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1、INTERNATIONAL STANDARD ISO. 2476 Fourth edition 1996-l O-l 5 ANSI Internat Lhx Set Rubber, butadiene (BR) - Solution-polymerized types - Evaluation procedures Caoutchouc butadi - standard materials, standard test formulations, equipment and processing methods for evalu- ating the vulcanization chara
2、cteristics of solution- polymerized butadiene rubbers (BR), including oil- extended types (OEBR), and the tensile stress- strain properties of vulcanized mixes. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this Inte
3、rnational Standard. At the time 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 in- vestigate the possibility of applying the most recent editions of the standards indicated bel
4、ow. Members of IEC and IS0 maintain registers of currently valid In- ternational Standards. IS0 37: 1994, Rubber, vulcanized or thermoplastic - Determination of tensile stress-s train properties. IS0 247:1990, Rubber - Determination of ash. IS0 248:1991, Rubbers, raw - Determination of volatile-matt
5、er content. IS0 289-l :I 994, Rubber, unvulcanized - Determi- nations using a shearing-disc viscometer - Part 1. Determination of Mooney viscosity. IS0 471 :I 995, Rubber - Temperatures, humidities and times for conditioning and testing. IS0 1795:1992, Rubber, raw, natural and synthetic - Sampling a
6、nd further preparative procedures IS0 2393: 1994, Rubber test mixes - Preparation, mixing and vulcanization - Equipment and pro- cedures. IS0 3417:1991, Rubber - Measurement of vulcan- ization characteristics with the oscillating disc cure- meter. IS0 6502:1991, Rubber - Measurement of vulcan- izati
7、on characteristics with rotor-less curemeters ISO/TR 9272:1986, Rubber and rubber products - Determination of precision for test method standards. 3 Sampling and preparation of test portion 3.1 A laboratory sample of approximately I,5 kg shall be taken by the method described in IS0 1795. 3.2 Prepar
8、ation of the test portion shall be in accor- dance with IS0 1795. 1 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Defense Supply Ctr/9960866100 Not for Resale, 04/24/2007 09:53:26 MDTNo reproduction or networking permitted without license fr
9、om IHS -,-,- IS0 2476: 1996(E) IS0 4 Physical and chemical tests on raw rubber 4.3 Ash Determine the ash in accordance with IS0 247 4.1 Mooney viscosity Determine the Mooney viscosity in accordance with IS0 289-l on a test portion prepared as indicated in IS0 1795 (preferably without milling). If mi
10、lling is necessary, maintain the mill roll surface temperature at 35 “C f 5 “C. 5 Preparation of test mixes for evaluation of butadiene rubbers 5.1 Standard test formulations Record the result as ML (I+41 at 100 “C. Two standard test formulations are given in table 1 4.2 Volatile matter Determine th
11、e volatile-matter content in accordance with IS0 248. The materials used shall be national or international standard reference materials (or, if no standard refer- ence material is available, as agreed by the interested parties). Table 1 - Standard test formulations Material Butadiene rubber Zinc ox
12、ide Current industry reference black Stearic acid ASTM 103 oil 2) Sulfur TBBS 3) Parts by mass Non-oil-extended Oil-extended 100.00 100,00 1) 3,00 3,00 60.00 60,OO 2.00 2,00 15,00 - I,50 1.50 0,90 0,90 Total 182,40 167,40 Calculated density, g/cm3 1.11 1,14to 1,164) 1) 100 parts of oil-extended rubb
13、er means 100 parts of the rubber including the extender oil 2) This oil, density = 0,92 g/ems, is available in 3,8 litre and 19 litre quantities from Sun Oil, Indus- trial products Dept , 1608 Walnut Street, Philadelphia, PA 19103, USA Alternative oils, such as Cir- cosol 4240, R E Carol1 IRM 43 or
14、Shellflex 724, are suitable but may give slightly different results ASTM 103 oil has the following characteristics Kinematic viscosity at 100 “C 16.8 mmz/s + 1,2 mmz/s Viscosity gravity constant: 0,889 + 0,002 The viscosity gravity constant (VGC) is calculated from the Saybolt universal viscosity at
15、 37,8 “C and the relative density (specific gravity) at 15,5/15,5 “C Use the following equation to calculate the VGC from the measured properties VGC = 1 Od - 1,075 2 log, (u - 38) 10 -log, - method C2, which is limited to non-oil-extended rubbers but gives easier mixing and leads to bet- ter disper
16、sion of the ingredients Methods Cl and C2 will not necessarily give identical results for non-oil-extended solution-polymerized bu- tadiene rubbers. In laboratory cross-checks or in a se- ries of evaluations, the same procedure shall therefore be used in all cases. 5.2.2.3.1 Method Cl The standard l
17、aboratory batch mass, in grams, shall be based on three times the formulation mass (i.e 3 x 182,40 g = 547,20 g or 3 x 167,40 g = 502,20 g). Adjust the mill roll cooling conditions to maintain a temperature of 35 “C f 5 “C throughout the mixing A good rolling bank at the nip of the rolls shall be ma
