ISO-10548-2002.pdf

INTERNATIONAL STANDARD ISO 10548 Second edition 2002-07-15 Reference number ISO 10548:2002(E) © ISO 2002 Carbon fibre Determination of size content Fibres de carbone Détermination du taux d'ensimage ISO 10548:2002(E) ii© ISO 2002 All rights reserved PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. 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ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland ISO 10548:2002(E) © ISO 2002 All rights reserved iii Contents Page 1Scope . 1 2Normative reference . 1 3Terms and definitions 1 4Principle 1 5Test specimens . 2 6Conditioning 2 7Test methods 2 7.1Method A: Solvent extraction . 2 7.2Method B: Digestion with sulfuric acid and hydrogen peroxide . 4 7.3Method C: Decomposition by pyrolysis 7 8Precision . 8 9Test report 8 ISO 10548:2002(E) iv© ISO 2002 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 10548 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 13, Composites and reinforcement fibres. This second edition cancels and replaces the first edition (ISO 10548:1994), which has been technically revised. -,-,- INTERNATIONAL STANDARDISO 10548:2002(E) © ISO 2002 All rights reserved 1 Carbon fibre Determination of size content 1Scope This International Standard specifies test methods for the determination of the size content of carbon fibre yarn. It is applicable to continuous-filament yarns and staple-fibre yarns. 2Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, this publication do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent edition of the normative document indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 1886:1990, Reinforcement fibres Sampling plans applicable to received batches 3Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 3.1 size any material applied to fibres to facilitate the handling and use of the fibres 3.2 size content mass of the size expressed as a percentage of the sized carbon fibre yarn 4Principle Test specimens are weighed before and after removal of the size by one of the following three methods: method A: size removal by Soxhlet extraction, to be used when the size is completely soluble in a suitable solvent; method B: size removal by chemical digestion using a mixture of sulfuric acid and hydrogen peroxide, used when the size is partially hardened and not completely soluble in solvents; method C: size decomposition by pyrolysis at high temperature in an atmosphere of nitrogen, used when the size is completely removed by pyrolysis. Methods A and B require the last weighing to be made to constant mass by repetition of the final drying and weighing procedure. In those cases where known materials are being tested regularly, it is permitted to define, by experiment, a minimum time for drying which will ensure that constant mass has been reached. Particular care may be required if the carbon fibre or sizing is water-absorbent. -,-,- ISO 10548:2002(E) 2© ISO 2002 All rights reserved 5Test specimens Two test specimens or more shall be taken from each lot or yarn sample. The size content is taken as the average of the two or more determinations. If the determination is carried out for the purpose of lot acceptance, the lot received shall be sampled in accordance with ISO 1886. When handling test specimens, gloves shall be worn or tweezers used to avoid damage to the specimens. NOTEThe specification or the person requiring the test may stipulate that additional determinations be carried out at different places within the elementary unit. 6Conditioning Elementary units and yarn samples shall be allowed to attain laboratory temperature before testing. Before weighing the yarn, it shall be dried if required. 7Test methods 7.1Method A: Solvent extraction 7.1.1Apparatus and materials 7.1.1.1Balance, accurate to , readable to . 7.1.1.2Hot-air oven, capable of being controlled to . 7.1.1.3Desiccator, containing a suitable desiccant, for example silica gel, anhydrous calcium chloride or phosphorous pentoxide. 