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1、BRITISH STANDARD BS 6063:1992 ISO 4097:1991 Method for Evaluation of general purpose ethylene- propylene-diene rubber (EPDM) Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 15:21:08 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6063:1992 This British Standard, having been prepared under the d
2、irection of the Plastics and Rubber Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 15 July 1992 BSI 06-1999 First published January 1981 Second edition July 1992 The following BSI references relate to the work on this standard: Committee
3、 reference PRM/50 Draft for comment 90/37862 DC ISBN 0 580 21051 0 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Plastics and Rubber Standards Policy Committee (PRM/-) to Technical Committee PRM/50, upon which the following bodies were
4、 represented: British Rubber Manufacturers Association Ltd. Chemical Industries Association Ministry of Defence Tropical Growers Association Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 15:21:08 GMT+00:00 2006, Uncontrolled Copy, (c)
5、 BSI BS 6063:1992 BSI 06-1999i Contents Page Committees responsibleInside front cover National forewordii 1Scope1 2Normative references 1 3Sampling and sample preparation 1 4Physical and chemical tests on raw rubber1 5Preparation of the test mixes for evaluation of EPDM rubbers1 6Evaluation of vulca
6、nization characteristics with a curemeter test4 7Evaluation of tensile stress-strain properties of vulcanized test mixes4 8Test report5 Annex A (normative) Internal mixer6 Table 1 Standard test formulae for evaluation of EPDM rubbers2 List of referencesInside back cover Licensed Copy: sheffieldun sh
7、effieldun, na, Wed Dec 06 15:21:08 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6063:1992 ii BSI 06-1999 National foreword This British Standard has been prepared under the direction of the Plastics and Rubber Standards Policy Committee and is identical with ISO 4097:1991 Rubber, ethylene-propylene
8、-diene (EPDM) General purpose types Evaluation procedure, published by the International Organization for Standardization (ISO). It supersedes BS 6063:1981 which is withdrawn. The Technical Committee has reviewed the provisions of ISO 37:1977, ISO 248:1991, ISO 289:1985 and ISO 6502:1991, to which r
9、eference is made in the text, and has decided that they are acceptable for use in conjunction with this standard. Additional information. It is customary in the UK to condition the rubber at 23 C which is one of the preferred temperatures given in ISO 2393:1973 (see 5.2.2.1 i), 5.2.2.2.1 g), 5.2.2.2
10、.2 g) and clause 7). A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-references Int
11、ernational standardCorresponding British Standard ISO 247:1990BS 7164 Chemical tests for raw and vulcanized rubber Part 5:1991 Methods for determination of ash content (Identical) ISO 471:1983BS 903 Physical testing of rubber Part A35:1985 Temperatures, humidities and times for conditioning, and tes
12、ting of test pieces (Identical) ISO 1795:1974 ISO 1796:1982 BS 6315:1982 Methods for sampling and sample preparation of raw rubber (Technically equivalent) ISO 2393:1973BS 1674:1976a Specification for equipment and general procedure for mixing and vulcanizing rubber test mixes (Technically equivalen
13、t) ISO 3417:1991BS 903 Physical testing of rubber Part A60 Curemetering Section 60.2:1992 Method for the determination of vulcanization characteristics using an oscillating disc curemeter (Identical) a BS 1674 was revised in 1991 and is now only related to ISO 2393:1973. Summary of pages This docume
14、nt comprises a front cover, an inside front cover, pages i and ii, pages 1 to 6, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy
15、: sheffieldun sheffieldun, na, Wed Dec 06 15:21:08 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 4097:1991(E) BSI 06-19991 1 Scope This International Standard specifies physical and chemical tests on raw rubbers; standard materials, standard test formulae, equipment and processing methods for evalu
16、ating the vulcanization characteristics of general purpose ethylene-propylene-diene (EPDM) rubbers, including oil-extended types. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time
17、 of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO mainta
18、in registers of currently valid International Standards. ISO 37:1977, Rubber, vulcanized Determination of tensile stress-strain properties. ISO 247:1990, Rubber Determination of ash. ISO 248:1991, Rubbers, raw Determination of volatile-matter content. ISO 289:1985, Rubber, unvulcanized Determination
