carried out at (23 5 2) “C end (50 t. 5) X relatcve humidity. The staiidord atmosphere shall be In accordance with EN 2743. 7.2.2 Tint: interval between coridicloning znd testing Aft.er conditioning, the test shall be carried out wi
27、thin G li, unless otliamise specified, the speciuer, being kept iti the standard atmosphere until the test: is carried o11 t 8 Samplliig and rest specimens 8. !. Test specimen The specimen shall be square and have a length of (100 2 1) IXTI x:d a width cf (100 -.a i- 12 nim. Ocher dimensions of the
28、test specimen may be used, subject to grceuieilt between the purchaser and the supplier, biit having i. surface area r; 100 cm2 wch an accuracy of f E. 8.2 Number aiid distribution of test specimens A n;lniinum of 3 test specimens shall be used. These huI.1 be evenlj- distributad and cut: Ii-oui the
29、 sample diagonaliy across the width or length, as shown in figures 1P rd 1B for woven fabrics rtd in figura 2 for unidirectional sheet or tqe. Note ; Specimens ixed from the determination of mass per un.it area (EN 2557) cui be used or the deternfnation of msin content. . 0619XSP078S5 AECMA PREN2559
30、 88 10L23LL 0003490 3 m prEN 2559 Page 7 9 Procedure 9.1 Wet. combustion nethod Weigh each specimen to the nearest mg (m ), drop into a double necked 9.1.1 pear shaped flask and carefully pour 20 nil of concentrated sulfuric acid into the flask. Fit a dropping funnel and air inlet to one neck and a
31、water pump to the other. 1 9.1.7 Pour a suitable amount (e.g. 20 ml of 50% w/v or 40 ml of 30% w/v) of the hydrogen peroxide solution into the dropping funnel (see note below) and heat the flask gently to (160 + - 10) OC until the acid starts to fume. Discontinue heating of the flask and allow the h
32、ydrogen peroxide solution to drip into the acid at a rate of about one drop every 2 s, increasing to one drop per second after 5 min. If, after all the hydrogen peroxide solution has been used, the solution is still brown, add further 5 ml portions at the latter rate and continue heating until the s
33、olution remains clear. 9.1.3 When the neck of the flask is cool enough to handle, ensure the air inlet is open, turn the water pump off, remove the attachments from the flask and cool the flask and contents down to room temperature in running water. 9.1.4 Pour the contents of the flask into 100 ml o
34、f distilled water in a 400 nil beaker, washing any fibres adhering to the flask into the beaker with distilled water. 9.1.5 Filter the contents of the beaker through a sintered glass crucible, previously weighed (m ), washing the beaker and contents of the crucible with distilled water until the was
35、hings are free from acid, followed by 10 ml of acetone. ? 9.1.6 Dry the crucible and contents at 17OoC for at least 45 min, cool in a desiccator for 20 min and weigh (m ) to the nearest mg. Note : Suitable protective clothing including rubber gloves is recommended for handling hydrogen peroxide and
36、sulfuric acid- solutions and the reactions shall be carried out behind a safety screen for eye protection. 3 9.2 Solvent extraction using a Soxhlet 9.2.1 Preparation of extraction thimble Dry the extraction thimble in an oven at (105 2 5) OC for 2 h, cool to room temperature in a desiccator and weig
37、h, to verify that the mass is constant to 1 mg. Otherwise, repeat this blank test until constant mass is achieved. 9.7.2 Weighing of specimen and solvent extraction of resin For each test specimen, carry out the following sequence of operations : 9.3.2.1 Weigh the thimble to the nearest mg (m ), as
38、indicated in clause 9.7.1. Place the test specimen, cut into pieces of convenient size, in the thimble, care being taken that no fragments are lost, and weigh to the nearest mg (m5). Place the thimble and its contents in the siphon tube of the extraction apparatus. Fit the condenser, siphon tube and
39、 flask together and add a suitable quantity of methyl ethyl ketone (MEK) or other suitable solvent, as agreed between purchaser and supplier. 4 0619XSP1287T5 - AECMA PREN2557 AB LOI12311 0003471 5 W prEN 2559 Page 8 O 9.2.3.2 Regulate the heating of the mantle so that the siphoning rate is compatibl
40、e with the total extraction of the resin during 1 h. Carry out the process for 1 h +10 -0 min or for another period as agreed between the. purchaser and the supplier. 9.3.3.3 Remove the thimble and contents, dry in an oven and then cool in a desiccator and weigh to the nearest mg (m ). 9.2.3.4 succe
41、ssive weighings is less than 1 mg. 6 Repeat the procedure specified above until the difference in mass on 3 9.3 Solvent extraction by soaking and decantation 9.3.1 desiccator and weigh to give the mass m 9.3.3 film or films. Clean and dry the empty container for 10 min at 105OC, then cool in a in g
42、to the nearest 1 mg. 7 Place the test specimen in the container after removing the protective O Weigh the test specimen with the container to give its mass m 9.3.3 9.3.4 Wash the test specimen in at least 50 ml of a suitable solvent until all the resin dissolves. A mechanical shaker is useful for a.
43、ccelerating the extraction. in g. 8 9.3.5 Repeat the operation and rinse several times with acetone. Allow to dry. 9.3.6 Place the container in the drying cctbinet at 105C 2nd leave fcr 1 hour. 9.3.7 Allow to cool in a desiccator and weigh the container with the dry residue (fibre or fabric) to give
44、 its mass m in g, Note : Complete extraction of the resin from the preimpregnate is considered as attained as soon as the remaining fibres are soft and silky. 9 10 Calculation and expression of results 10.1 Uncorrected resin content 10.1.1 Wet combustion method The uncorrected resin content for each
45、 test specimen, expressed as a percentage of the original mass, is calculated from the formula : where : (m3 - = 100 . - - 1 “1 m2) R1 RI m is the initial mass of the specimen, in g 1 m2 is the uncorrected resin content expressed as a percentage of the initial mass is the mass of the sintered glzss
46、crucible, in g is the final total mass of the sintered glass crucible and the residue after wet combustion, in g. O m3 0619XSP1387T5 AECMA PREN2559 88 = LOL23LL 0003Y92 7 W- prEN 3553 Page 9 10.1.3 Tb.e resin content for each test specimen, expressed as a percentage of the j.Eitia1 mass, Is calculat
47、ed from the formula : Solvent extractior, using a Soshlet R, = 100 . c where : is the uncorrected resin conteiits expressed 2s a percentage of the Initial mass R? m4 is the initial mass of the thimble, in g m is the initial total mass of the thimble plus the specinen, in g 5 is the final total mass,
48、 after solvent extraction, of the thimble and the residue: in g. “6 10.1.3 Solvent extraction by soaking and decantation The uncorrected resin contenc of each test specimen is calculated from the formula : im!, - m7 7 R3 = 100 .I - where : R3 m is the mass of the container, i.n g 7 m8 m9 is the unco
49、rrected resin content expressed as percentage of the initiul mass is the initial total mass of the test specimen and the container, in g is the uiass of the container and the dry residue after solvent extraction by soaking and decantation, in g. 10.2 Corrected resin content (corrected for voltilea) The corected resln content of the test specimen is calculated from one of the foll.owing three formulae : RY3 = R3 - V where : RV , RV2, RV initial mass. are the corrected resin contents, expressed as percentage of the 3 R , R2, R, a
