BS ISO 2303:2019 BSI Standards Publication Isoprene rubber (IR) — Non-oil-extended, solution- polymerized types — Evaluation procedures bsi.BS ISO 2303:2019 INTERNATIONAL Iso STANDARD 2303 Isoprene rubber (IR) — Non-oil- extended, solution-polymerized types — Evaluation procedures Caoutchouc isopréne (IR) — Types polymérisés en solution et non étendus a l'huile— Méthode d’évaluation Reference number 180 2303:2019(E) © 180 2019BS ISO 2303:2019 ISO 2303:2019(E) A COPYRIGHT PROTECTED DOCUMENT © 1502019 Al rights reserved. Unless otherwise specified, or required in the context ofits implementation, no part ofthis publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, Including photocopying, or posting fon the internet or an intranet, without prior written permission, Permission can be requested from either ISO at the address ‘below or 1S0's member body inthe country ofthe requester. 180 copyright office CP 401 *Ch.de Blandonnet 8 CH-1214 Vernier, Geneva Phone: #41 2274901 11 Fax: +4122 749 09.47 Email: copyright@'so.0rg Website: wwwiso.ong Published in Switzerland it © 150 2019 ~ All rights reservedBS ISO 2303:2019 ISO 2303:2019(E) Contents Foreword 1 Scope. 2 Normative references 3 Terms and definitions 4 Sampling and sample preparation a 8 9 10 Physical and chemical tests on raw rubber 5.1 Mooney viscosity. 5.2 Volatile matter 5.3 Ash Preparation of the test mixes for evalu: 6.1 Standard test formulation. 62 Procedure 62.1 Equipment and procedure 622 Mill mixing procedures 623 Laboratory internal mixer (LIM) mixing procedure Evaluation of vulcanization characteristics by a curemeter test 7.1 Usingan oscillating-disc curemeter 7.2 Usinga rotorless curemeter mn of isoprene rubbers Evaluation of tensile stress-strain properties of vulcanized test mixes. Precision Test report. Annex A (informative) Precision data for both mill mixer and laboratory internal mixer Annex B (informative) Additional precision data for natural rubber Bibliography. © 150 2019 ~ Allrights reserved Page © © & BOO NYWUNN NNNN NR 10 12 14 ilBS ISO 2303:2019 ISO 2303:2019(E) 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 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 all matters of electrotechnical standardization. The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives), 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. Details of any patent rights identified during the development of the document will be in the Introduction and or ‘on the ISO list of patent declarations received (see www.iso.org/patents). Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement, For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISO's adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www.iso This document 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 sixth edition cancels and replaces the fifth edition (ISO 2303:2011), which has been technically revised. ‘The main change compared to the previous edition is to allow the use of the method given in ISO 248-2 in 5.2 and in Clause 10. Any feedback or questions on this document should be directed to the users national standards body. A complete listing of these bodies can be found at www.iso.org/members.html. iv © 150 2019 ~ All rights reservedBS ISO 2303:2019 INTERNATIONAL STANDARD ISO 2303:2019(E) Isoprene rubber (IR) — Non-oil-extended, solution- polymerized types — Evaluation procedures WARNING — Persons u: This document does use. It is the responsil ig this document should be familiar with normal laboratory practices. purport to address all of the safety problems, if any, associated with its ity of the user to establish appropriate safety and health practices. 1 Scope This document specifies, for general-purpose non-oil-extended, solution-polymerized polyisoprene rubbers (IR): — physical and chemical tests on raw rubbers; — standard materials, a standard test formulation, equipment and processing methods for evaluating the vulcanization characteristics. 