BS ISO 1407-2011 Rubber Determination of solvent extract《橡胶 溶剂提取物的测定》.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 1407:2011Rubber Determination of solvent extractBS ISO 1407:2011 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 1407:2011. It super

2、sedes BS ISO 1407:2009, which is withdrawn.The UK participation in its preparation was entrusted to T e c h n i c a l C o m m i t t e e P R I / 2 3 , T e s t m e t h o d s f o r r u b b e r a n d non-black compounding ingredients.A list of organizations represented on this committee can be obtained

3、on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. BSI 2011 ISBN 978 0 580 66329 1 ICS 83.060 Compliance with a British Standard cannot confer immunity from legal obligations.This Bri

4、tish Standard was published under the authority of the Standards Policy and Strategy Committee on 31 December 2011.Amendments issued since publicationDate T e x t a f f e c t e dBS ISO 1407:2011Rubber Determination of solvent extractCaoutchouc Dtermination de lextrait par les solvants ISO 2011Refere

5、nce numberISO 1407:2011(E)Fourth edition2011-12-01ISO1407INTERNATIONAL STANDARDBS ISO 1407:2011ISO 1407:2011(E)COPYRIGHT PROTECTED DOCUMENT ISO 2011All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or me

6、chanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.or

7、gPublished in Switzerlandii ISO 2011 All rights reservedBS ISO 1407:2011ISO 1407:2011(E) ISO 2011 All rights reserved iiiContents PageForeword iv1 Scope 12 Normative references .13 Principle .14 Solvent .25 Apparatus 26 Preparation of test pieces .26.1 Methods A and B 26.2 Method C (raw rubbers only

8、) 26.3 Method D (raw rubbers only) 47 Procedure 47.1 General .47.2 Method A 47.3 Method B 47.4 Method C 57.5 Method D 68 Calculation and expression of results .78.1 Method A 78.2 Method B 78.3 Method C 88.4 Method D 88.5 Expression of results .89 Precision 810 Test report .8Annex A (informative) Rec

9、ommended solvents .10Annex B (informative) Precision .12Annex C (informative) Example of determination of minimum number of extraction cycles for a raw rubber plus solvent combination of EPDM and 2-butanone16Bibliography .17BS ISO 1407:2011ForewordISO (the International Organization for Standardizat

10、ion) 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 r

11、epresented 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

12、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 Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an Internatio

13、nal 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 document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 1407 was prepa

14、red by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 2, Testing and analysis.This fourth edition cancels and replaces the third edition (ISO 1407:2009), which has been technically revised with the addition of a Method D for raw rubbers only.ISO 1407:2011(E)iv ISO 2011 Al

15、l rights reservedBS ISO 1407:2011INTERNATIONAL STANDARD ISO 1407:2011(E)Rubber Determination of solvent extractWARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associate

16、d with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.IMPORTANT Certain procedures specified in this International Standard may involve the use or generation of substances, or the gen

17、eration of waste, that could constitute a local environmental hazard. Reference should be made to appropriate documentation on safe handling and disposal after use.1 ScopeThis International Standard specifies four methods for the quantitative determination of the material extractable from raw rubber

18、s, both natural and synthetic; two of the methods are also applicable to the unvulcanized and vulcanized compounds of raw rubbers.Method A measures the mass of the solvent extract, after evaporation of the solvent, relative to the mass of the original test portion.Method B measures the difference in

19、 the mass of the test portion before and after extraction.Method C, which is for raw rubbers only, measures the difference in the mass of the test portion before and after extraction using boiling solvent.Method D, which is for raw rubbers only, measures the difference in the mass of the test portio

20、n before and after extraction relative to the mass of the original test portion.NOTE 1 Depending on the test method used, the conditioning of the test portion and the solvent used, the test result is not necessarily the same.NOTE 2 Method C generally gives results which are lower than those obtained

21、 with methods A and B due to the fact that an equilibrium is set up, particularly if large test portions are used, depending on the content and the nature of the extractable matter. Method C is, however, a quicker method than method A or method B.NOTE 3 Methods C and D are not suitable if the test p

