1、BSI Standards Publication PD ISO/TS 16095:2014 Reclaimed rubber derived from products containing mainly natural rubber Evaluation procedurePD ISO/TS 16095:2014 PUBLISHED DOCUMENT National foreword This Published Document is the UK implementation of ISO/TS 16095:2014. The UK participation in its prep
2、aration was entrusted to Technical Committee PRI/50, Rubber - Raw, natural and synthetic, including latex and carbon black. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of
3、a contract. Users are responsible for its correct application. The British Standards Institution 2014. Published by BSI Standards Limited 2014 ISBN 978 0 580 80801 2 ICS 83.040.10 Compliance with a British Standard cannot confer immunity from legal obligations. This Published Document was published
4、under the authority of the Standards Policy and Strategy Committee on 30 April 2014. Amendments issued since publication Date Text affectedPD ISO/TS 16095:2014 ISO 2014 Reclaimed rubber derived from products containing mainly natural rubber Evaluation procedure Caoutchouc rgnr driv principalement de
5、 produits contenant du caoutchouc naturel Mthode dvaluation TECHNICAL SPECIFICATION ISO/TS 16095 First edition 2014-04-01 Reference number ISO/TS 16095:2014(E)PD ISO/TS 16095:2014ISO/TS 16095:2014(E)ii ISO 2014 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2014 All rights reserved. Unless oth
6、erwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
7、 below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in SwitzerlandPD ISO/TS 16095:2014ISO/TS 16095:2014(E) ISO 2014 All rights reserved iii Co
8、ntents Page Foreword iv 1 Scope . 1 2 Normative references 1 3 Sampling and sample preparation 1 4 Physical and chemical tests on raw rubber 2 4.1 Mooney viscosity . 2 4.2 Acetone extract . 2 4.3 Ash . 2 4.4 Carbon black . 2 4.5 Rubber content . 2 5 Preparation of test mix for evaluation . 2 5.1 Sta
9、ndard test formulation . 2 5.2 Mixing procedure Mixing with a laboratory mill . 3 6 Evaluation of vulcanization characteristics by a curemeter test . 4 6.1 Using an oscillating disc curemeter 4 6.2 Using a rotorless curemeter 5 7 Evaluation of Mooney viscosity of test mixes 5 8 Evaluation of tensile
10、 stress-strain properties of vulcanized test mixes .5 9 Evaluation of Shore hardness of vulcanized test mixes . 5 10 Test report . 6PD ISO/TS 16095:2014ISO/TS 16095:2014(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO m
11、ember 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, governm
12、ental 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 maintenan
13、ce 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). Attentio
14、n 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 an
15、d/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 on the meaning of ISO specific terms and expressions related to conformity
16、 assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information. The committee responsible for this document is ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials
17、(including latex) for use in the rubber industry. NOTE 1 ISO/TC 45/SC 3 decided to publish a Technical Specification, because the result of the interlaboratory test procedure (ITP) to validate the evaluation procedure on reclaimed natural rubber may be dubious. NOTE 2 If the result of this ITP shows
18、 that the procedure is reproductible and reproducible, then this Technical Specification will be converted into International Standard.iv ISO 2014 All rights reservedPD ISO/TS 16095:2014TECHNICAL SPECIFICATION ISO/TS 16095:2014(E) Reclaimed rubber derived from products containing mainly natural rubb
19、er Evaluation procedure 1 Scope This Technical Specification defines the physical and chemical tests on raw reclaimed natural rubber, and the standard materials, standard test formulations, equipment, and processing methods for evaluating the vulcanization characteristics, and the mechanical propert
20、ies of reclaimed natural rubber. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referen
21、ced document (including any amendments) applies. ISO 37, Rubber, vulcanized or thermoplastic Determination of tensile stress-strain properties ISO 247:2006, Rubber Determination of ash ISO 289-1, Rubber, unvulcanized Determinations using a shearing-disc viscometer Part 1: Determination of Mooney vis