2 Normative references ‘The following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (inchiding any amendments) applies. ISO 37, Rubber, vulcanized or thermoplastic — Determination of tensile stress-strain properties 1S0 247-1:2018, Rubber — Determination of ash — Part 1: Combustion method ISO 248-1, Rubber, raw — Determination of volatile-matter content — Part 1: Hot-mill method and oven method 1S0 248-2, Rubber, raw — Determination of volatile-matter content — Part 2: Thermogravimetric methods using an automatic analyser with an infrared drying ISO 289-1, Rubber, unvulcanized — Determinations using a shearing-disc viscometer — Part 1: Determination of Mooney viscosity ISO 1795, Rubber, raw natural and raw synthetic — Sampling and further preparative procedures ISO 2393, Rubber test mixes — Preparation, mixing and vulcanization — Equipment and procedures ISO 6502-1, Rubber — Measurement of vulcanization characteristics using curemeters — Part 1: Introduction ISO 6502-2, Rubber — Measurement of vulcanization characteristics using curemeters — Part 2: Oscillating disc curemeter ISO 23529, Rubber — General procedures for preparing and conditioning test pieces for physical test methods 3 Terms and definitions No terms and definitions are listed in this document. 1S and 1EC maintain terminological databases for use in standardization at the following addresses: — 180 Online browsing platform: available at https://www.iso.org/obp © 150 2019 ~ Allrights reserved 1BS ISO 2303:2019 ISO 2303:2019(E) — IEC Electropedia: available at http://www.electronedia.org/ 4 Sampling and sample preparation 4.1 Alaboratory sample of approximately 1,5 kg shall be taken by the method described in ISO 1795. 4.2. Preparation of the test portion shall be in accordance with ISO 1795, 5S Physical and chemical tests on raw rubber 5.1 Mooney viscosity ‘The Mooney viscosity shall be determined in accordance with ISO 289-1 on a test portion prepared as described in ISO 1795 (without massing). ‘The result shall be recorded as ML(1 + 4) at 100 °C. 5.2 Volatile matter The volatile-matter content shall be determined in accordance with ISO 248-1 or ISO 248-2. 5.3. Ash The ash content shall be determined in accordance with ISO 247-1. 6 Preparation of the test mixes for evaluation of isoprene rubbers 6.1 Standard test formulation ‘The standard test formulation is given in Table 1. The materials shall be national or international standard reference materials. If no standard reference material is available, the materials to be used shall be agreed by the interested parties. Table 1 — Standard test formulation for evaluation of IR rubbers Material Parts by mass Isoprene rubber (IR) 100,00 [Stearic acid 2,00 zinc oxide 5,00 sulfur 2,25 Industry reference black (N330) 35,00 TBBSe 0.70 Total 144,95 fs TBBS or N-tert-butylbenzothiazole-2-sulfenamide In accordance with| 1S0 6472. This shall be supplied in powder form having an initial insoluble- matter content, inaccordance with I$0 11235, ofless than 0,3 %. The material shall be stored at room temperature in a closed container and insoluble| matter shall be checked every 6 months. If this is found to exceed 0,75 %, the material shall be discarded. TBBS may be purified by reprocessing, Jeg. by recrystallization; the procedure for this is beyond the scope of this [document. 2 © 150.2019 ~ Allrights reservedBS ISO 2303:2019 ISO 2303:2019(E) 6.2 Procedure 6.2.1 Equipmentand procedure Equipment and procedure for the prepar: 180 2393, ‘ion, mixing and vulcanization shall be in accordance with 6.2.2 Mill mixing procedures 6.2.24 General ‘Two mill mixing procedures are specified: methods A and B. The mixing time is shorter in Method B than in Method A. ‘The two methods do not necessarily give identical results, In laboratory cross-checks or in a series of evaluations, the same procedure shall be used in all cases. In both methods, the standard laboratory mill batch mass, in grams, shall be based on four times the formula mass. The surface temperature of the rolls shall be maintained at 70 °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 in 6.2.2.2 and 6,2.2.3, small adjustments to the mill openings might be necessary. 