19、 of Mooney viscosity. ISO 471:1983, Rubber Standard temperatures, humidities and times for tire conditioning and testing of test pieces. ISO 1795:1974, Raw rubber in bales Sampling. ISO 1796:1982, Rubber, raw Sample preparation. ISO 2393:1973, Rubber test mixes Preparation, mixing and vulcanization
20、Equipment and procedures. ISO 3417:1991, Rubber Measurement of vulcanization characteristics with the oscillating disc curemeter. ISO 6502:1991, Rubber Measurement of vulcanization characteristics with rotorless curemeters. 3 Sampling and sample preparation 3.1 A sample of mass approximately 1 500 g
21、 shall be taken by the method described in ISO 1795. 3.2 Preparation of the test portion shall be in accordance with ISO 1796. 4 Physical and chemical tests on raw rubber 4.1 Mooney viscosity Determine the Mooney viscosity in accordance with ISO 289 on a test portion prepared as indicated in ISO 179
22、6. If a massing process is necessary, maintain the mill roll surface temperature at 35 C 5 C. Record the result as ML (1 + 4) at 125 C. Other test conditions, 100 C or 150 C instead of 125 C, and 8 min instead of 4 min, may be used by agreement between the interested parties. 4.2 Volatile matter Det
23、ermine the volatile matter content by the oven method as specified in ISO 248. 4.3 Ash Determine the ash in accordance with method A or method B of ISO 247. 5 Preparation of the test mixes for evaluation of EPDM rubbers 5.1 Standard test formulae The standard test formulae are given in Table 1, in w
24、hich formula 1 is applicable to non-oil-extended EPDM with an ethylene content no higher than 67 % by mass; formula 2 is applicable to non-oil-extended EPDM with an ethylene content higher than 67 % by mass; formula 3 is applicable to oil-extended EPDM containing less than 80 parts by mass of oil pe
25、r 100 parts of rubber; formula 4 is applicable to oil-extended EPDM containing 80 or more parts by mass of oil per 100 parts of rubber. The materials shall be NIST1) standard reference materials as indicated in Table 1, or other equivalent national or international standard reference materials. 5.2
26、Procedure 5.2.1 Equipment and procedure Equipment and procedure for the preparation, mixing and vulcanization shall be in accordance with ISO 2393. Details of a suitable internal mixer are given in Annex A. 1) National Institute of Standards and Technology (formerly the National Bureau of Standards)
27、 of the USA. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 15:21:08 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 4097:1991(E) 2 BSI 06-1999 5.2.2 Mixing procedures Two alternative mixing procedures are specified. Method A Mill mixing. Method B Internal mixer for initial and mill for final
28、 mixing. NOTE 1Mixing of ethylene-propylene-diene rubbers in the standard test formulae using a mill is more difficult than for other rubbers and the use of an internal mixer allows better results to be obtained. Because of the difficulty of mixing EPDM rubbers, it is recommended that method B be us
29、ed whenever such apparatus is available. Table 1 Standard test formulae for evaluation of EPDM rubbers MaterialNIST standard reference material number Test formula 1234 Parts by mass EPDM100,00100,00100,00 + Ya100,00 + Zb Stearic acid3721,001,001,001,00 Oil furnace black (HAF)c37880,00100,0080,00150
30、,00 ASTM 103 oild50,0075,0050,00 Ya Zinc oxide3705,005,005,005,00 Sulfur3711,501,501,501,50 Tetramethyl thiuram disulfide (TMTD)e 1,001,001,001,00 Mercaptobenzothiazole (MBT) 3830,500,500,500,50 Total239,00284,00239,00 + (Y 50) 259,00 + Z if Y 50 a “Y” is the number of parts by mass of oil per 100 p
31、arts of base rubber in the oil-extended rubber. If Y is greater than 50, do not add oil to formula 3. In this case, the total mass of the formula will be higher than 239. b “Z” is the number of parts by mass of oil per 100 parts of base rubber for types having a minimum oil content of 80. c The curr
32、ent Industry Reference Black may be used in place of NIST 378, but this may give slightly different results. d This oil, density 0,92 g/cm3, is produced by the Sun Refining and Marketing Company and distributed by R.E. Carroll Inc., P.O. Box 139, Trenton, NJ 08601, USA. Overseas requests should be d
33、irected to Sunoco Overseas Inc., 1801 Market Street, Philadelphia, PA 19103, USA. Alternative oils, such as Circosol 4240 or Shellflex 724, are suitable but may give slightly different results. ASTM 103 oil has the following characteristics: Kinematic viscosity at 100 C: 16,8 mm2/s 1,2 mm2/s; Viscos
34、ity gravity constant: 0,889 0,002. The viscosity gravity constant is calculated from the Saybolt Universal viscosity at 37,8 C and the relative density at 15,5/15,5 C. Use the following equation to calculate the VGC from the measured properties: where dis the density at 15,5/15,5 C; vis the Saybolt
