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1、 Reference number ISO 2302:2005(E) ISO 2005 INTERNATIONAL STANDARD ISO 2302 Fifth edition 2005-01-15 Isobutene-isoprene rubber (IIR) Evaluation procedures Caoutchouc isobutne-isoprne (IIR) Mthodes dvaluation ISO 2302:2005(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance
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4、very care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. ISO 2005 All rights reserved. Unless otherwise specified, no part of this publica
5、tion may be reproduced or utilized in any form or by any means, electronic or mechanical, 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 office Case postale 56 CH-1211 Geneva
6、20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2005 All rights reserved -,-,- ISO 2302:2005(E) ISO 2005 All rights reserved iii Contents Page Forewordiv 1 Scope1 2 Normative references .1 3 Sampling and further preparative proc
7、edures.1 4 Physical and chemical tests on raw rubber.2 4.1 Mooney viscosity2 4.2 Volatile matter .2 4.3 Ash2 5 Preparation of test mixes for evaluation of isobutene-isoprene rubbers.2 5.1 Standard test formulation 2 5.2 Procedure.2 6 Evaluation of vulcanization characteristics by a curemeter test.6
8、6.1 Using oscillating-disc curemeter 6 6.2 Using rotorless curemeter .7 7 Evaluation of tensile stress-strain properties of vulcanized test mixes.7 8 Precision7 8.1 General.7 8.2 Precision details7 8.3 Precision results .8 9 Test report8 Bibliography .10 -,-,- ISO 2302:2005(E) iv ISO 2005 All rights
9、 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
10、 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 a
11、ll 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 Standards. Draft International Standards adopted by the technical committees are
12、 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 document may be the subject of patent rights. ISO shall not be held re
13、sponsible for identifying any or all such patent rights. ISO 2302 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry. This fifth edition cancels and replaces the fourth edition (ISO 2302:1995),
14、which has been technically revised. The precision data in this edition have been taken, with permission of ASTM, from ASTM D 3188-95, Standard Test Methods for Rubber Evaluation of IIR (Isobutene-Isoprene Rubber), copyright ASTM. -,-,- INTERNATIONAL STANDARD ISO 2302:2005(E) ISO 2005 All rights rese
15、rved 1 Isobutene-isoprene rubber (IIR) Evaluation procedures WARNING 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, associated with its use. It is the responsibility of the us
16、er to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. 1 Scope This International Standard specifies physical and chemical tests on raw rubbers; standardized materials, a standardized test formulation, equipment and processing method
17、s for evaluating the vulcanization characteristics of all types of isobutene-isoprene rubber (IIR). 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the late
18、st edition of the referenced document (including any amendments) applies. ISO 37, Rubber, vulcanized or thermoplastic Determination of tensile stress-strain properties ISO 247:1990, Rubber Determination of ash ISO 248, Rubbers, raw Determination of volatile-matter content ISO 289-1, Rubber, unvulcan
19、ized Determinations using a shearing-disc viscometer Part 1: Determination of Mooney viscosity ISO 1795:2000, Rubber, raw natural and raw synthetic Sampling and further preparative procedures ISO 2393:1994, Rubber test mixes Preparation, mixing and vulcanization Equipment and procedures ISO 3417, Ru
20、bber Measurement of vulcanization characteristics with the oscillating disc curemeter ISO 6502, Rubber Guide to the use of curemeters ISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods 3 Sampling and further preparative procedures A laboratory s
21、ample of approximately 1,5 kg shall be taken in accordance with the method described in ISO 1795. Preparation of the sample shall be in accordance with ISO 1795. -,-,- ISO 2302:2005(E) 2 ISO 2005 All rights reserved 4 Physical and chemical tests on raw rubber 4.1 Mooney viscosity Prepare a test port