6.2.2.2. Method A Duration Cumulative time (min) (min) a) Pass the rubber between the mill-rolls twice without banding, with the mill opening set at 05 mm, for approximately 2 min and weigh 2,0 2.0 the rubber; b) Band the rubber with the mill opening set at 1,4 mm and make two» 4 4p 3/4 cuts from each side; NOTE Some types of isoprene rubber go to the back roll, in which case the stearic acid should be added and, after its incorporation, the rubber can usually be transferred to the front roll. In addition, certain tougher types of isoprene rubber might require slightly longer breakdown before the addition of other materials in order to obtain a good rolling bank. ©) Set the mill opening to 1,7 mm and add the stearic acid. Make one 4 6a 3/4 cut from each side; x , d) Add the zinc oxide and the sulfur. Make two 3/4 cuts from each side; 3,0 9,0 @) Add the carbon black evenly across the mill at a uniform rate. When approximately half the black has been incorporated, open the mill to 1,9 mm and make one 3/4 cut from each side, then add the remainder of the carbon black. Be certain to add any black that has dropped into the mill pan. When all the black has been incorporated, make one 3/4 cut from each side; 13,0 22,0 f) Add the TBBS with the mill opening still at 19 mm. Make three 3/4 cuts from each si 3,0 25,0 © 150 2019 All rights reserved 3BS ISO 2303:2019 ISO 2303:2019(E) g) 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 28,0 h)_ Sheet the batch to an approximate thickness of 6 mm and check-weigh the batch (see ISO 2393). If the mass of the batch differs from the theoretical value by more than *{'3 %, discard the batch and re-mi i) Remove sufficient material from the batch for evaluating the vulcanization characteristics in accordance with ISO 6502-1 or ISO 6502-2. Condition this material for 2 h to 24 h, if possible at a standard temperature and humidity as defined in ISO 23529, before testing. j) Sheet the batch to approximately 2,2 mm for preparing test slabs or to the appropriate thickness for preparing ISO ring test pieces in accordance with ISO 37. k) Condition the batch for 2 h to 24h prior to vulcanizing, if possible at a standard temperature and humidity as defined in ISO 23529. 6.2.2.3 Method B Duration Cumulative time (min) (min) a) Pass the rubber between the rolls twice without banding, with the mill opening set at 0,5 mm + 0,1 mm, then band the rubber between 2,0 20 the rolls with the mill opening gradually increased to 1.4mm. b) Add the stearic acid. Make one 3/4 cut from each side, 2,0 4,0 ©) Add the sulfur and the zinc oxide. Make two 3/4 cuts from each side. 3,0 70 ) Add half of the carbon black. Make two 3/4 cuts from each side. 3,0 10,0 ©) Add the remaining half of the carbon black and any black that has dropped into the mill pan. Make three 3/4 cuts from each side. a 15,0 f) Add the TBBS. Make three 3/4 cuts from each side. 30 180 8) Cut the batch from the mill Set the mill opening to 0,5 mm £0,1mm 9 4 wo and pass the rolled batch endwise through the rolls six times. h) Sheet the batch to an approximate thickness of 6 mm and check-weigh the batch (see ISO 2393). If the mass of the batch differs from the theoretical value by more than *1'3 %, discard the batch and re-mix. i) Remove sufficient material from the batch for evaluating the vulcanization characteristics in accordance with ISO 6502-1 or ISO 6502-2. Condition this material for 2 h to 24 h, if possible at a standard temperature and humidity as defined in ISO 23529, before testing, j) Sheet the batch to approximately 2,2 mm for preparing test slabs or to the appropriate thickness for preparing ISO ring test pieces in accordance with ISO 37. 1) Condition the batch for 2 h to 24 h prior to vulcanizing, if possible at a standard temperature and humidity as defined in ISO 23529. 4 © 150 2019 ~ All rights reservedBS ISO 2303:2019 ISO 2303:2019(E) 6.2.3. Laboratory internal mixer (LIM) mixing procedure 6.2.3.1 General For a LIM having a nominal mixing capacity of 65 cm3 to about 2 000 cm3, the batch mass shall be equal to the nominal mixer capacity, in cubic centimetres, multiplied by the compound density. The LIM conditions shall be the same for each batch mixed during the preparation of a series of identical mixes. At the beginning of each series of test mixes, a machine-conditioning batch shall be mixed using the same formulation as the mixes under test. The LIM shall be allowed to cool down to 60°C between the end of one test batch and the start of the next. Temperature control settings shall not be altered during the mixing of a series of test batches. 