1、BS ISO 19246:2016Rubber compoundingingredients Silica Oilabsorption of precipitated silicaBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 19246:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 19246:2016.The UK partic
2、ipation in its preparation was entrusted to TechnicalCommittee PRI/50, Raw materials (including latex) for use in therubber industry.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisio
3、ns of a contract. Users are responsible for its correctapplication. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 86997 6ICS 83.040.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published und
4、er the authority of theStandards Policy and Strategy Committee on 31 July 2016.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 19246:2016 ISO 2016Rubber compounding ingredients Silica Oil absorption of precipitated silicaIngrdients de mlange du caoutchouc Silice Abso
5、rption dhuile des silices prcipitesINTERNATIONAL STANDARDISO19246First edition2016-07-15Reference numberISO 19246:2016(E)BS ISO 19246:2016ISO 19246:2016(E)ii ISO 2016 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2016, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no
6、 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 below or ISOs membe
7、r body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 19246:2016ISO 19246:2016(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Principle 14 Ma
8、terials . 15 Equipment . 26 Sampling 27 Procedure. 27.1 Preliminary note 27.2 Determination . 37.2.1 Method A (powder sample, micro-perls) . 37.2.2 Method B (granulated samples) . 47.3 Evaluation 47.3.1 Evaluation for powder and micro-perl materials 47.3.2 Evaluation of granulated materials 58 Preci
9、sion data 59 Test report . 5Annex A (normative) Normalization of the mixer chamber by using reference materials . 6Annex B (informative) Precision data 12Bibliography .14 ISO 2016 All rights reserved iiiContents PageBS ISO 19246:2016ISO 19246:2016(E)ForewordISO (the International Organization for St
10、andardization) 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 rig
11、ht 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
12、 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 rul
13、es 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 identi
14、fied 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 on
15、 the meaning of ISO specific terms and expressions related to conformity 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 informationThe committee responsible for this document is IS
16、O/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry.iv ISO 2016 All rights reservedBS ISO 19246:2016ISO 19246:2016(E)IntroductionDue to health and environmental safety precautions, the determination of DOA absorption number has been
17、worked out to substitute the determination of the DBP absorption number.Dibutylphthalate (DBP) and dioctylphthalate (DOP) were commonly used in the past for determining the absorption capacity of pigments and extenders, like carbon black and silica. In the meantime, both substances have been banned
18、as carcinogenic, mutagenic, reprotoxic substances (CMR) in different countries.The search of a suitable alternative for DBP and DOP, especially for measuring the absorption capacity of polar pigments and extenders, like silica, calcium silicates and sodium aluminium silicates has been carried out in
19、 a task group of the Association of Synthetic Amorphous Silica Producers (ASASP) between 2004-2008. Out of different tested liquids, like linseed oil, paraffinic oil, etc., DOA was found as the most suitable alternative which leads to evaluated absorption numbers close to DBP measurement. ISO 2016 A
20、ll rights reserved vBS ISO 19246:2016BS ISO 19246:2016Rubber compounding ingredients Silica Oil absorption of precipitated silica1 ScopeThis International Standard specifies a general method for determining the liquid absorption capacity of a pigment and extender by using di-(2-ethylhexyl) adipate (
21、DOA, CAS 103-23-1). The determination of the DOA absorption number is performed by means of an absorptometer which is equipped with a torque measurement and processing system. The DOA absorption number provides an indication of the void volume formed by the aggregates and agglomerates of the pigment
22、s and extenders.2 Normative referencesThe 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 referenced document (incl
23、uding any amendments) applies.ISO 787-2, General methods of test for pigments and extenders Part 2: Determination of matter volatile at 105 CISO 787-11, General methods of test for pigments and extenders Part 11: Determination of tamped volume and apparent density after tampingISO 15528, Paints, var
24、nishes and raw materials for paints and varnishes Sampling3 PrincipleFor the determination of the DOA absorption number, a defined amount of pigment or extender shall be transferred to the mixer chamber of the absorptometer.Under permanent kneading, DOA shall be added with a constant rate. The indic
25、ation is the torque of the kneaders. While the torque is low at the beginning, it increases rapidly near the point of liquid absorption of the sample and decreases after reaching the maximum torque. The mixture changes from a free-flowing state to one of a pasty consistency.On basis of the raw data
26、torque curve and the settings, a polynom shall be calculated. The value for 70 % of the maximum torque of this third order polynomial (smoothed curve) shall be used for the evaluation of the DOA absorption number.4 Materials4.1 Di-(2-ethylhexyl)adipate (DOA), which density is approximately 0,925 5 g
27、/cm3at 20 C and which refractive index n(D, 20 C) is approximately 1,447.4.2 Pigment or extender, as powder or micro-perls.It can be added directly to the absorptometer chamber. In case of testing granulated materials, the determination is performed using a granular size fraction of between 1,0 mm a
28、nd 3,15 mm, that is received by pre-sieving.INTERNATIONAL STANDARD ISO 19246:2016(E) ISO 2016 All rights reserved 1BS ISO 19246:2016ISO 19246:2016(E)5 Equipment5.1 Absorptometer, with burette and system for measurement, storage and evaluation of torque data of the kneader.The following pieces of equ
29、ipment1)may be used: Absorptometer E, Fa. Brabender, Duisburg (equipped with extended functionality/evaluation unit); Absorptometer C, Fa. Brabender, Duisburg; Hitec DBP-Absorptometer, Fa. Hitec, Luxembourg.5.2 Beaker.5.3 Sieves, one with mesh width of 1,0 mm, another one with mesh width of 3,15 mm.
