1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Determination of fibre lengthICS 83.120Plastics Glass-fibre-reinforced products BRITISH STANDARDBS
2、ISO 22314:2006BS ISO 22314:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 May 2006 BSI 2006ISBN 0 580 48390 8Cross-referencesThe British Standards which implement international publications referred to in this document may be found in
3、 the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsibl
4、e for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations.Summary of pagesThis document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 4, an inside back cover and a back cover.The BSI co
5、pyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsA list of organizations represented on this committee can be obtained on request to its secretary. present to the responsible international/European committe
6、e any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK.National forewordThis British Standard reproduces verbatim ISO 22314:2006 and implements it as the UK national standar
7、d.The UK participation in its preparation was entrusted to Technical Committee PRI/42, Fibre reinforced thermosetting plastics and prepregs, which has the responsibility to: aid enquirers to understand the text;Reference numberISO 22314:2006(E)INTERNATIONAL STANDARD ISO22314First edition2006-05-01Pl
8、astics Glass-fibre-reinforced products Determination of fibre lengthBS ISO 22314:2006ii iiiForeword 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 o
9、ut 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 c
10、ollaborates 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 2. The main task of technical committees is to prepare International
11、 Standards. 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 elemen
12、ts of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 22314 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 13, Composites and reinforcement fibres. BS ISO 22314:2006iv Introduction There
13、 is global interest in the determination of the length of glass fibres in all types of composite, to predict their characteristics (essentially mechanical ones). For these determinations, three steps are necessary: separation of the fibres from the composite; dispersion of the fibres to obtain indiv
14、idual fibres; measurement of their length. After considering all the existing methods for separating the fibres from the resin, it was decided to develop the proposed method only for short glass fibres from thermoplastic resins, extracted by calcination. The principles of the method are probably sui
15、table for other composites, but it would need more development to obtain a method suitable for other conditions (thermoset resins, long fibres in thermoplastic or thermoset resins, carbon fibres). BS ISO 22314:20061Plastics Glass-fibre-reinforced products Determination of fibre length 1 Scope This I
16、nternational Standard specifies a method of determining the length of the fibres present in a fibre-reinforced product. The method is applicable to moulding materials and to moulded parts. The test conditions specified limit the application of this method to thermoplastics reinforced with short glas
17、s fibres (less than 1 mm long), i.e. fibres whose length is less than or equal to 7,5 mm prior to incorporation in the moulding material and moulding. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edit
18、ion cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 472, Plastics Vocabulary ISO 1172, Textile-glass-reinforced plastics Prepregs, moulding compounds and laminates Determination of the textile-glass and mineral-filler conte
19、nt Calcination methods 3 Terms and definitions For the purpose of this document, the terms and definitions given in ISO 472 apply. 4 Principle The fibres are separated from the reinforced polymer and their length measured from a magnified image on a screen. 5 Apparatus 5.1 Muffle furnace, capable of
20、 maintaining a temperature of 625 C 25 C. 5.2 Crystallizing dish, diameter 80 mm to 110 mm. 5.3 Ultrasonic device. NOTE A basic ultrasonic device, like those used in laboratories for cleaning purposes, has been found suitable. 5.4 Microscope or stereoscope (with fixed or variable magnification facto
21、rs), equipped with a video camera, giving at least 50 magnification. 5.5 Image acquisition device, that enables the image to be displayed on a TV monitor. BS ISO 22314:20062 5.6 Reference micrometer, to calibrate the images at the selected magnification. 5.7 Data-processing equipment, with suitable
22、image analysis software. 5.8 Drying oven, capable of maintaining a temperature of 130 C 5 C. 5.9 Laboratory and observation accessories (crucibles, evaporation dishes, spatulas, glass microscope slides). 6 Procedure 6.1 Preparation of the test specimen From the sample to be examined, take the quanti
23、ty of material necessary to obtain a concentration of fibres such that each image displayed on the screen contains a hundred or so fibres. This quantity will depend on the fibre content of the material and on the test conditions, in particular on the diameter of the crystallizing dish (the water dep
