1、BRITISH STANDARD AEROSPACE SERIES BS EN 2559:1997 Carbon fibre preimpregnates Determination of the resin and fibre content and the mass of fibre per unit area The European Standard EN2559:1997 has the status of a British Standard ICS49.025.40BSEN2559:1997 This British Standard, having been prepared
2、under the directionof the Engineering SectorBoard, was published underthe authority of the Standards Board and comes intoeffect on 15August1997 BSI09-1999 The following BSI references relate to the work on this standard: Committee reference ACE/64 Draft for comment88/78342 DC ISBN 0 580 26694 X Comm
3、ittees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee ACE/64, Aerospace structural reinforced plastics, upon which the following bodies were represented: British Plastics Federation Ministry of Defence Society of British Aerospace
4、Companies Amendments issued since publication Amd. No. Date CommentsBSEN2559:1997 BSI 09-1999 i Contents Page Committees responsible Inside front cover National foreword ii Foreword 2 1 Scope 3 2 Normative references 3 3 Principle 3 4 Apparatus and reagents 3 5 Specimens 4 6 Procedure 6 7 Expression
5、 of results 8 8 Health and safety requirements 9 9 Designation 9 10 Test report 9 Figure 1 Example of positioning of specimens on woven fibre fabrics sample across the width 5 Figure 2 Example of positioning of specimens on woven carbon fibre fabric sample along an axis inclined at an angle as close
6、 as possible to the weft direction 5 Figure 3 Example of positioning of specimens on carbon fibre undirectional sheet or tape sample 6 List of references Inside back coverBSEN2559:1997 ii BSI 09-1999 National foreword This British Standard has been prepared by Technical Committee ACE/64 and is the E
7、nglish language version of EN2559:1997 Aerospace series Carbon fibre preimpregnates Determination of the resin and fibre content and the mass of fibre per unit area, published by the European Committee for Standardization (CEN). EN2559:1997 was produced as a result of international discussions in wh
8、ich the United Kingdom took an active part. Cross-references The British Standards corresponding to the European Standards referred to in the text are identical in number and title with those given in clause2. A British Standard does not purport to include all the necessary provisions of a contract.
9、 Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, theEN title page, pages2 to10, an insi
10、de back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN2559 March1997 ICS49.025.40 Descriptors: Aircraft
11、industry, preimpregnated product, carbon fibre, determination, resin, fibre, specific area English version Aerospace series Carbon fibre preimpregnates Determination of the resin and fibre content and the mass of fibre per unit area Srie arospatiale Primprgns de fibres de carbone Dtermination des te
12、neurs en rsine et en fibres et de la masse surfacique de la fibre Luft- und Raumfahrt Kohlenstoffaser-Prepregs Bestimmung des Harz- und Fasermasseanteils und der flchenbezogenen Fasermasse This European Standard was approved by CEN on1996-08-04. CEN members are bound to comply with the CEN/CENELEC I
13、nternal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN me
14、mber. The European Standards exist in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN member
15、s are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches
16、Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1997 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN2559:1997EEN2559:1997 BSI 09-1999 2 Foreword This European Standard has been prepared by the European A
17、ssociation of Aerospace Manufacturers (AECMA). After inquiries and votes carried out in accordance with the rules of this Association, this Standard has received the approval of the National Associations and the Official Services of the member countries of AECMA, prior to its presentation to CEN. Th
18、is European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by September1997, and conflicting national standards shall be withdrawn at the latest by September1997. According to the CEN/CENELEC Internal Regulations
19、, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the UnitedKingdom.EN2559:19