6.2.3.2 Single-stage mixing procedure ‘The mixing technique shall be such as to obtain a good dispersion of all the ingredients. The final temperature of the batch discharged after mixing shall not exceed 120 °C. If necessary, adjust the batch mass, head temperature and/or rotor speed so that this condition is met. NOTE 1 Compounding materials other than rubber, carbon black and oil can be added to LIM batches more precisely and with greater ease if they are previously blended together in the proportions required by the formulation, Such blends can be made using a mortar and pestle, by mixing for 10 min in a biconical blender with the intensifier bar turning, or by mixing in a blender for five 3 s periods and scraping the inside ofthe blender to dislodge materials stuck to the sides after each 3 5 mix. A Waring blender!) has been found suitable for this method. Caution: if mixed longer than 3 s, the stearic acid might melt and prevent good dispersion. NOTE2 —Anexample of a mixing procedure for a LIM is as follows: Duration Cumulative time (min) (min) a) Load the rubber, lower the ram and allow the rubber to be masticated. 10 1,0 b) Raise the ram and add the pre-blended zinc oxide, sulfur, stearic acid and ‘TBBS, taking care to avoid any loss. Then add the carbon black, sweep the 1,0 20 orifice and lower the ram, 9) Allow the batch to mix. 70 90 d) Turn offthe motor, raise the ram, remove the mixing chamber and discharge the batch. Record the maximum, batch temperature. 6) After discharging the mixed batch, pass it through a mill set at 70°C +5 °C once ata 0,5 mm mill opening, and then twice ara 0,3 mm mill opening f) Sheet the batch to an approximate thickness of 6 mm and check-weigh the batch (see ISO 2393). If the mass of the batch difers from the theoretical value by more than 96, discard the batch and re-mix, adi Bigeyeaten anol Yon te bled acenthalbante vifenilnaion shomesielitondroncmmbane ‘with 150 6502-1 or ISO 6502-2. Condition this material for 2 h to 24h, if possible at a standard temperature and humidity as defined in ISO 23529, before testing. h) Sheet the batch to approximately 2,2 mm for preparing test slabs or to the appropriate thickness for preparing ISO ring test pieces in accordance with ISO 37. 1) Condition the batch for 2 h to 24h prior to vulcanizing, if possible at a standard temperature and humidity as defined in ISO 23529. 1) Thisis an example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by 1S0 of this product. © 150 2019 All rights reserved 5BS ISO 2303:2019 ISO 2303:2019(E) 6.2.3.3 Two-stage mixing including mill for final mixing procedure 6.2.3.3.1 General ‘The LIM shall be allowed to cool down to 60 °C between the end of one test batch and the start of the next. 62.3.3.2 Stage 1— Initial mixing stage The mixing technique shall be such as to obtain a good dispersion of all the ingredients. The final temperature of the batch discharged after mixing shall be between 150 °C and 170 °C. If necessary, adjust the batch mass, head temperature and/or rotor speed so that this condition is met. NOTE — Anexample of a mixing procedure for the initial mixii 1g is as follows: Duration Cumulative time (min) (min) a) Adjust the temperature of the LIM to a starting temperature of 60 °C + 3 °C. Close the discharge door, set the rotor speed to 77 rpm, start the rotorsand = — ~ raise the ram, ¥) Load half of the rubber, all the carbon black, zinc oxide and stearicacid, then 5 os the remaining half of the rubber. Lower the ram. : i Allow the batch to mix. 30 35 4) Raise the ram and clean the mixer throat and the top ofthe ram. Lower g¢ 40 ©) Allow the batch to mix. 0s 4s A) Discharge the batch, 15 60 g) After discharging the batch, immediately check the temperature of the batch with a suitable measuring device. Ifthe temperature as measured falls outside the range 150 °C to 170°C, discard the batch. 