24、th in the crystallizing dish does not have any influence on the concentration of the fibres deposited on the glass slide, as the fibres precipitate in a horizontal plane). EXAMPLE For a 30 % glass-fibre-reinforced polyamide, around 0,006 g of material are required when a 90 mm diameter crystallizing
25、 dish is used. NOTE This assumes that the fibre length is less than 1 mm. Calcine the material at 625 C in accordance with ISO 1172 for 1 h 30 min and allow to cool. NOTE The ash obtained is mainly made up of glass fibres and possibly also mineral fillers. The fibres are very fragile and all subsequ
26、ent handling must be conducted with extreme caution in order not to break them and therefore invalidate the results. Place a previously degreased glass microscope slide in a crystallizing dish (5.2) and pour in a quantity of demineralized water (containing a small amount of surfactant) just sufficie
27、nt to cover the slide. The quantity of water is limited in order to avoid the formation of convection currents during subsequent evaporation, which lead to a selection of the fibres on the basis of their mass and therefore of their size. Pour the ash into the crystallizing dish prepared as described
28、 above (or transfer a sufficient quantity on the tip of a spatula). Place the crystallizing dish containing the ash in the ultrasonic device in order to disperse the fibres without any mechanical action. The time required for this dispersion is in the region of a few seconds to 1 min. Then place the
29、 crystallizing dish in an oven (5.8) preheated to 130 C and leave it there for approximately 1 h, in order to eliminate the water. Allow to cool down. This procedure may be omitted if heating tends to cause the fibres to stick together. Place the crystallizing dish beside the microscope or stereosco
30、pe (5.4). Take the slide covered with fibres and place it under the microscope or stereoscope lens. If necessary, wipe off any fibres present on the underside of the slide. 6.2 Calibration Calibrate the system using a reference gauge; a 1 mm or 1,5 mm length micrometric glass slide has been found su
31、itable. Calibration can be carried out by measuring the length of the reference gauge, pointing to the two ends as would be done when measuring the lengths the fibres, and comparing the reading with the gauge length. The recommended tolerance is 0,01 mm. BS ISO 22314:20063Calibrate the microscope as
32、 frequently as necessary. 6.3 Examination and measurements The fibres are examined directly, without microscope cover glass or mounting fluid, in reflected or transmitted light, in the light-field or dark-field (annular illumination) mode. Adjust the overall magnification chain (optics and projectio
33、n) in order to obtain on the screen an image magnified between 50 and 100 times. The magnification shall be such that the whole lengths of 100 20 fibres appear on the screen. Measure manually the lengths of all the complete fibres appearing on the screen by clicking with the mouse on the ends of eac
34、h fibre. Measure 100 20 fibres in this way from each of three images, for a total of 300 60 fibres. NOTE 1 This manual measurement method can be replaced by a semi-automatic method. However, it must be realized that such methods are biased towards the smaller fibres and that the results obtained wil
35、l therefore be systematically lower than those obtained by manual measurement. NOTE 2 While outside the scope of this method, if longer fibres up to 5 mm in length are measured, the magnification can be reduced to as little as 15, provided the quality of the optical system is good enough to permit s
36、atisfactory measurement. 6.4 Expression of results The results to be reported are: Ln, the mean fibre length, expressed in micrometres, calculated from the following equation: 1niniiLLn=where Liis the length of the ith fibre, n is the number of fibres measured; , the standard deviation of the indivi
37、dual values; a histogram plotted for individual ranges over the entire measurement range (e.g. 50 ranges of 40 m each over a measurement range extending from 0 m to 2 000 m); Lp, a weighted mean length, expressed in micrometres, calculated from the following equation: 2piiiiiinLLnL=where niis the nu
38、mber of fibres of length Li; the ratio Lp/Ln. BS ISO 22314:20064 7 Test report The test report shall contain the following information: a) a reference to this International Standard, i.e. ISO 22314:2006; b) all details necessary for identification of the sample; c) the quantity of material sampled,
39、the diameter of the crystallizing dish and the quantity of water added; d) the magnification used; e) the results obtained as described in Clause 6, as well as the minimum and maximum lengths measured; f) the date of the measurement; g) all procedural details not specified in this method. BS ISO 223
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