22、ion in accordance with the preferred procedure in ISO 1795, i.e. without milling, cutting the test portion directly from the laboratory sample. The test portion shall be as free as possible from air and pockets that may trap air against the rotor and die surface. If agreed between the interested par
23、ties or if the condition of the sample (e.g. excessive porosity) makes milling necessary, it shall be performed in accordance with ISO 1795:2000, Subclause 8.3.2.2, paragraphs 1 and 2. Determine the Mooney viscosity in accordance with ISO 289-1 on this test portion, as ML(1+8) at 125 C. 4.2 Volatile
24、 matter Determine the volatile-matter content by the hot-mill method or by the oven method as specified in ISO 248. 4.3 Ash Determine the ash in accordance with either method A or method B of ISO 247:1990. 5 Preparation of test mixes for evaluation of isobutene-isoprene rubbers 5.1 Standard test for
25、mulation The standard test formulation is given in Table 1. The materials shall be national or international standard reference materials (or as agreed by the interested parties). Table 1 Standard test formulation Material Parts by mass Isobutene-isoprene rubber (IIR) 100,00 Stearic acid a 1,00 Indu
26、stry reference black b 50,00 Zinc oxide a 3,00 Sulfur a 1,75 Tetramethylthiuram disulfide(TMTD) a 1,00 Total 156,75 a Powder materials shall be used (standard curing ingredients used in the industry). b The current industry reference black shall be used. 5.2 Procedure 5.2.1 Equipment and procedure T
27、he equipment and procedure for the preparation, mixing and vulcanization shall be in accordance with ISO 2393:1994, Clauses 6, 7, 8 and 9. ISO 2302:2005(E) ISO 2005 All rights reserved 3 5.2.2 Mixing procedures 5.2.2.1 General Three alternative mixing procedures are specified: Method A: mixing with
28、a laboratory mill; Method B: mixing with a miniature internal mixer (MIM); Method C: mixing with an internal mixer. NOTE These procedures may not give identical results. 5.2.2.2 Method A Mixing with a laboratory mill The standard laboratory mill-batch mass, in grams, shall be based on four times the
29、 formulation mass (i.e. 4 156,75 g = 627 g). The surface temperature of the rolls shall be maintained at 45 C 5 C throughout the mixing. A good rolling bank at the nip of the rolls shall be maintained during mixing. If this is not obtained with the nip settings specified hereunder, small adjustments
30、 to the mill openings may be necessary. A mill batch mass based on two times the formulation mass may also be used, but, in this case, more adjustments to the mill openings will be necessary. Duration (min) Cumulative time (min) a) Band the rubber with the mill opening set at 0,65 mm. 1,0 1,0 b) Mix
31、 the carbon black and the stearic acid and add evenly across the mill rolls at a uniform rate. Increase the mill opening at intervals to maintain a constant rolling bank. When all the carbon black has been incorporated, make a 3/4 cut from each side. Do not cut the batch while free carbon black is e
32、vident in the bank or on the milling surface. Be certain to return to the batch any materials that drop through the mill. 10,0 11,0 c) Add the zinc oxide, the sulfur and the TMTD. 3,0 14,0 d) Make three alternating 3/4 cuts from each side. 2,0 16,0 e) Cut the batch from the mill. Set the mill openin
33、g to 0,8 mm and pass the rolled batch endwise through the mill six times. 2,0 18,0 f) Sheet the batch to approximately 6 mm and check-weigh the batch (see ISO 2393). If the mass of the batch differs from the theoretical value by more than 0,5 1,5 + %, discard the batch and re-mix. g) Remove sufficie
34、nt material for curemeter testing. h) Sheet the batch to approximately 2,2 mm for preparing test sheets or to the appropriate thickness for preparing ISO ring or dumbbell test pieces in accordance with ISO 37. i) After mixing, condition the batch for at least 2 h but not more than 24 h, if possible
35、at standard laboratory temperature and humidity as defined in ISO 23529. -,-,- ISO 2302:2005(E) 4 ISO 2005 All rights reserved 5.2.2.3 Method B Mixing with a miniature internal mixer (MIM) For a miniature internal mixer having a nominal mixing capacity of 64 cm3, a batch mass corresponding to 0,47 t