20、97 BSI 09-1999 3 1 Scope This standard specifies methods for determining the resin content, fibre content and mass of fibre per unit area of carbon fibre preimpregnates for aerospace use. 2 Normative references This European Standard incorporates by dated or undated reference provisions from other p
21、ublications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or rev
22、ision. For undated references the latest edition of the publication referred to applies. EN2558, Aerospace series Carbon fibre preimpregnates Determination of the volatile content 1) . EN2743, Aerospace series Reinforced plastics Standard procedures for conditioning prior to testing 1) . 3 Principle
23、 3.1 Wet combustion extraction method (code A) Determination of the difference in mass by means of weighing to constant mass before and after extraction of the resin by acid digestion. Use a solution of concentrated sulphuric acid and hydrogen peroxide. 3.2 Soxhlet extraction method (code B) Determi
24、nation of the difference in mass by means of weighing to constant mass before and after extraction of the resin with methyl-ethyl-ketone or other suitable solvent agreed between the user and manufacturer. 3.3 Method of extraction by soaking and decantation (code C) Similar to3.2 but faster. In case
25、of dispute,3.2 shall be applied. 3.4 Information on the use of the methods 3.4.1 Code A method If the preimpregnate contains only carbon fibre and a resin which is completely “combustible”, the resin content is equal to the loss on wet combustion. The carbon fibre used as a reinforcement may be coat
26、ed with a resin size, which is normally removed during wet combustion. The size is therefore included in the resin content. Where undissolved fillers are lost by filtering, they are thus included in the resin content. NOTEThere may be a partial loss of undissolved fillers, one part being counted wit
27、h the resin and the rest being counted with the fibres. 3.4.2 Code B method Size normally removed during Soxhlet extraction is included in the resin content. If the resin contains fillers which do not dissolve in the solvent, the resin content does not include these fillers. 3.4.3 Code C method Size
28、 normally removed during solvent extractions included in the resin content. Where undissolved fillers are lost by decantation, they are thus included in the resin content. NOTEThere may be a partial loss of undissolved fillers, one part being counted with the resin and the rest being counted with th
29、e fibres. 4 Apparatus and reagents 4.1 For all methods: balance with an accuracy of0,1mg; template of standard specimen; ancillary items such as a sharp knife and tweezers. 1) Published as AECMA Prestandard at the date of publication of this standardEN2559:1997 4 BSI 09-1999 4.2 For code A method: E
30、rlenmeyer250ml double necked pear shaped flask with50ml dropping funnel equipped with air inlet and a water pump; heat source with suitable temperature control; 400ml beaker; 20ml sintered glass crucible(n2porosity) and suitable filtration assembly; desiccator containing a suitable drying agent (for
31、 example silica gel, calcium chloride or phosphorus pentoxide); electric oven capable of maintaining a temperature of120 C with an accuracy of5 C; protective clothing and rubber gloves resistant to hydrogen peroxide and sulphuric acid solutions, safety screen for eye protection; concentrated sulphur
32、ic acid (specific gravity:1,84 to1,89); hydrogen peroxide solution (concentration:300g/l to500g/l); acetone (propanone); distilled water. 4.3 For code B method: single thickness extraction thimble, nominal diameter20mm to22mm, nominal length60mm to80mm; electric oven capable of maintaining a tempera
33、ture of105 C with an accuracy of5 C; an extraction apparatus of the Soxhlet type, comprising a condenser, siphon tube and flask and provided with an electric heating mantle; vacuum desiccator; Methyl-ethyl-ketone (MEK : butanone2) analytical grade or other suitable solvent agreed between the user an
34、d manufacturer. 4.4 For code C method container400ml (Erlenmeyer flask or beaker); electric oven capable of maintaining a temperature of105 C with an accuracy of5 C; vacuum desiccator; a suitable solvent for extraction, as agreed between the user and manufacturer; acetone (propanone). 5 Specimens 5.
