1、BRITISH STANDARD BS ISO 10119:2002 Carbon fibre Determination of density ICS 59.100.20 BS ISO 10119:2002 This British Standard, having been prepared under the direction of the Materials and Chemicals Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and
2、Strategy Committee on 26 July 2002 BSI 26 July 2002 ISBN 0 580 40122 7 National foreword This British Standard reproduces verbatim ISO 10119:2002 and implements it as the UK national standard. It supersedes BS 7658-1:1993 which is withdrawn. The UK participation in its preparation was entrusted to T
3、echnical Committee PRI/42, Fibre reinforced thermosetting plastics and prepregs, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European public
4、ations referred to in this document may be found in 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 nece
5、ssary provisions of a contract. Users are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the in
6、terpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 10, an insid
7、e back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments Reference number ISO 10119:2002(E)INTERNATIONAL STANDARD ISO 10119 Second edition 2002-05-01 Carbon fibre Determina
8、tion of density Fibre de carbone Dtermination de la masse volumique BSISO10119:2002ii BSISO10119:2002 iiiContents Page Foreword.iv 1 Scope 1 2 Normative references1 3 Term and definition .1 4 Test specimens General requirements.1 5 Conditioning and test conditions 2 6 Test methods .2 6.1 Method A: L
9、iquid-displacement method.2 6.2 Method B: Sink/float method5 6.3 Method C: Density-gradient column6 7 Precision.7 8 Test report 8 Annex A (normative) Preparation of the density-gradient column9 BSISO10119:2002iv Foreword ISO (the International Organization for Standardization) is a worldwide federat
10、ion 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 committe
11、e. 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
12、with the rules given in the ISO/IEC Directives, Part 3. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires app
13、roval 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. ISO 10119 was prepared by T
14、echnical Committee ISO/TC 61, Plastics, Subcommittee SC 13, Composites and reinforcement fibres. This second edition cancels and replaces the first edition (ISO 10119:1992), which has been technically revised. Annex A forms a normative part of this International Standard. BSISO10119:2002 1Carbon fib
15、re Determination of density 1 Scope This International Standard specifies three methods for the determination of the density of carbon fibre yarn: method A: liquid-displacement method; method B: sink/float method; method C: density-gradient column method. Method C is the reference method. 2 Normativ
16、e references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based
17、 on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of curren
18、tly valid International Standards. ISO 291, Plastics Standard atmospheres for conditioning and testing ISO 1675, Plastics Liquid resins Determination of density by the pyknometer method ISO 10548, Carbon fibre Determination of size content 3 Term and definition For the purposes of this International
19、 Standard, the following term and definition apply. 3.1 density the mass per unit volume of a substance at a specified temperature NOTE This property is expressed in grams per cubic centimetre or in kilograms per cubic metre at the specified temperature. The recommended temperature is 23 C. 4 Test s
20、pecimens General requirements Test specimens shall be taken from desized samples unless otherwise agreed between the supplier and the customer. To remove the size, use the solvent extraction, chemical digestion or pyrolysis method specified in ISO 10548. The determination of the density may also be
21、carried out on sized fibre by agreement between customer and supplier. The density of sized fibre may be taken to be identical to that of unsized fibre when the size content is low. BSISO10119:20022 5 Conditioning and test conditions Before testing, test specimens shall be conditioned in a standard