36、imes the formulation mass (i.e. 0,47 156,75 = 73,67 g) has been found to be suitable. Mix with the head temperature of the miniature internal mixer maintained at 60 C 3 C and a starting (unloaded) rotor speed of 6,3 rad/s to 6,6 rad/s (60 rpm to 63 rpm). Prepare the rubber by passing it once through
37、 a laboratory mill with the roll temperature set at 50 C 5 C and an opening of 0,5 mm. Cut the sheet thus produced into strips 25 mm wide. In the following procedure, compounding materials other than rubber, e.g. carbon black, may be added to the batch more precisely and with greater ease if they ar
38、e previously blended together in the proportions required by the formulation. Such blends may be made using one of the following: a mortar and pestle; a double-cone mixer (mix for 10 min with the intensifier bar turning); a blender (mix for five periods of 3 s each, scraping the inside of the blende
39、r to dislodge material stuck to the sides after each 3 s period) (a “Waring”-type blender has been found suitable for this method). CAUTION If the mixing periods are longer than 3 s, the stearic acid may melt, thus preventing good dispersion. Duration (min) Cumulative time (min) a) Load the rubber,
40、lower the ram and allow the rubber to be masticated. 1,0 1,0 b) Raise the ram and add the zinc oxide, sulfur, stearic acid and TMTD, taking care to avoid any loss. Then add the carbon black. Sweep the mouth of the mixing chamber and lower the ram. 1,0 2,0 c) Allow the batch to mix. 3,0 5,0 d) Turn o
41、ff the rotor, raise the ram, remove the mixing chamber and discharge the batch. Record the maximum batch temperature. The final temperature of the discharged batch after the cumulative mixing time of 5 min shall not exceed 120 C. If it does, discard the batch and repeat the procedure with a differen
42、t batch mass or head temperature. e) Pass the batch through a mill set at 50 C 5 C twice with a 3,0 mm mill opening. f) Check the batch mass (see ISO 2393) and record. If it differs from the theoretical value by more than 0,5 1,5 + %, discard the batch and re-mix. g) Cut out a test piece for determi
43、ning the vulcanization characteristics in accordance with ISO 3417 or ISO 6502, if required. Condition the test piece for 2 h to 24 h at 23 C 3 C before testing. h) If required, sheet the batch to approximately 2,2 mm for preparing test sheets or to the appropriate thickness for preparing ISO ring o
44、r dumbbell test pieces in accordance with ISO 37. To obtain the effects of mill direction, pass the folded batch four times between mill rolls set at 50 C 5 C and at the appropriate mill opening. Cool on a flat, dry surface. i) After mixing and prior to vulcanizing, condition the batch for at least
45、2 h but not more than 24 h, if possible at standard laboratory temperature and humidity as defined in ISO 23529. ISO 2302:2005(E) ISO 2005 All rights reserved 5 5.2.2.4 Method C Internal mixer for initial and mill for final mixing 5.2.2.4.1 General For an internal mixer of Type A1 (see ISO 2393) hav
46、ing a nominal capacity of 1 170 cm3 40 cm3, a batch mass corresponding to (8,5 156,75 g = 1 332 g) has been found to be suitable. The speed of the fast rotor shall be set at 7 rad/s to 8 rad/s (67 rpm to 87 rpm). During final mixing, a good rolling bank at the nip of the rolls shall be maintained. I
47、f this is not obtained with the nip setting specified, small adjustments to the mill openings may be necessary. 5.2.2.4.2 Stage 1 Initial mixing procedure Duration (min) Cumulative time (min) a) Adjust the temperature of the internal mixer to a starting temperature of 50 C. Close the discharge door,
48、 start the rotors and raise the ram. b) Load the rubber, lower the ram and allow the rubber to be masticated. 0,5 0,5 c) Raise the ram, load the zinc oxide, stearic acid and carbon black, and lower the ram. 0,5 1,0 d) Allow the batch to mix. 2,0 3,0 e) Raise the ram, clean the mixer throat and the top of the ram, and lower the ram. 0,5 3,5 f) Allow the batch to mix. 1,5 5,0 g) Discharge the batch. h) Immediately check the temperature of the batch with a suitable measuring device. If the measured temperature is outside the range