7.1.1.4Soxhlet extractor, capacity, with a flask. 7.1.1.5Soxhlet extraction thimbles, measuring . NOTEThe sizes of the Soxhlet extractor, the flask and the Soxhlet extraction thimbles are given as an indication only and may be varied to suit individual requirements. IMPORTANT The extraction and all handling of organic solvents should be carried out in a fume cupboard. 7.1.1.6Rubber gloves or tweezers. 7.1.1.7Cutting blade. 7.1.1.8Heating mantle, fitted with a power regulator capable of controlling the boiling rate of the solvent. 7.1.1.9Distilled water, or an organic solvent such as butan-2-one (methyl ethyl ketone), tetrahydrofuran, dichloromethane (methylene chloride), acetone or dichloroethane. NOTEThe choice of solvent depends upon the type of size applied to the carbon fibre under test. This choice is best made by consultation between the customer and the supplier. 0,5 mg0,1 mg ±5 C 200 ml500 ml 41 mm×123 mm ISO 10548:2002(E) © ISO 2002 All rights reserved 3 7.1.2Procedure 1 7.1.2.1Dry an extraction thimble (7.1.1.5) at in the oven (7.1.1.2) for and allow to cool to room temperature in a desiccator (7.1.1.3). 7.1.2.2Weigh the thimble to the nearest (). 7.1.2.3Place a test specimen in the thimble and weigh to the nearest (). 7.1.2.4Place the thimble and its contents in the siphon chamber of the Soxhlet apparatus (7.1.1.4), and place a sufficient volume of solvent in the flask to ensure operation of the siphon during the reflux cycles. 7.1.2.5Extract for , adjusting the heating mantle (7.1.1.8) so that at least four reflux cycles occur during the extraction period (a shorter extraction period may, however, be used if it can be demonstrated to give complete extraction). 7.1.2.6Turn off the heating mantle. Wait for the apparatus to cool. Remove the thimble and contents. Allow to stand at ambient temperature for to allow excess solvent to evaporate. 7.1.2.7Dry the thimble and contents for in the oven (7.1.1.2) at (or, if the solvent used has a boiling point higher than , at a temperature above the boiling point of the solvent) and allow to cool in a desiccator. Weigh to the nearest . 7.1.2.8Repeat the drying and weighing procedure until the difference in mass between two successive weighings () is less than . If a minimum drying time known to give constant mass has been established (see clause 4), this requirement does not apply. 7.1.3Procedure 2 7.1.3.1If the specimen is free of loose fibre and can be coiled into a form which can be inserted into the Soxhlet extraction chamber without the danger of loss of fibre during extraction, an extraction thimble need not be used. 7.1.3.2Weigh the test specimen to the nearest (). 7.1.3.3Carry out the extraction as described in Procedure 1, but without the extraction thimble. 7.1.3.4Dry the specimen for at or a higher temperature (see 7.1.2.7) and allow to cool in a desiccator. Weigh to the nearest . 7.1.3.5Repeat the drying and weighing procedure until the difference in mass between two successive weighings () is less than . If a minimum drying time known to give constant mass has been established (see clause 4), this requirement does not apply. 7.1.4Expression of results 7.1.4.1Procedure 1 Calculate the size content SC, expressed as a percentage by mass, from the equation: 105 C ±5 C 1 h 0,1 mgm1 0,1 mgm2 2 h2 h 10 min 10 min 1 h110 C ±5 C 100 C 10 C 0,1 mg m3±0,2 mg 0,1 mgm4 1 h110 C ±5 C 0,1 mg m5±0,2 mg SC= m2 m3 m2 m1 ×100 ISO 10548:2002(E) 4© ISO 2002 All rights reserved where is the initial mass, in grams, of the extraction thimble; is the initial mass, in grams, of the thimble plus test specimen; is the final mass, in grams, of the thimble plus test specimen after extraction. 7.1.4.2Procedure 2 Calculate the size content SC, expressed as a percentage by mass, from the equation: where is the initial mass, in grams, of the specimen; is the final mass, in grams, of the specimen after extraction. 