1、BRITISH STANDARD AEROSPACE SERIES Carbon fibre preimpregnates - Determination of the resin and fibre content and the mass of fibre per unit area The European Sandard EN 2559 : 1997 has the status of a British Standard BS EN 2659 : 1997 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIG
2、HT LAW - STD-BSI BS EN 2557-ENGL 1777 = lb24bb Ob31028 Lb W BS EN 2669 : 1997 Committees responsible for this British Standard The prepamtion of this British Standard was entrusted to Technical Committee ACW64, Aerospace structural reinforced plastics, upon which the following bodies were represente
3、d: British Plastics Federation iibu.sQ of Defence Society of British Aerospace Companies This British Standard, having been prepared under the direction of the Engineering Sector Board, was published under the authority of the Standards Board and comes into effect on 15 August 1997 O BSI 1997 Amendm
4、ents issued since publication ID* ITextaffected Amd No. The following BSI references relate to the work on this standard Committee reference ACH64 Draft for comment 88/78342 DC ISBN O 680 26694 X * m * STD-BSI BS EN 2559-ENGL 1797 1624bb9 Ob31027 O22 BS EN 2669 : 1997 Contents Committees responsible
5、 pae Inside front cover National foreword ii Foreword 2 Specification 1 Scope 2 Normativereferences 3 Principle 4 Apparatusandreagents 6 Specimens 6 Procedure 7 Expressionofresults 3 3 3 4 5 8 10 8 Health and safety requirements 11 9 Designation 11 10 Testreport 12 Figures 1 2 Example of positioning
6、 of specimens on woven fibre fabrics sample across the width Example of positioning of specimens on woven carbon fibre fabric sample along an axis inclined at an angle as close as possible to the weft direction Example of positioning of specimens on carbon fibre unirectional sheet or tape sample 6 3
7、 O BSI 1997 1 STD-BSI BS EN 2559-ENGL 1997 W LbZi(bb9 Ob31030 - template of standard specimen ; - ancillary items such as a sharp knife and tweezers. 4.2 For code A method : - Erlenmeyer 250 ml double necked pear shaped flask with 50 ml dropping funnel equipped with air inlet and a water pump ; - he
8、at source with suitable temperature control ; - 400 ml beaker ; - 20 ml sintered glass crucible (n02 porosity) and suitable filtration assembly ; - desiccator containing a suitable drying agent (for example silica gel, calcium chloride or phosphorus pentoxide) ; - electric oven capable of maintainin
9、g a temperature of 120 OC with an accuracy of 5 OC ; - protective clothing and rubber gloves resistant to hydrogen peroxide and sulphuric acid solutions, safety screen for eye protection ; - concentrated sulphuric acid (specific gravity : 1,84 to 1,89) ; - hydrogen peroxide solution (concentration :
10、 300 g/l to 500 g/l) ; - acetone (propanone) ; - distilled water. * * m STD.BSI BS EN 2557-ENGL L777 Lb2Libb7 Ob3E035 32b W Page 5 EN 2559:1997 4.3 For code B method : - single thickness extraction thimble, nominal diameter 20 mm to 22 mm, nominal length 60 mm to 80 mm ; - electric oven capable of m
11、aintaining a temperature of 105 OC with an accuracy of 5 OC ; - 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 : butanone 2) - analytical grade - or other suita
12、ble solvent agreed between the user and manufacturer. 4.4 For code C method - container 400 ml (Erlenmeyer flask or beaker) ; - electric oven capable of maintaining a temperature of 105 OC with an accuracy of 5 OC ; - vacuum desiccator ; - a suitable solvent for extraction, as agreed between the use
13、r and manufacturer ; - acetone (propanone). 5 Specimens 5.1 Shape and dimensions The specimen shall be square and have sides of (1 O0 ? 1) mm. Other specimens may be used, subject to agreement between the user and manufacturer on condition that they have an area of 100 cm2 with a tolerance of f 2 %.