22、cosity ISO 1407:2011, Rubber Determination of solvent extract ISO 1408:1995, Rubber Determination of carbon black content Pyrolytic and chemical degradation methods ISO 1795, Rubber, raw natural and raw synthetic Sampling and further preparative procedures ISO 2393, Rubber test mixes Preparation, mi
23、xing and vulcanization Equipment and procedures ISO 3417, Rubber Measurement of vulcanization characteristics with the oscillating disc curemeter ISO 6502, Rubber Guide to the use of curemeters ISO 7619-1, Rubber, vulcanized or thermoplastic Determination of indentation hardness Part 1: Durometer me
24、thod (Shore hardness) ISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods ASTM D297-13, Standard Test Methods for Rubber Products Chemical Analysis 3 Sampling and sample preparation 3.1 Take a laboratory sample of approximately 1,5 kg by the meth
25、od described in ISO 1795. 3.2 Prepare the test sample in accordance with ISO 1795. ISO 2014 All rights reserved 1PD ISO/TS 16095:2014ISO/TS 16095:2014(E) 4 Physical and chemical tests on raw rubber 4.1 Mooney viscosity Determine the Mooney viscosity in accordance with ISO 289-1 on a test piece prepa
26、red as indicated in 3.2. Record the result as ML(1 + 4) at 100 C. 4.2 Acetone extract Determine the acetone extract in accordance with method A or method B of ISO 1407:2011. 4.3 Ash Determine the ash content in accordance with method A of ISO 247:2006. 4.4 Carbon black Determine the carbon black con
27、tent in accordance with ISO 1408:1995, Method A. 4.5 Rubber content Determine the rubber content, R (in %), in accordance with ASTM D297-13, Part A, Clauses 11, 12, and 13. R = 100 (a + b + c) (1) where a is the carbon black content, in percent (%); b is the ash content, in percent (%); c is the ace
28、tone extract, in percent (%). 5 Preparation of test mix for evaluation 5.1 Standard test formulation The standard test formulation for evaluation of reclaimed natural rubber is given in Table 1. The materials used shall be national or International Standard reference materials. If no standard refere
29、nce material is available, the materials to be used shall be agreed between the interested parties.2 ISO 2014 All rights reservedPD ISO/TS 16095:2014ISO/TS 16095:2014(E) Table 1 Standard test formulation Material Parts by mass Reclaimed natural rubber 100,00 + x + y + z Stearic acid a 2,00 Zinc oxid
30、e a 5,00 Sulfur a 3,00 Mercaptobenzothiazole (MBT) 0,50 Diphenyl guanidine (DPG) 0,20 Total 110,70 + x + y + z NOTE 1 x is the number of parts of carbon black to 100 parts of rubber in reclaimed natural rubber. NOTE 2 y is the number of parts of acetone extract to 100 parts of rubber in reclaimed na
31、tural rubber. NOTE 3 z is the number of parts of ash to 100 parts of rubber in reclaimed natural rubber. aPowder materials are used (standard curing ingredients used in the industry). 5.2 Mixing procedure Mixing with a laboratory mill The standard laboratory mill-batch mass, in g, shall be enough to
32、 form proper rolling band. The surface temperature of the rolls shall be maintained at 40 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 to the mill openi
33、ngs might be necessary. A mill batch mass based on two times the formulation mass can also be used. But in this case, more adjustment to the mill openings will be necessary. a) Weigh accurately natural reclaimed rubber to the nearest 1 mg. b) Weigh accurately activators and curatives, to the nearest
34、 0,02 mg, according to the test recipe given above in proportion to the amount of reclaim used. Duration min Cumulative time min c) Band the reclaimed rubber with the mill opening set at 1,2 mm. 1,0 1,0 d) Add the zinc oxide and stearic acid across the mill rolls at a uniform rate. When all the zinc
35、 oxide and stearic acid have been incorporated, make a 3/4 cut from each side. Do not cut the batch while powder is evident in the bank or on the mill- ing surface. Be certain to return to the batch any materials that drop through the mill. 1,0 2,0 e) Add the MBT across the mill rolls at a uniform r