35、Universal viscosity at 37,8 C. e A standard reference material for TMTD is available as IRM 1 from Forcoven Products Inc., P.O. Box 1556, Humble, Texas 77338, USA. VGC 10d1,0752 log10v 38() 10 log10v 38() - -= Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 15:21:08 GMT+00:00 2006, Uncontroll
36、ed Copy, (c) BSI ISO 4097:1991(E) BSI 06-19993 5.2.2.1 Method A Mill mixing 5.2.2.2 Method B Internal mixer for initial and mill for final mixing 5.2.2.2.1 Stage 1 Initial mixing procedure a) The standard laboratory mill batch mass, in grams, shall be based on twice the formula mass. The surface tem
37、peratures of the rolls shall be maintained at 35 C 5 C throughout the mixing. Mix the zinc oxide, stearic acid, oil and carbon black together in a suitable container before starting to mix. A good rolling bank at the nip of the rolls shall be maintained during mixing. If this is not obtained with th
38、e nip settings specified here-under, small adjustments to the mill openings may be necessary. Duration (min) Cumulative time (min) b) Band the rubber on the fast roll with the mill set at 35 C and 0,7 mm opening.1,01,0 c) Add the mixture of oil, carbon black, zinc oxide and stearic acid, with a spat
39、ula, evenly across the mill. When about half of the mixture is incorporated, open the mill to 1,3 mm and make one 3/4 cut from each side. Then add the remainder of the mixture, opening the mill to 1,8 mm. When all the mixture has been incorporated, make two 3/4 cuts from each side. 13,014,0 d) Add a
40、ccelerators and sulfur, evenly across the rolls still at 1,8 mm opening.3,017,0 e) Make three 3/4 cuts from each side, allowing 15 s between each cut.2,019,0 f) Cut the batch from the mill. Set the mill opening at 0,8 mm and pass the rolled batch endwise through the rolls six times, introducing it f
41、rom each end alternately.2,021,0 Total time 21,0 g) Sheet the batch to approximately 6 mm. Check-weigh the batch (see ISO 2393). If the mass of the batch differs from the theoretical value by more than 0,5 %, discard the batch and re-mix. Remove sufficient material for curemeter testing. h) Sheet th
42、e batch to approximately 2,2 mm for preparing test slabs or to the appropriate thickness for preparing ISO ring specimens. i) Condition the batch for 2 h to 24 h after mixing and prior to vulcanizing, if possible at standard temperature and humidity as defined in ISO 471. Duration (min) Cumulative t
43、ime (min) a)Adjust the temperature of the internal mixer to achieve a final mix temperature of 150 C in about 5 min. Close the discharge door, set the rotor at 8 rad/s (77 r/min), start the rotor and raise the ram. b)Load the rubber, the zinc oxide, the carbon black, the oil and the stearic acid Low
44、er the ram.0,50,5 c)Allow the batch to mix.2,53,0 d)Raise the ram and clean the mixer throat and the top of the ram. Lower the ram.0,53,5 e)Discharge the batch when the temperature reaches 150 C or after 5 min, whichever occurs first. 1,5 (max.)5,0 Total time (max.) 5,0 f)Immediately pass the batch
45、three times through a laboratory mill with a mill opening of 2,5 mm and a temperature of 50 C 5 C. Check-weigh the batch (see ISO 2393). If the mass of the batch differs from the theoretical value by more than 0,5 %, discard the batch and re-mix. g)Leave the batch for at least 30 min and up to 24 h,
46、 if possible at standard temperature and humidity as defined in ISO 471. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 15:21:08 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 4097:1991(E) 4 BSI 06-1999 5.2.2.2.2 Stage 2 Final mill mixing procedure A good rolling bank at the nip of the rolls
47、 shall be maintained during mixing. If this is not obtained with the nip settings specified hereunder, small adjustments to the mill openings may be necessary. 6 Evaluation of vulcanization characteristics with a curemeter test Measure the following standard test parameters: ML, MH (at defined time)
48、, tst, t9c(50) and t9c(90) in accordance with ISO 3417 or ISO 6502, using the following test conditions: 7 Evaluation of tensile stress-strain properties of vulcanized test mixes Vulcanize sheets at 160 C for three periods chosen from a cure series of 10 min. 20 min, 30 min, 40 min and 50 min. The t
49、hree periods of cure shall be chosen to cover the undercure, optimum cure and overcure of the material under test. Condition the vulcanized sheets for 16 h to 96 h at a standard temperature, and if possible a standard humidity, defined in ISO 471. Measure the stress-strain properties in accordance with ISO 37. a)The standard laboratory mill batch mass, in grams, shall be based on twice the formula mass.