22、ortion disintegrates during the extraction.NOTE 4 Method D is normally used for production controls.Recommendations as to the solvent most appropriate for each type of rubber are given in Annex A.2 Normative referencesThe following referenced documents are indispensable for the application of this d

23、ocument. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 1795, Rubber, raw natural and raw synthetic Sampling and further preparative proceduresISO 4661-2, Rubber, vulcanized Preparatio

24、n of samples and test pieces Part 2: Chemical tests3 PrincipleA rubber test piece is extracted with an appropriate solvent in suitable equipment. ISO 2011 All rights reserved 1BS ISO 1407:2011The amount extracted is obtained by measuring either the mass of the extract or the mass of the test piece a

25、fter extraction and comparing it to the mass of the original test piece.4 SolventDuring the analysis, use only solvents of recognized analytical grade.One of the solvents recommended in Table A.1 should preferably be used, unless otherwise specified or agreed between the interested parties.IMPORTANT

26、 Persons using this International Standard should consult the safety data sheet for the solvent before its use and take appropriate measures.5 Apparatus5.1 Balance, precision 0,1 mg.5.2 Extraction apparatus: Examples of suitable types of extraction apparatus are shown in Figure 1. Any other type of

27、apparatus which performs the same extraction function may be used, provided it can be demonstrated to give results which are the same as those obtained using the types of apparatus shown in Figure 1.NOTE The apparatus used for methods C and D is the same as that used for methods A and B, but does no

28、t have an extraction cup.5.3 Regulated heating system.5.4 Rotary evaporator or any other suitable type of evaporation equipment.5.5 Drying equipment, of the oven or vacuum desiccator type.6 Preparation of test pieces6.1 Methods A and BFor raw rubber and unvulcanized compounds, select a laboratory sa

29、mple in accordance with ISO 1795 and pass it at ambient temperature through a two-roll laboratory mill or a press to obtain sheets about 0,5 mm in thickness.For vulcanized rubber, select a laboratory sample in accordance with ISO 4661-2. Since the efficiency of the extraction is a function of the so

30、lid-solvent contact area, comminute the laboratory sample, if necessary, to give fragments of maximum surface area 2 mm2.6.2 Method C (raw rubbers only)6.2.1 Select a laboratory sample in accordance with ISO 1795 and prepare it by either procedure 6.2.2 or procedure 6.2.3.6.2.2 Pass the laboratory s

31、ample at ambient temperature through a two-roll laboratory mill or a press to obtain sheets of 0,5 mm or less in thickness.The thickness of the sheets is important for the efficiency of the extraction. If it is difficult to obtain sheets of thickness 0,5 mm or less, the roll or press temperature may

32、 be increased to a maximum of 100 C.6.2.3 Comminute the laboratory sample to give fragments of maximum surface area 2 mm2.ISO 1407:2011(E)2 ISO 2011 All rights reservedBS ISO 1407:2011a) Kumagawa all-glass extraction apparatusb) Soxhlet all-glass extraction apparatusKey1 condenser2 extraction chambe

33、r3 receiver flaskIt is recommended that the ground joints be ungreased.Figure 1 Suitable types of extraction apparatusISO 1407:2011(E) ISO 2011 All rights reserved 3BS ISO 1407:20116.3 Method D (raw rubbers only)Select a laboratory sample in accordance with ISO 1795. Press a test piece into chromium

34、-nickel wire gauze and roll the gauze into a tube.7 Procedure7.1 GeneralCarry out the determination in duplicate.7.2 Method A7.2.1 Dry the empty receiver flask to constant mass and weigh it (m1).7.2.2 Weigh, to the nearest 1 mg, a test piece of 2 g to 5 g (m0), depending on the amount of extract exp

35、ected.7.2.3 Place the weighed test piece in a cellulose extraction thimble or wrap it in a filter paper or in a woven wire cloth with a mesh suited to the nature and size of the fragments in the test piece (e.g. 150 m or 100 mesh). These wrapping materials shall have been previously cleaned in the s