18、intained during mixing. If this is not obtained with the nip settings specified hereunder, make small ad- justments to the mill openings. Dura- Cumulat- tion ive time (min) (min) a) Band the rubber with the mill opening set at I,3 mm. I,0 I,0 NOTE 3 Non-oil-extended rubbers may require longer millin
19、g to achieve a good band b) cl d) e) Add the zinc oxide and the stearic acid evenly across the rolls Make two 314 cuts from each side 2,o 3,O Add the carbon black evenly across the rolls at a uniform rate. When about half the black has been in- corporated, open the rolls to I,8 mm and then add the r
20、emainder of the black. Make two 3/4 cuts from each side, allowing 30 s between each cut. Be cer- tain to add the black that has dropped into the mill 15,0 to 18,0 to pan. 18,0 21 ,o Add the oil (omit from oil- extended BR) very slowly 8,0 to 26,0 to drop by drop. IO,0 31,0 Add the sulfur and the TBB
21、S. Sweep up any ma- terial which has fallen into the mill pan and add it to 28,0 to the mix. 2,o 33,0 4 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Defense Supply Ctr/9960866100 Not for Resale, 04/24/2007 09:53:26 MDTNo reproduction or net
22、working permitted without license from IHS -,-,- 0 IS0 IS0 2476:1996(E) f) 9) h) i) Make six successive 314 cuts from each side Cut the batch from the mill. Set the mill opening to 0,8 mm and pass the rolled batch endwise through the rolls six times. 30,o to 2,o 35,0 32,0 to zo 37,0 Sheet the batch
23、to approximately 6 mm. Check- weigh the batch (see IS0 2393). If the mass of the batch differs from the theoretical value by more than + 0,5 % or - 1,5 %, discard the batch and re-mix. Remove sufficient material for cure- meter testing. Sheet the batch to approximately 2,2 mm for preparing test shee
24、ts or to the appropriate thick- ness for preparing IS0 ring specimens in accord- ance with IS0 37. 5.2.2.3.2 Method C2 The standard laboratory batch mass, in grams, shall be based on two times the formulation mass (i.e. 2 x 182,40 g = 364,80 g). Adjust the mill roll cooling conditions to maintain a
25、temperature of 35 “C f 5 “C throughout the mixing. Add the ingredients to the batch slowly and evenly across the rolls. Do not cut the batch before all the ingredients have been incor- porated. A good rolling bank at the nip of the rolls shall be maintained during mixing. If this is not obtained wit
26、h the nip settings specified hereunder, make small ad- justments to the mill openings. a) b) c) Dura- Cumulat- tion ive time (min) (min) Pass the rubber twice through the rolls with the mill opening set at 0,45 mm f 0,Ol mm and then band it. Make two successive 3/4 cuts from each side. 24 zo Add the
27、 stearic acid and the zinc oxide. Make three successive 3/4 cuts from each side. 2,o 4,O Add successively half of the oil and half of the car- bon black. Make seven successive 3/4 cuts from each side. 12.0 16,O d) e) f) 9) h) 6 Add successively the re- mainder of the oil and the remainder of the car
28、bon black. Add any black that has dropped into the mill pan. Make seven 314 cuts from each side. 12,0 28,0 Add the TBBS and the sul- fur. Make six 3/4 cuts from each side. 480 32.0 Cut the batch from the mill. Set the mill opening to 0,7 mm to 0,8 mm and pass the rolled batch end- wise through the r
29、olls six times. 3,o 35,0 Sheet the batch to approximately 6 mm and check-weigh the batch (see IS0 2393). If the mass of the batch differs from the theoretical value by more than + 0,5 % or - I,5 %, discard the batch and re-mix. Remove sufficient material for curemeter testing. Sheet the batch to app
30、roximately 2,2 mm for preparing test sheets or to the appropriate thick- ness for preparing IS0 ring specimens in accord- ance with IS0 37. Conditioning of batches Condition all batches produced by method A, B, Cl or C2 for 2 h to 24 h after mixing and prior to vulcanizing, if possible at standard t
31、emperature and humidity as defined in IS0 471. 7 Evaluation of vulcanization characteristics 7.1 Using an oscillating-disc curemeter Measure the following standard test parameters ML, MH at defined time, t,t , t ,(50) and t ,(90) in accordance with IS0 3417, using the following test conditions: osci
32、llation frequency: I,7 Hz (100 cycles per minute) amplitude of oscillation: lo arc selectivity: To be chosen to give at least 75 % of full-scale deflection. NOTE 4 With some rubbers, 75 % may not be attainable 5 Copyright International Organization for Standardization Provided by IHS under license w
33、ith ISO Licensee=Defense Supply Ctr/9960866100 Not for Resale, 04/24/2007 09:53:26 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 2476:1996(E) 0 IS0 die temperature: 160 “C I!I 0,3 “C pre-heat time. None 7.2 Using a rotorless curemeter the 17 laboratories that particip