1h) Pass the batch three times through a mill with a mill opening of 2,5 mm and a temperature of 70 °C «5 °C. i) Sheet the batch to an approximate thickness of 10 mm and check-weigh the batch (see [SO 2393). Ifthe mass ofthe batch differs from the theoretical value by more than *25 9, discard the batch and re-mix j) Leave the batch for at least 30 min and up to 24 h, if possible at a standard temperature and humidity as defined in 150 23529. ‘The smaller LIMs do not provide enough compound for the final mill mixing, as a batch mass of three times the formula mass is required. In these cases, the LIM may be used for the final mixing. The head temperature and/or the batch mass may be adjusted so that the final temperature of the discharged batch does not exceed 120 °C. 6.2.3.3.3 Stage 2— Final mixing stage Rest the batch for at least 30 min, or until it reaches room temperature, before proceeding with the final mixing stage. The mixing technique shall be such as to obtain a good dispersion of all the ingredients, ‘The final temperature of the batch discharged after mixing shall not exceed 120 °C. When a LIM is used, adjust, if necessary, the batch mass, the head temperature and/or the rotor speed so that this condition is met. When mill mixing is used, set the surface temperature of the rolls to 70 °C 5 °C and maintain it at this temperature during mixing. The standard laboratory mill batch 6 © 150.2019 ~ Allrights reservedBS ISO 2303:2019 ISO 2303:2019(E) ‘mass, in grams, shall be based on two times the formula mass. A good rolling bank at the nip of the rolls shall be maintained during mixing. If this is not obtained with the nip settings given hereunder, small adjustments to the mill openings may be necessary. NOTE1 An example ofa LIM mixing procedure for the final mixing stage is as follows: 9 f) a) 4) Duration Cumulative time (min) (min) Close the discharge door, set the rotor speed and raise the ram, - - Load the rubber, the sulfur and the accelerator, and lower the ram. 045 05 Allow the batch to mix. 45 20 Raise the ram, open the mixing chamber and discharge the batch. Record 4 5 a8 the maximum batch temperature. M After discharging the mixed batch, pass it four times through a mill ata roll g 5 46 ‘temperature of 70 °C + 5 °C and with a mill opening of 0,8 mm, " Sheet the batch to an approximate thickness of 6 mm and check-weigh the batch (see ISO 2393). Ifthe mass ofthe batch differs from the theoretical value by more than 96, discard the batch and re Remove sufficient material from the batch for evaluating the vulcanization characteristics in accordance with 10 6502-1 or ISO 6502-2. Condition this material for 2 h to 24h, if possible at a standard temperature and humidity as defined in ISO 23529, before testing, Sheet the batch to approximately 2,2 mm for preparing test slabs or to the appropriate thickness for preparing ISO ring test pieces in accordance with ISO 37. Condition the batch for 2 h to 24 h prior to vulcanizing, if possible at a standard temperature and humidity as defined in ISO 23529, NOTE2 Anexample ofa mill mixing procedure for the final mixing is as follows: ») a a) 2 f) Duration Cumulative time (min) (min) Set the mill temperature at 70°C 5 °C and the mill opening to 1,9 mm. Band ‘the masterbatch on the slow roll ‘Add the accelerators. Do not cut the band until the accelerators are completely dispersed. Then make three 3/4 cuts from each side. 3.0 30 Add the sulfur. Do not cut the band until the sulfur is completely dispersed. ‘Then make three 3/4 cuts from each side. 3.0 60 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 from each end alternately. 20 80 Set the mill opening at approximately 6 mm and pass the rolled batch endwise through the rolls six times, introducing it from each end alternately. Sheet the batch. 10 90 Check-weigh the batch (see ISO 2393). If the mass of the batch differs from the theoretical value by more than £72 %, discard the batch and re-mix. © 150 2019 All rights reserved 7BS ISO 2303:2019 ISO 2303:2019(E) 4g) Remove sufficient material from the batch for evaluating the vulcanization characteristics in accordance with 1S0 6502-1 or ISO 6502-2. Condition this material for 2 h to 24 h, if possible at a standard temperature and humidity as defined in ISO 23529, before testing, h) Sheet the batch to approximately 2,2 mm for preparing test slabs or to the appropriate thickness for preparing ISO ring test pieces in accordance with ISO 37. 