22、test atmosphere as specified in ISO 291. During the test, the test apparatus and specimens shall be maintained at the same conditions as used for conditioning. The preferred conditions are 23 C 2 C and (50 10) % relative humidity. 6 Test methods 6.1 Method A: Liquid-displacement method 6.1.1 Princip
23、le A specimen is weighed in air and then in a liquid which completely wets out the specimen and which has a known density at least 0,2 g/cm 3less than that of the specimen. The difference in weight of the specimen in the two media is due to the Archimedean upthrust. 6.1.2 Apparatus and materials Sta
24、ndard laboratory apparatus and the following: 6.1.2.1 Analytical balance, readable to 0,1 mg, with a maximum permissible error of 0,5 mg, and with a range from 0 g to 100 g. 6.1.2.2 Suspension wire, made of stainless steel, of diameter 0,4 mm or less, or a specimen support, made of glass or stainles
25、s steel, with perforations so that it can be immersed easily in the immersion liquid (see Figure 1). Perforated stainless-steel support Perforated glass support Stainless-steel gauze support Figure 1 Examples of test specimen supports 6.1.2.3 Pyknometer or hydrometer, maximum permissible error 0,001
26、 g/cm 3 . 6.1.2.4 Beaker, made of borosilicate glass. 6.1.2.5 Vacuum pump (optional). 6.1.2.6 Ultrasonic device (optional). BSISO10119:2002 36.1.2.7 Immersion liquids (examples): ethanol 23= 0,79 g/cm 3 ; acetone 23= 0,79 g/cm 3 ; methanol 23= 0,80 g/cm 3 ; dichloroethane 23= 1,25 g/cm 3 ; o-dichlor
27、obenzene 23= 1,31 g/cm 3 ; trichloroethane 23= 1,35 g/cm 3 ; trichloromethane 23= 1,48 g/cm 3 ; carbon tetrachloride 23= 1,59 g/cm 3 . WARNING Take the necessary safety precautions when handling these liquids. 6.1.3 Test specimen Take a continuous length of yarn and form it into a convenient shape,
28、for example a bow or knot. 6.1.4 Procedure 6.1.4.1 Carry out all weighings using the analytical balance (6.1.2.1). 6.1.4.2 Determine the exact density of the immersion liquid (6.1.2.7) at the temperature of the test, using the pyknometer (see 6.1.2.3) in accordance with ISO 1675, or the hydrometer (
29、see 6.1.2.3). 6.1.4.3 Weigh the specimen in air to the nearest 0,1 mg (w 1 ). If the specimen is weighed using a suspension wire or specimen support (6.1.2.2), the wire or support shall be tared or weighed and, if weighed, its weight shall be deducted from subsequent weighings of the specimen. 6.1.4
30、.4 Immerse the test specimen in the beaker (6.1.2.4) containing the immersion liquid (6.1.2.7) and remove any air bubbles by agitating the specimen or by pressing it. Weigh the specimen to the nearest 0,1 mg (w 2 ), watching the balance display for a few seconds to make sure that it does not drift a
31、s a result of convection currents. NOTE 1 The main sources of error are: a) air bubbles adhering to the surfaces of the specimen when weighing in the immersion liquid; b) surface tension effects on the specimen or suspension wire; c) convection currents in the liquid in which the specimen is suspend
32、ed, to minimize which the temperature of the liquid and of the air in the balance case should be the same. NOTE 2 A vacuum pump (6.1.2.5) or ultrasonic device (6.1.2.6) may be used to eliminate air bubbles. NOTE 3 In order to minimize the adherence of air bubbles to the test specimen, it is recommen
33、ded that one of the immersion liquids listed in 6.1.2.7 is used. If water is used, it is permissible to add a trace (say 1 part in 10 000) of surface-active material such as a detergent to the water. BSISO10119:20024 Key 1 Balance 2 Support framework 3 Suspension wire 4 Beaker 5 Beaker support jack
34、6 Balance 7 Suspension hook 8 Suspension wire 9 Test specimen 10 Support bridge Figure 2 Examples of apparatus for determining density by the liquid-displacement method 6.1.5 Expression of results The density, in grams per cubic centimetre, of the test specimen at a temperature is given by the equat
35、ion: 1 L 12 w ww q r r = -where w 1is the weight, in grams, of the specimen in air; BSISO10119:2002 5w 2is the weight, in grams, of the specimen in the immersion liquid; Lis the density, in grams per cubic centimetre, of the immersion liquid. 6.2 Method B: Sink/float method 6.2.1 Principle This meth