36、ate. When all the powder has been incorporated, make a 3/4 cut from each side. 1,0 3,0 f) Add the DPG across the mill rolls at a uniform rate. When all the pow- der has been incorporated, make a 3/4 cut from each side. 1,0 4,0 g) Add the sulfur across the mill rolls at a uniform rate. When all the s
37、ulfur has been incorporated, make a 3/4 cut from each side. 1,0 5,0 ISO 2014 All rights reserved 3PD ISO/TS 16095:2014ISO/TS 16095:2014(E) h) Cut the batch from the mill and take off the mill rolls. 2,0 7,0 i) Set the mill opening to 1,2 mm and pass the rolled batch endwise through the mill six time
38、s. 3,0 10,0 Total time 10,0 j) Sheet the batch in grain direction 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 +0,5 % or -1,5 %, discard the batch and re-mix. k) Remove sufficient material for c
39、uremeter testing. l) Sheet the batch in grain direction to approximately 2,2 mm for preparing test slabs or to the appropriate thickness for preparing ISO ring or dumbbell test pieces in accordance with ISO 37. m) After mixing, condition the batch for at least 2 h, but not more than 24 h, if possibl
40、e at standard laboratory temperature and humidity as defined in ISO 23529. Mould the slab at 140 C for 20 min. For buttons over 6 mm, 2 min extra time can be added. NOTE For very low Mooney viscosity reclaim rubber, tendency of reclaim sticking to the roll can be observed. Hence, cutting as mentione
41、d in the procedure might not be possible. In such case, scraper blade as shown in Figure 1 can be used. After scraping the material each time, it should be folded two times and passed through mill again to ensure proper blending of chemical. a Key a scraper blade Figure 1 Example of scraper blade 6
42、Evaluation of vulcanization characteristics by a curemeter test 6.1 Using an oscillating disc curemeter Measure the following standard test parameters: M L , M Hat defined time, t s1 , t c (50), t c (90), and t c (95)4 ISO 2014 All rights reservedPD ISO/TS 16095:2014ISO/TS 16095:2014(E) in accordanc
43、e with ISO 3417, using the following test conditions: oscillation frequency: 1,7 Hz (100 cycles per minute); amplitude of oscillation: 1 of arc (An amplitude of oscillation of 3 of arc is permitted as an alternative. If such an amplitude is chosen, measure t s2instead of t s1 .); torque range: to be
44、 chosen to give at least 75 % of full-scale deflection at M H ; die temperature: trials to be done at 140 C 0,3 C; pre-heat time: none. 6.2 Using a rotorless curemeter Measure the following standard test parameters: F L , F maxat defined time, t s1 , t c (50), t c (90), and t c (95) in accordance wi
45、th ISO 6502, using the following test conditions: oscillation frequency: 1,7 Hz (100 cycles per minute); amplitude of oscillation: 0,5 of arc (An amplitude of oscillation of 1 of arc is permitted as an alternative. If such an amplitude is chosen, measure t s2instead of t s1 .); torque range: to be c
46、hosen to give at least 75 % of full-scale deflection at F max ; die temperature: 140 C 0,3 C; pre-heat time: none. The two types of curemeter might not give identical results. 7 Evaluation of Mooney viscosity of test mixes Determine the Mooney viscosity in accordance with ISO 289-1. Record the resul
47、t as ML(1 + 4) at 100 C. 8 Evaluation of tensile stress-strain properties of vulcanized test mixes WARNING Formation of nitrosamines is possible during the cure. Vulcanize sheets at 140 C for 20 min. Condition the vulcanized sheets/buttons for 16 h to 96 h at a standard laboratory temperature and, i
48、f possible, at a standard laboratory humidity as defined in ISO 23529. Measure the stress-strain properties in accordance with ISO 37. 9 Evaluation of Shore hardness of vulcanized test mixes Measure the Shore hardness using durometers with the A-scale for rubbers in the normal hardness range in acco
49、rdance with ISO 7619-1. ISO 2014 All rights reserved 5PD ISO/TS 16095:2014ISO/TS 16095:2014(E) 10 Test report The test report shall include the following: a) a reference to this Technical Specification (i.e. ISO/TS 16095:2014); b) all details necessary for the identification of the sample; c) the method used for the ash determination (method A of ISO 247:2006); d) the method used for the acetone extract determination (method A or method B of ISO
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