1) Condition the batch for 2 h to 24 h prior to vulcanizing, if possible at a standard temperature and humidity as defined in ISO 23529, 7 Evaluation of vulcanization characteristics by a curemeter test WARNING — Formation of nitrosamines is possible during the cure. 7.1. Using an oscillating-disc curemeter Measure the following standard test parameters: ‘My, My at defined time, ts1,t'c (50) and t(90) in accordance with ISO 6502-2, using the following test conditions: — oscillation frequency: 1,7 Hz. (100 cycles per minute); — amplitude of oscillation: 1P of arc; — selectivity: to be chosen to give at least 75 % of full-scale deflection at My (note that with some rubbers, 75 % might not be attainable); — die temperature: 160°C +0,3° — pre-heat time: none. 7.2 Usinga rotorless curemeter Measure the following standard test parameters: A, Fiat defined time, t/(50) and t'<(90) in accordance with ISO 6502-1, using the following test conditions: — oscillation frequency: 1,7 Hz (100 cycles per minute); — amplitude of oscillation; 05° of are; — selectivity: to be chosen to give at least 75 % of full-scale deflection at Fy (note that with some rubbers, 75 % might not be attainable); — die temperature: 160°C + 0,3 °C; — pre-heat time: none. 8 Evaluation of tensile stress-strain properties of vulcanized test mixes Vulcanize sheets at 135 °C for three periods chosen from a cure series of 20 min, 30 min, 40 min and 60 min. 8 © 150 2019 Allright reservedBS ISO 2303:2019 ISO 2303:2019(E) The three 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, as defined in ISO 23529. Measure the stress-strain properties in accordance with ISO 37. 9 Pre n See Annex.A for the information on precision data for both mill mixer and laboratory internal mixer. See Annex B for the information on additional precision data for natural rubber. 10 Test report ‘The test report shalll include the following information: a) areference to this document, ie. ISO 2303:2019;, b) all details necessary for the identification of the sample; the time and temperature conditions used for the Mooney viscosity determination, and whether a massing process was used; @)_ the method used for the volatile-matter content (ISO 248-lor ISO 248-2); €) the method used for the ash determination (Method A or B of ISO 247-1:2018); f) the standard test formulation used; g)_ the reference materials used; h)_ the mixing procedure used; i) the conditioning conditions used in 6.2.2.2, 6.2.2.3, 6.2.3.2 or 6.2.3.3; i) for Clause 7: — the reference standard, — the time for My or Fi: k) the vulcanization periods used in Clause 8; }) any unusual features noted during the determination; m) any operation not included in this document or in the International Standards to which reference is made, as well as any operation regarded as optional; n) the results and the units in which they have been expressed; 0} the date of the test. © 150 2019 ~ Allrights reserved 9BS ISO 2303:2019 ISO 2303:2019(E) Annex A (informative) Precision data for both mill mixer and laboratory internal mixer Al General An interlaboratory test programme (ITP) was carried out using the procedures and guidelines described in ISO/TR 9272. Reference should be made to this Technical Report for other details and for terminology on precision determination. A type 2 (interlaboratory) precision was determined for cure characteristics, using an oscillating- disc curemeter. A sample of isoprene rubber was used in the ITP. Five laboratories participated in a programme using the mill mixing procedure (method A) and eight laboratories in a programme using the two-stage LIM mixing procedure, utilizing a LIM for initial and a mill for final mixing. The test was done on three different days in each laboratory. ‘The precision results as determined from this ITP may not be applied to acceptance or rejection testing of any group of materials or products without documentation that the results of this precision determination actually apply to the materials or products tested. A.2 Results A.2.1 General ‘The results of the precision calculation for repeatability and reproducibility are given in Table A.1 for the mill mixing procedure and Table A.2 for the LIM mixing procedure. A.2.2 Repeatability The repeatability r of the test method has been established as the appropriate value tabulated in Table A.1 or A.2. Two single test results that differ by more than this value should be considered suspect and suggest that some appropriate investigative action be taken. A.2.3 Reproducibility The reproducibility R of the test method has been established as the appropriate value tabulated in ‘Table A.1 or A.2. Two single test results that differ by more than this value should be considered suspect and suggest that some appropriate investigative action be taken. 