36、od is based on the observation of the state of equilibrium of the carbon fibre in a liquid mixture that has the same density as the fibre. Two versions of this method are specified: method B1: a dynamic method in which the mixture of liquids required to hold the test specimen in uniform suspension i
37、s made progressively; method B2: test portions of finely chopped yarn are placed in a series of liquid mixtures of different known densities. 6.2.2 Apparatus and materials 6.2.2.1 Thermometer. 6.2.2.2 Pyknometer or hydrometer, maximum permissible error 0,001 g/cm 3 . 6.2.2.3 Test tubes or sample tub
38、es, of 5 cm 3capacity, fitted with stoppers resistant to the liquid employed. 6.2.2.4 Measuring cylinder, of 250 cm 3capacity. 6.2.2.5 Thermostatic bath, capable of maintaining the temperature of the solution in the tubes at 23 C 0,1 C. 6.2.2.6 Tweezers. 6.2.2.7 Razor blades. 6.2.2.8 Liquid-storage
39、flask, of 250 cm 3capacity. 6.2.2.9 Immersion liquids: Two liquids which, when mixed, will cover the range of densities required (examples): acetone, methanol, ethanol, petroleum spirit 23= 0,8 g/cm 3 ; trichloroethane 23= 1,35 g/cm 3 ; carbon tetrachloride 23= 1,59 g/cm 3 ; dibromoethane 23= 2,17 g
40、/cm 3 ; bromoform 23= 2,89 g/cm 3 . WARNING Take the necessary safety precautions when handling these liquids. 6.2.3 Test specimens Take lengths of yarn with a mass of approximately 10 mg to 20 mg (method B1) or approximately 100 g portions of finely chopped fibre (method B2). BSISO10119:20026 6.2.4
41、 Procedure 6.2.4.1 Method B1 6.2.4.1.1 Prepare a mixture of the two selected immersion liquids (6.2.2.9) in the flask (6.2.2.8) to obtain a mixture whose density is less than that of the specimens. Mix the liquids thoroughly, bring the mixture to 23 C 0,1 C and maintain it at this temperature. 6.2.4
42、.1.2 Form a test specimen into a knot, place in the liquid mixture then de-aerate under a vacuum of 60 hPa, maintaining the vacuum for at least 2 min. 6.2.4.1.3 Add progressively several drops of the denser liquid, stirring to ensure thorough mixing. Continue the addition until the specimen remains
43、in suspension in the middle of the flask. Wait 5 min. If the specimen sinks add several drops of the denser liquid, if it floats add several drops of the less dense liquid until the specimen remains stationary. Filter the liquid mixture and determine its density using the pyknometer (see 6.2.2.2) in
44、 accordance with ISO 1675, or the hydrometer (see 6.2.2.2). 6.2.4.2 Method B2 6.2.4.2.1 Prepare mixtures of immersion liquids (6.2.2.9) covering the required density range at increments of 0,2 g/cm 3 . Determine the density of each mixture using the pyknometer in accordance with ISO 1675, or hydrome
45、ter, noting the temperature at which the determinations were carried out. A small quantity of wetting agent may be added if necessary. 6.2.4.2.2 Fill six 5 cm 3test tubes (6.2.2.3) with 2,5 cm 3of the liquid mixture. Introduce into each test tube a quantity of finely chopped carbon fibres sufficient
46、 to cover a pin head (about 100 g). Stopper and shake the tubes well, and allow the tubes to stand at the same temperature as that at which the determinations of the densities of the solutions were carried out. 6.2.4.2.3 After 60 min, observe the position of the fibres in the tubes against a white b
47、ackground. 6.2.4.2.4 The density of the yarn is given by the density of the mixture in which the majority of the fibres are held in suspension. 6.2.5 Expression of results Express the density of the carbon fibre yarn in grams per cubic centimetre or in kilograms per cubic centimetre. 6.3 Method C: D
48、ensity-gradient column 6.3.1 Principle This method is based on the observation of the equilibrium position of a test specimen in a column of liquid having a linear density gradient. Density-gradient columns are columns of liquid whose density increases uniformly from the top to the bottom of the col
49、umn. 6.3.2 Apparatus and materials 6.3.2.1 Density-gradient column, consisting of a vertical graduated tube, open at the top, length approximately 1 m, diameter 40 mm to 50 mm, surrounded by a water jacket maintained at a temperature of 23 C 0,1 C. A stainless-steel basket, which can be raised and lowered by means of a wire not attacked by the liquids used, is situated at the base of the column. 6.3.2.2 A seri