34、ated in the programme, on each of two days approximately one week apart Formula 1 contained a non-oil-extended BR, while formula 2 contained an oil-extended BR. Measure the following standard test parameters: Only method Cl of this International Standard (mill mixing) was used for preparing the mixe
35、s. FL, Fmax at defined time, t,l, t c,sc and t c,go in accordance with IS0 6502, using the following test conditions: oscillation frequency: I,7 Hz (100 cycles per minute) amplitude of oscillation: 0,5” arc selectivity: To be chosen to give at least 75 % of full-scale deflection at F,ax. NOTE 5 With
36、 some rubbers, 75 % may not be attainable die temperature: 160 “C + 0,3 “C pre-heat time: None The mixes were prepared from special samples of all the necessary materials, sent to each laboratory prior to the actual testing. For each material, the samples were drawn from a uniform and homogeneous lo
37、t. Stress-strain tests were conducted on cured sheets of each of the mixes or compounds as specified by the test programme 9.2.2 Determinations of modulus (stress at 300 %), tensile strength and percent elongation were made, taking as the result the median of five individual de- terminations, as spe
38、cified in IS0 37. All 17 labora- tories performed the test using dumb-bell test pieces Five of the laboratories also performed the test using ring test pieces. The precision thus evaluated is a type 2 precision, and the time period for repeatability and reproducibility is on a scale of days. 8 Evalu
39、ation of tensile stress-strain properties of vulcanized test mixes 9.3 Precision results Vulcanize sheets at 145 “C for 25 min, 35 min and 50 min or, alternatively, at 150 “C for 20 min, 30 min and 50 min. The three periods of cure shall be chosen to cover the undercure, optimum cure and overcure of
40、 the material under test. 9.3.1 The precision results are given in table 2 for dumb-bell test pieces and in table 3 for ring test pieces. The symbols used in tables 2 and 3 are defined as follows: Condition the vulcanized sheets for 16 h to 96 h, if possible at standard temperature and humidity as d
41、e- fined in IS0 471. r = repeatability, in measurement units. This is the value below which the absolute difference between two “within-laboratory” test results may be expected to lie with a specified probability. Measure the stress-strain properties in accordance with IS0 37. (r) = repeatability, i
42、n percent (relative). 9 Precision 9.1 General The precision calculations to express repeatability and reproducibility were performed in accordance with lSO/TR 9272. Consult this for precision concepts and nomenclature. Annex A of this International Standard gives guidance on the use of repeatability
43、 and repro- ducibility. The two test results are obtained with the same method on nominally identical test material under the same conditions (same operator, apparatus and lab- oratory) and within a specified time period; unless stated otherwise, the probability is 95 %. R = reproducibility, in meas
44、urement units. This is the value below which the absolute difference between two “between-laboratory” test results may be ex- pected to lie with a specified probability (R) = reproducibility, in percent (relative). 9.2 Interlaboratory test programme 9.2.1 An interlaboratory test programme was organ-
45、 ized in 1987. Formulations containing two types of BR were selected and mixes were prepared in each of The two test results are obtained with the same method on nominally identical test material under dif- ferent conditions (different laboratories, operators and 6 Copyright International Organizati
46、on for Standardization Provided by IHS under license with ISO Licensee=Defense Supply Ctr/9960866100 Not for Resale, 04/24/2007 09:53:26 MDTNo reproduction or networking permitted without license from IHS -,-,- 0 IS0 IS0 2476:1996(E) apparatus) and within a specified time period; unless stated other
47、wise, the probability is 95 %. 9.3.2 It shall be borne in mind that these precision results apply to the mill mixing procedure of IS0 2476:1988, Rubber, butadiene (BR) - Solution- polymerized types - Evaluation procedure, only (method Cl of this International Standard) NOTE 6 For the general procedu
48、re for using precision re- suits, and their interpretation, see ISO/TR 9272 10 Test report The test report shall include the following: a) a reference to this International Standard; b) all details necessary for the identification of the sample; c) the standard test formula used; d) the reference ma
49、terials used; e) the method used for the volatile-matter determi- nation (mill or oven); f) the mixing procedure used in 5.2.2; g) the vulcanizing temperature and times used in clause 8; h) any unusual features noted during the determi- nation; i) any operation not included in this International Standard or in the International Standards to which reference is made, as well as any operation regarded as optional; 0 the results and the unit