7.2Method B: Digestion with sulfuric acid and hydrogen peroxide 7.2.1Apparatus and reagents 7.2.1.1Balance, accurate to , readable to . 7.2.1.2Hot-air oven, capable of being controlled to . 7.2.1.3Desiccator, containing a suitable desiccant, for example silica gel, anhydrous calcium chloride or phosphorus pentoxide. 7.2.1.4Fume cupboard. 7.2.1.5Rubber gloves, face shield and laboratory coat. 7.2.1.6Sintered-glass filters, porosity P 40, pore diameter to , capacity to . 7.2.1.7Cutting blade. 7.2.1.8Dry-block heater (see Figure 1), fitted with an exhaust hood connected to a scrubbing system and suction pump, and also fitted with a fixed support rack designed to hold digestion tubes and graduated dropping funnels for the addition of reagents. The heating block shall be placed on a secure laboratory jack or similar item of equipment. 7.2.1.9Concentrated sulfuric acid, at least (by mass) (). 7.2.1.10Hydrogen peroxide solution, containing at least (by mass) H2O2. The volumes given in the procedure are for (by mass). 7.2.1.11Sodium hydroxide solution, containing approximately (by mass) NaOH, for use in neutralizing acid fumes extracted by the exhaust hood. m1 m2 m3 SC= m4 m5 m4 ×100 m4 m5 0,5 mg0,1 mg ±0,5 C 20µm30µm30 ml70 ml 96 % =1,84 g/ml 30 % 30 % 15 % ISO 10548:2002(E) © ISO 2002 All rights reserved 5 Key 1Exhaust hood 2Extraction line for acid fumes 3Support rack 4To suction pump 5Sodium hydroxide solution 6Dropping funnel 7Hydrogen peroxide 8Digestion tube 9Test specimen in concentrated sulfuric acid 10Heating block Figure 1 Apparatus for method B: Chemical digestion -,-,- ISO 10548:2002(E) 6© ISO 2002 All rights reserved 7.2.2Procedure IMPORTANT This procedure must be carried out in a fume cupboard. During the oxidation operation, the fume cupboard door must be lowered. Face visor, gloves and laboratory coat must be worn. 7.2.2.1Pre-heat the heating block (7.2.1.8) to for before use. 7.2.2.2Fill each of the dropping funnels with approximately of hydrogen peroxide solution (7.2.1.10). 7.2.2.3Weigh a test specimen of carbon fibre yarn to the nearest () and place it in a digestion tube. Add at least of concentrated sulfuric acid (7.2.1.9). Swirl to ensure that the test specimen is immersed in the acid. Place the tube in the support rack. Repeat the procedure for other specimens if more than one determination is being carried out. 7.2.2.4Place the exhaust hood (see 7.2.1.8) over the digestion tubes in the rack. 7.2.2.5Start the suction pump (see Figure 1). 7.2.2.6Slowly open the dropping funnels containing the hydrogen peroxide solution and allow about of this solution to run into each digestion tube. The reaction mixture will fume as the reaction starts. 7.2.2.7Use the laboratory jack to raise the heating block round the digestion tubes. 7.2.2.8Allow the digestion tubes to remain in the heating block at for . 7.2.2.9Lower the heating block away from the digestion tubes. If a solution is not clear, allow to cool for , add a further of hydrogen peroxide solution and repeat the procedure from 7.2.2.7. If the solution is still not clear, repeat the digestion procedure on a fresh test specimen. 7.2.2.10Allow the digested specimens to cool to room temperature. 7.2.2.11Heat sintered-glass filters (7.2.1.6) (one for each digested specimen) in the oven (7.2.1.2) at for , allow to cool in a desiccator (7.2.1.3) and weigh to the nearest (). 7.2.2.12Filter each solution slowly through a sintered-glass filter and wash each specimen with distilled water until the washings are neutral to indicator paper. 7.2.2.13Dry the sintered-glass filters and specimens for in the oven at and allow to cool in a dessicator. Weigh to the nearest . 7.2.2.14Repeat the drying and weighing procedure until the difference in mass between two successive weighings () is less than . If a minimum drying time known to give constant mass has been established (see clause 4), this requirement does not apply. 7.2.2.15A correction factor will be required if the digestion causes a significan