30、5.4 Sieve pan.5.5 Plastic or soft metal spatula and brush, for cleaning the kneading chamber.5.6 Precision balance, accuracy of 0,01 g.5.7 Oven, capable of being maintained at 105 C 2 C.6 SamplingTake a representative sample of the material to be tested according to ISO 15528.7 Procedure7.1 Prelimin
31、ary note7.1.1 The following most important factors which affect the determination shall be pointed out.a) Pore volume: the porosity of the material is the real cause for the absorption of liquid.b) Moisture content: as the moisture content increases, the absorptive capacity decreases.c) Particle siz
32、e: at the same material family but different degree of milling, the particle size can influence the DOA absorption. This is to take into account for comparison. In case of extremely fine milled samples, an overload with DOA in connection with inhomogeneity of the mixture can occur that results in in
33、correct values.d) Sample weight: with increasing sample weight, the specific DOA absorption number decreases.7.1.2 Carry out the determination in duplicate.7.1.3 To avoid erroneous results, check the feeding pipe before starting the measurement. It shall be free of air bubbles. If necessary, the pip
34、e shall be purged and the burette refilled.1) Examples of suitable products available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of these products.2 ISO 2016 All rights reservedBS ISO 19246:2016ISO 19246:2016(E)
35、7.1.4 The following settings should be used in the program.7.1.4.1 Measurement settings Dosing rate (burette): 4,0 ml/min; Rotation speed First blade: 125 min-1; Second blade: 250 min-1; Temperature: 23 C.The temperature of 23 C in the settings should be used as a target value. Actually, the tempera
36、ture during the measurement should be in a range of 23 C 5 C.7.1.4.2 Evaluationa) Test end Threshold: 100 mNm; End time: 40 s after maximum; Torque limit: 10 000 mNm.b) Polynom Start percent: 50 % of maximum torque; End time: 20 s after maximum.7.1.5 The evaluation of the aging status of the absorpt
37、ometer shall be done according to Annex A.7.2 Determination7.2.1 Method A (powder sample, micro-perls)7.2.1.1 The loss on drying of the sample material should not exceed 10 %. Material with a higher content of moisture should be dried to a lower value.7.2.1.2 Weigh 12,50 g 0,02 g of the sample mater
38、ial by means of a precision balance (5.6) into a beaker (see 5.2), transfer to the kneader chamber and enter the sample weight into the program.A sample weight of 12,5 g represents an optimum for most silica or silicates. It is advisable to use an integrated or separated funnel for filling the knead
39、er chamber during the operation of the absorptometer. This allows also in case of material with lower tamped density (300 g/l), it is recommended to use a higher sample amount (preferably 20,0 g) to achieve a sufficient filling of the kneader chamber and repeatable measurements.The tamped density sh
40、all be measured according to ISO 787-11.Ideally, the sample amount should be designed to fill the kneader chamber sufficiently. It should neither be worked with too low sample amount (there is no sufficient increase of torque), nor the chamber ISO 2016 All rights reserved 3BS ISO 19246:2016ISO 19246
41、:2016(E)should be overfilled, that does not ensure a sufficient mixing of the sample. Any deviation of the sample weight of 12,5 g shall be documented in the test report.7.2.1.3 Close the safety device of the equipment, bring the feeding pipe into position and start the determination.7.2.1.4 After t
42、he determination is ended, read the DOA absorption (based on original substance) as expressed as the 70 % value of the maximum torque from the measurement report.During the determination, however, in the range of the maximum DOA absorption, the observable silica-DOA-mixture forms a paste, that is in
43、dicated in the increase of the torque. After reaching the torque maximum, the torque decreases to lower values. The DOA absorption number based on original substance in ml/100 g is the consumption of DOA related to the sample amount at 70 % of the maximum torque of the polynom. This polynom curve is
44、 calculated automatically at the end of the determination based on the settings (see 7.1.3) using the raw data of the measured torque curve.7.2.1.5 Refill the burette, if there is no automatic refilling mode, and clean the mixing chamber and kneader blades carefully. The DOA sample mixture is dispos
45、ed conveniently, considering legal restrictions.The DOA-sample mixture may cause difficulties during cleaning. In this case, it is recommended to add some portion of a silica powder, switch on the kneader only for a short time and then dismount the mixing chamber for cleaning.7.2.2 Method B (granula
46、ted samples)7.2.2.1 Prepare a granular size fraction of between 1,0 mm and 3,15 mm by means of the appropriate sieves (5.3).7.2.2.2 The further determination shall be carried out according to method A.7.3 Evaluation7.3.1 Evaluation for powder and micro-perl materialsThe result of the determination c
47、an be given as DOA absorption based on original substance or optional as moisture corrected DOA absorption, as based on dried substance. This result shall be specified in the test report.The calculation of the DOA absorption number based on dried substance can be calculated on the basis of Formulae
48、(1) and (2) and is given without decimal place.DOADOA porig dry= (1)andpLOD=100100(2)where4 ISO 2016 All rights reservedBS ISO 19246:2016ISO 19246:2016(E)DOAorigis the DOA absorption based on original substance, in ml/100 g;DOAdryis the DOA absorption number based on dry substance, in ml/100 g;p is
49、the correction factor;LOD is the loss on drying (2 h at 105 C), in %.The loss on drying (2 h at 105 C) shall be determined separately according to ISO 787-2.7.3.2 Evaluation of granulated materialsThe result of the determination is the DOA absorption number based on original substance that is given without decimal place.8 Precision dataSee Annex B.9 Test reportThe test report shall include the following information:a) a reference to this International Standard, i.e. ISO 19246:2016;b) all detai