36、olvent to be used. Place the wrapped test portion in the extraction chamber of the apparatus.7.2.4 Introduce a quantity of solvent equal to two or three times the extraction chamber volume into the receiver flask. Then assemble the extraction apparatus.7.2.5 Carry out the extraction for 16 h 0,5 h (

37、or for a shorter time if it can be demonstrated that the extraction is complete). Adjust the heating conditions during the extraction so that the solvent distils at a rate at which the extraction cup is filled at least five times per hour.7.2.6 At the end of the heating period, turn off the heater,

38、allow the apparatus to cool, remove the extraction chamber from the apparatus and discard the rubber test portion unless it is required for further testing.7.2.7 Using a rotary evaporator and/or other suitable equipment, remove the solvent from the extract until a constant mass is obtained (i.e. unt

39、il the difference between two successive weighings at 30 min intervals is 0,2 % or less). Record the mass of the receiver flask plus extract (m2).The solvent may also be evaporated from the open flask by gentle heating on the heater used for the extraction.CAUTION This may be done only where local h

40、ealth and safety regulations permit and only in a well-ventilated fume cupboard.7.2.8 Carry out a blank test, going through the entire procedure using the same type of apparatus and same quantity of solvent as for the test piece, but omitting the test piece.7.3 Method B7.3.1 Weigh, to the nearest 1

41、mg, a test piece of 0,5 g to 5 g (m0), depending on the amount of extract expected.7.3.2 Place the weighed test piece in a cellulose extraction thimble or wrap it in a filter paper or in a woven wire cloth with a mesh suited to the nature and size of the fragments in the test piece (e.g. 150 m or 10

42、0 mesh). These wrapping materials shall have been previously cleaned in the solvent to be used. Place the wrapped test piece in the extraction chamber of the apparatus.ISO 1407:2011(E)4 ISO 2011 All rights reservedBS ISO 1407:20117.3.3 Introduce a quantity of solvent equal to two or three times the

43、extraction chamber volume into the receiver flask. Then assemble the extraction apparatus.7.3.4 Carry out the extraction for 16 h 0,5 h (or for a shorter time if it can be demonstrated that the extraction is complete). Adjust the heating conditions during the extraction so that the solvent distils a

44、t a rate at which the extraction cup is filled at least five times per hour.7.3.5 At the end of the heating period, turn off the heater, allow the apparatus to cool, remove the extraction chamber from the apparatus and take out the test piece. Discard the solvent in an appropriate manner.7.3.6 Dry t

45、he test piece in an oven to constant mass (i.e. until the difference between two successive weighings at 30 min intervals is 0,2 % or less) at a temperature higher than the boiling point of the solvent used. A drying time of about 1 h at 100 C in a ventilated oven is usually sufficient.CAUTION For s

46、afety reasons, gently blot the test piece with absorbent tissue to remove excess solvent or air dry it in a drying chamber before placing it in the oven.Allow the dried test piece to cool in a desiccator and weigh.It is recommended that the dried test piece be checked to verify that oxidation has no

47、t occurred.NOTE In the presence of air, too high a drying temperature can cause degradation of the test piece and influence the result. The use of a vacuum lowers the boiling point of the solvent.7.4 Method C7.4.1 Cut the laboratory sample of raw rubber into sheets weighing between 90 mg and 110 mg.

48、7.4.2 Weigh, to the nearest 0,1 mg, a test piece of 200 mg to 600 mg (m0), depending on the amount of extract expected.7.4.3 Place the weighed test piece in a 150 ml to 300 ml receiver flask.7.4.4 Add 25 cm3of solvent for each 100 mg of test piece. Connect the condenser to the receiver flask and ref

49、lux for 30 min.7.4.5 At the end of the reflux period, allow the apparatus to cool and remove the receiver flask from the condenser. Decant the solvent and add the same amount of fresh solvent as was added in 7.4.4. Connect the condenser to the receiver flask and reflux for another 30 min.7.4.6 At the end of the second reflux period, allow the apparatus to cool and remove the receiver flask from the condenser. Decant off the solvent and add the same amount of fresh solvent as was added in 7.4.4. Connect the condenser to the