14、 5.2 Number and distribution A minimum of three specimens shall be used. 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
15、 sheet or tape. STD-BSI BS EN 2557-ENGL 1997 1b24bb7 Ob3103b 2b2 Page 6 EN 2559:1997 Dimensions in millimetres Figure 1 Example of positioning of specimens on woven carbon fibre fabrics sample across the width Dimensions in millimetres I Weft vorn I it I I Figure 2 Example of positioning of specimen
16、s on woven carbon fibre fabric sample along an axis inclined at an angle as close as possible to the weft direction - STD-BSI BS EN 2557-ENGL 1777 H 1b24bb7 Ob31037 IT7 I Width of sheet or tape Page 7 EN 2559:1997 Figure 3 Example of positioning of specimens on carbon fibre unidirectional sheet or t
17、ape sample STD-BSI BS EN 2557-ENGL 1777 = 1bZqbb7 Ob31038 035 Page 8 EN 2559:1997 6 Procedure 6.1 Conditioning 6.1.1 The amount of preimpregnate required for testing shall be sampled and then conditioned in the test atmosphere (see 6.2) for a minimum of 2 h, unless otherwise specified. Preimpregnate
18、s stored at ambient temperature 6.1.2 The preimpregnate, suitably packed in an airtight and solvent resistant bac to prevent moisture pick- up, shall be allowed to reach ambient temperature over a per d of time depending on its mass. This tuane shaii not be esc inan n. Preimpregnates stored below am
19、bient temperature. When the material has reached ambient temperature, the amount required for testing shall be sampled and then conditioned in the test atmosphere (see 6.2) for a minimum of 2 h, unless otherwise specif ied. 6.i Atmosphere for testing EN 2743. condition class B. 6.3 After conditionin
20、g, the sample shall be maintained in the test atmosphere. Unless otherwise specified, tests heil: be 23:;kd su: within 6 h. Time interval between conditioning and testing 6.4 Tests Cut the specimens 6.4.1 Code A method Use protective clothing and rubber gloves for handling hydrogen peroxide and sulp
21、huric acid solutions. The reactions shall be carried out behind the safety screen for eye protection. 6.4.1.1 Remove the protective films and weigh the specimen to the nearest milligram (m,), place it into the Erlenmeyer and carefully pour 20 ml of concentrated sulphuric acid into the flask. Fit the
22、 funnel to one neck and the water pump to the other. 6.4.1.2 Pour a suitable amount 4e.g. 20 ml of hydrogen peroxide at 500 g/l or 40 ml of hydrogen peroxide at 300 9/11 of the hydrogen peroxide solution into the dropping funnel and heat the flask gently to (160 f 10) OC until the acid starts to fum
23、e. Discontinue heating of the flask and allow the hydrogen peroxide solution to drip into the acid at the 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 portion
24、s of hydrogen peroxide solution at the latter 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
25、contents down to ambient temperature in running water. 6.4.1.4 Pour the contents of the Erlenmeyer into a 400 ml beaker containing 100 ml of distilled water, wash with distilled water any fibres adhering to the Erlenmeyer into this beaker. * * rn Page 9 EN 2559:1997 6.4.1.5 Filter the contents of th
26、e beaker through the sintered glass crucible, previously weighed (m2), washing the beaker and contents of the crucible with distilled water until the washings are free from acid, followed by 10 ml of acetone. 6.4.1.6 Dry the crucible and contents at 120 OC for at least 45 min, cool in a desiccator f
27、or 20 min and weigh (m3) to the nearest milligram. 6.4.2 Code B method 6.4.2.1 Dry the extraction thimble in the oven at (105 15) OC, for 2 h, cool to room temperature in the desiccator and weigh. Repeat this blank test until the mass is constant to 1 mg (m41. This operation need only be carried out
28、 once as long as each subsequent test leaves the thimble dry and clean. 6.4.2.2 Remove 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 (m5). 6.4.2.3 Place the thimble in the siphon tube of
29、 the extraction apparatus. Fit the condenser, siphon tube and flask together and add a suitable quantity of solvent (see 4.3). 6.4.2.4 Regulate the heatir 3 so that the siphoning rate is compatible with the total extraction of the resin during 1 h. Carry out the test for 1 h + 0 min or for another p
30、eriod as agreed between the user and manufacturer. 6.4.2.5 Remove the thimble, dry in the oven and then cool in the vacuum desiccator and weigh to the nearest milligram (me). 6.4.2.6 Repeat 6.4.2.3 to 6.4.2.5 until the difference in mass on two successive weighings is less than 1 mg. 6.4.2.7 Clean a
31、nd dry the thimble. 6.4.3 Code C method 6.4.3.1 Take a clean container. Dry it for 10 min at 105 OC. Cool in a desiccator and weigh to the nearest milligram (rn7). 6.4.3.2 Remove the protective films. Place the specimen in the container. Weigh it to the nearest milligram (m8). 6.4.3.3 Wash the speci
32、men in at least 50 ml of suitable solvent until all the resin dissolves. A mechanical shaker may be used for accelerating the extraction. Carefully decant the solution from the container ensuring that no fibres are allowed to escape. 6.4.3.4 Repeat the operation and rinse several times with acetone.