35、1 Shape and dimensions The specimen shall be square and have sides of(100 1)mm. Other specimens may be used, subject to agreement between the user and manufacturer on condition that they have an area of100cm 2with a tolerance of 2%. 5.2 Number and distribution A minimum of three specimens shall be u
36、sed. They shall: be evenly distributed across the width of the sample; have their centres positioned along a straight line. See Figure 1 for wide woven fabrics, Figure 2 for narrow woven fabrics and Figure 3 for unidirectional sheet or tape. EN2559:1997 BSI 09-1999 5 Figure 1 Example of positioning
37、of specimens on woven carbon fibre fabrics sample acrossthe width Figure 2 Example of positioning of specimens on woven carbon fibre fabric sample alonganaxis inclined at an angle as close as possible to the weft directionEN2559:1997 6 BSI 09-1999 6 Procedure 6.1 Conditioning 6.1.1 Preimpregnates st
38、ored at ambient temperature The amount of preimpregnate required for testing shall be sampled and then conditioned in the test atmosphere (see6.2) for a minimum of2h, unless otherwise specified. 6.1.2 Preimpregnates stored below ambient temperature The preimpregnate, suitably packed in an airtight a
39、nd solvent resistant bag to prevent moisture pick-up, shall be allowed to reach ambient temperature over a period of time depending on its mass. This time shall not be less than8h. When the material has reached ambient temperature, the amount required for testing shall be sampled and then conditione
40、d in the test atmosphere (see6.2) for a minimum of2h, unless otherwise specified. 6.2 Atmosphere for testing EN2743, condition class B. 6.3 Time interval between conditioning and testing After conditioning, the sample shall be maintained in the test atmosphere. Unless otherwise specified, tests shal
41、l be carried out within6h. 6.4 Tests Cut the specimens 6.4.1 Code A method Use protective clothing and rubber gloves for handling hydrogen peroxide and sulphuric acid solutions. The reactions shall be carried out behind the safety screen for eye protection. 6.4.1.1 Remove the protective films and we
42、igh the specimen to the nearest milligram (m 1 ), place it into the Erlenmeyer and carefully pour20ml of concentrated sulphuric acid into the flask. Fit the funnel to one neck and the water pump to the other. Figure 3 Example of positioning of specimens on carbon fibre unidirectional sheet ortapesam
43、pleEN2559:1997 BSI 09-1999 7 6.4.1.2 Pour a suitable amount (e.g.20ml of hydrogen peroxide at500g/l or40ml of hydrogen peroxide at300g/l) of the hydrogen peroxide solution into the dropping funnel and heat the flask gently to(160 10) C until the acid starts to fume. Discontinue heating of the flask
44、and allow the hydrogen peroxide solution to drip into the acid at the rate of about one drop every2s, increasing to one drop per second after5min. If, after all the hydrogen peroxide solution has been used, the solution is still brown, add further5ml portions of hydrogen peroxide solution at the lat
45、ter rate and heat until the solution becomes clear. 6.4.1.3 Stop heating. When the neck of the Erlenmeyer is cool enough to handle, ensure the air inlet is open, turn the water pump off, remove the attachments from the Erlenmeyer and cool the Erlenmeyer and contents down to ambient temperature in ru
46、nning water. 6.4.1.4 Pour the contents of the Erlenmeyer into a400ml beaker containing100ml of distilled water, wash with distilled water any fibres adhering to the Erlenmeyer into this beaker. 6.4.1.5 Filter the contents of the beaker through the sintered glass crucible, previously weighed (m 2 ),
47、washing the beaker and contents of the crucible with distilled water until the washings are free from acid, followed by10ml of acetone. 6.4.1.6 Dry the crucible and contents at120 C for at least45min, cool in a desiccator for20min and weigh(m 3 ) to the nearest milligram. 6.4.2 Code B method 6.4.2.1
48、 Dry the extraction thimble in the oven at(105 5) C, for2h, cool to room temperature in the desiccator and weigh. Repeat this blank test until the mass is constant to1mg (m 4 ). This operation need only be carried out once as long as each subsequent test leaves the thimble dry and clean. 6.4.2.2 Rem
49、ove the protective films. Cut the specimen into pieces and place them into the thimble, care being taken that no fragments are lost. Weigh to the nearest milligram (m 5 ). 6.4.2.3 Place the thimble in the siphon tube of the extraction apparatus. Fit the condenser, siphon tube and flask together and add a suitable quantity of solvent (see4.3). 6.4.2.4 Regulate the heating so that the siphoning rate is compatible with the total extraction of the resin d
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