10 © 180.2019 - Allrights reservedTable A.1 — Precision for mill mixing (method A) BS ISO 2303:2019 ISO 2303:2019(E) Within-laboratory Between laboratories Property Units Mean levela 1 Se r o se kT & Mi, am 6.05) o15 | 040 | 661 | 036 | 101 | 1669 Mu aN 39,87 025 | 069 | 173 | 173 | 486 | 1219 ta min 319 o19_|_053 | 1661 | 0.36 [1.00 | 31.35 (50) min 497 007 | 020 | 402 | o14 | 030 | 785 (90) min 709 oos | 023 [324 [ 010 [ 028 | 395 fy Is the repeatability standard deviation, [+ isthe repeatability, in measurement units; (©) Is the repeatability, in percent (relative); sq Is the reproducibility standard deviation; Je is the reproducibility, in measurement units; (8) is the reproducibility, in percent (relative). 2 Measured at 160 °C, 1,7 Hz, 1° of are — midpoint of range used for (r) and (R) calculations. Table A.2 —Preci jon for two-stage LIM-mill mixing - Within-laboratory Between laboratories Property Units Mean levele Sr r oO Sk R @ Mi aN 6.85 009 | 026 | 380 | 018 | 050 | 7.30 Ma aNm 39,12 oss | 124 | 3a7 [ 1as | 321 | 8.20 ts min 3,82 009 | 026 | 680 | 024 | 066 | 1728 (50) min 6.23 oo7 | 019 | 304 | 045 | 125 | 20,06 (90) min, 847 0,10 0,27 319 044 123 | 14,52 For the meanings of the symbols used for the precision parameters in the column headings, see Table Ad. Js Measured at 160 °C, 1,7 Hz, 1° of are — midpoint of range used for (°) and (R) calculations. © 150 2019 - Allrights reserved uwBS ISO 2303:2019 ISO 2303:2019(E) Additional precision data for natural rubber Annex B (informative) ‘The following precision data for mill mixing (Tables B.1 and B.2) and LIM mixing (Tables B.3 and B.4), obtained natural rubber, have been taken from ISO 1658:2009). They were determined not only for curemeter properties but also for stress-strain properties. The reader is referred to ISO 1658:2009, Annex B, for full details of the ITP and a discussion of the results. Table B.1 — Precision (type 2) — Mill mixing — Stress-strain properties tmeaurea | Meamtevel |r @fr |e) | oratones aga a |S3o0 is the stress (modulus) at 300 % elongation. Table B.2 — Precision (type 2) — Mill mixing — Curemeter properties measured Mean level Z ? o 5 R ® oratories - ; Mu, dN-m 14,70 0,22 0,62 | 4,20 | 1,96 5,50 37,30 4 'e(50), min 3,17 012 0,34 | 10,60 | 0,27 0,75. 23,5 6 Rooney sie | 235 | 687 | 127 | 305 | 108 | 208 5 pe =e = =a For the meanings of the symbols used for the precision parameters in the column headings, see Table Al. 2). Withdrawn, 12 © 150 2019 ~ All rights reservedBS ISO 2303:2019 ISO 2303:2019(E) ‘Table B.3 — Precision (type 2) — LIM mixing — Stress-strain properties Within laboratory Between laboratories _| Nu 7 rarmet_[ Meaney Wabi berson[ sen baratories_[ une th Stoo, MPa 2.55 005 | 013 | 510 | 023 | 064 | 25,2 a S200, MPa 6,69 o1s_| 043 | 640 | 061 | 170 | 25.4 8 S300. MPa 13.0 020 | 056 | 430 | 083 | 233 | 180 8 Elongation at break, % 518 710 | 199 | 380 | 196 | 549 | 106 [Tensile strength, MPa| 29,2 o44 | 1.24 | 420 | 266 | 746 | 25,5 faverage — | — [a [TT — [209 Stoo isthe stress (modulus) at 100 % elongation; Szoo isthe stress (modulus) at 200 % elongation: soo isthe stress (modulus) at 300 % elongation. For the meanings ofthe symbols used for the precision parameters in the column headings, se Table A. Table B.4 — Precision (type 2) — LIM mixit ing — Curemeter properties Parameter Within-laboratory Between laboratories Number of lab- measured Mesileval rl ols R (®) oratories My, dNem 149 0,15 0,41 | 2,80 | 0,81 2,26 15,2 7 [My dN-m_ 1,94 0,06 0,17 | 8,80 | 0,18 049 25,2 8 tsi, min 1,57 0,04 012 | 740 | 0,33 0,91 58,2 9 (50) min 300 | 006 | 017 | 570 | 034 | 095 | au7 7 (00) min 540 | 009 | 026 | 490 | 0.33 | 09s | 173 6 Mooneywiacosty | ssa | az | as7 | 70 | ano | oa2 | 110 8 Average == se [== or the meanings oe sbi ued forthe peo parameters inthe column feadingh see BIT ©0150 2019- sights resered 3BS ISO 2303:2019 ISO 2303:2019(E) i) 2) (3) (4] 14 Bibliography ISO 1658:2009, Natural rubber (NR) — Evaluation procedure 180 6472, Rubber compounding ingredients — Abbreviated terms IS0/TR 9272, Rubber and rubber products — Determination of precision for test method standards 180 11235, Rubber compounding ingredients — Sulfenamide accelerators — Test methods © 150 2019 ~ All rights reservedThis page deliberately left blank