33、 Allow to dry. 6.4.3.5 Place the container with the specimen in the drying oven at 105 OC and leave for 1 h. 6.4.3.6 Allow to cool in the desiccator and weigh the container with the dry residue (fibre or woven fabric) to the nearest milligram (mg). NOTE : Complete extraction of the resin from the pr
34、eimpregnate is considered to be achieved as soon as the remaining fibres are soft and silky. - - STD-BSI BS EN 2559-ENGL 1777 1b24bb7 Ob31040 793 Page 10 EN 2!559:1997 7 Expression of results 7.1 Uncorrected resin content 7.1.1 Code A method where : RA m, m2 m3 is the uncorrected resin content expre
35、ssed as a percentage of the initial mass ; is the mass of the specimen, in grams ; is the masa u? the sintered glass crucible, in grams ; is the mass of the sintered glass crucible and tl.2 residue after wet combustion, in grams. 7.1.2 Code B method where : , m4 m5 m6 is the uncorrected resin conten
36、t expressed as a percentage of the initial mass ; is the mass of the thimble, in grams ; is the mass of the thimble plus the specimen, in grams ; is the mass, after solvent extraction, of the thimble and the residue, in grams. where : c rn7 rns mg is the uncorrected resin content expressed as percen
37、tage of the initial mass ; is the mass of the container, in grams ; is the mass of the specimen and the container, in grams ; is the mass of the container and the dry residue after solven: extraction, in grams. 7.2 Corrected resin content (corrected for volatiles) #?VA = RA - v RVB = RB - V Vc = Rc
38、- V where : VA, RVB, Vc are the corrected resin contents, expressed as a percentage of the initial mass , RA, R, RC are the uncorrected resin contents, determined in accordance with 7.1 ; V is the volatile content determined in accordance with EN 2558. STD-BSI BS EN 2559-ENGL 1997 D Lb2LibbS Ob3LOLi
39、L b2T D Page 11 EN 2559:1997 7.3 Fibre content MFc =,( mg -m7) ma -mi where : MFA, MF, MFc are the fibre contents, expressed as a percentage of the initial mass (methods coded A, B, Cl. 7.4 Mass of fibre per unit area m3 - m2 S MSFA = where : MsFA, MsFB, MsFc are the mass of fibre per unit area, in
40、grams per square meter (methods coded A, B, Cl ; S is the area of the specimen, in square metres. 8 Health and safety requirements It is the responsibility of the user of this standard to adopt appropriate health and safety precautions. 9 Designation EXAMPLE : Number of this standard Test method (co
41、da see 3) STD.BSI BS EN 2557-ENGL 1777 m 1b24bb9 Ob31042 5bb m Page 12 EN 2559:1997 10 Test report It shall include the following : - designation (see 9) ; - all data ensuring the traceability of the material (trade mark, identification marking, date of receipt, etc.) ; - all information regarding t
42、he sampling procedure ; - form and dimensions of specimens ; - perid of conditioning ; - test atmosphere, for example temperature, relative humidity if these differ from 6.2 ; - time interval between conditioning and testing (see 6.3) ; - solvent used (methods coded B or Cl ; - volume of the Soxhlet
43、 apparatus and the siphoning rate (method coded B) ; - the uncorrected and corrected resin contents, fibre content and mass of fibre per unit area ; - individual values and arithmetic mean ; - any incident which may have affected the results. STD.BS1 BS EN 2559-ENGL 1997 Lb24bb9 Ob31Oq3 4T2 II BS EN
44、 2569 : 1997 List of references See national foreword O BSI 1997 STD-BSI BS EN 2557-ENGL 1797 m lb24bb7 b31044 337 m BS EN 2559 : 1997 BSI 389ChiswickHighRoad London w4 4AL BSI - British Standards Institution BSI is the independent national body responsible for preparing British standards. It presen
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