1、BS ISO 1304:2016Rubber compoundingingredients Carbon black Determination of iodineadsorption numberBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 1304:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 1304:2016. It su
2、persedes BS ISO 1304:2006 which is withdrawn. The UK participation 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 public
3、ation does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2016. Published by BSI Standards Limited 2016ISBN 978 0 580 89099 4ICS 83.040.20Compliance with a British Standard cannot confer immunity f
4、romlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 October 2016.Amendments/corrigenda issued since publicationDate Text affectedBS ISO 1304:2016 ISO 2016Rubber compounding ingredients Carbon black Determination of iodine a
5、dsorption numberIngrdients de mlange du caoutchouc Noir de carbone Dtermination de lindice dadsorption diodeINTERNATIONAL STANDARDISO1304Fifth edition2016-10-15Reference numberISO 1304:2016(E)BS ISO 1304:2016ISO 1304:2016(E)ii ISO 2016 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2016, Publis
6、hed in SwitzerlandAll rights reserved. Unless otherwise 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. Permissio
7、n can be requested from either ISO at the address below or ISOs member 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 1304:2016ISO 1304:2016(E)Foreword i
8、v1 Scope . 12 Normative references 13 Principle 14 Apparatus . 25 Reagents 36 Preparation of solutions . 37 Standardization of the solutions 67.1 General . 67.2 Sodium thiosulfate solution . 67.3 Iodine solution 78 Procedure. 88.1 Conditions of test 88.2 Sample preparation 88.3 Iodine number determi
9、nation . 89 Expression of results 910 Verification using standard reference blacks1011 Test report 10Annex A (informative) Precision 11Annex B (informative) CAS numbers of reagents .13Bibliography .14 ISO 2016 All rights reserved iiiContents PageBS ISO 1304:2016ISO 1304:2016(E)ForewordISO (the Inter
10、national 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
11、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 st
12、andardization.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 accor
13、dance 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
14、 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 endor
15、sement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html.
16、The committee responsible for this document is ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry.This fifth edition cancels and replaces the fourth edition (ISO 1304:2006), which has been technically revised with the following ch
17、anges: Clause 2 “Normative references” has been updated; the preferred method is stated in the scope and in 7.2.5; 4.1 (analytical balance) and 4.12 (desiccator) have been updated; the tolerance of the weighting in 6.1.5 has been modified to 0,01 g; the precision data have been moved to an informati
18、ve annex.iv ISO 2016 All rights reservedBS ISO 1304:2016INTERNATIONAL STANDARD ISO 1304:2016(E)Rubber compounding ingredients Carbon black Determination of iodine adsorption numberWARNING Persons using this International Standard should be familiar with normal laboratory practice. This International
19、 Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.1 ScopeThis International Standard specifies m
20、ethods for the determination of iodine adsorption number of carbon blacks for use in the rubber industry. Two titration methods are described: method A: titration using a burette and starch as indicator; method B: potentiometric titration with an automatic titrator.The iodine adsorption number is re
21、lated to the surface area of a carbon black and is generally in agreement with the nitrogen surface area. However, it is significantly depressed in the presence of a high content of volatile or solvent-extractable materials; the iodine adsorption number therefore does not always provide a measure of
22、 the specific surface area of a carbon black. Ageing of carbon black can also influence the iodine number.In case of dispute, the preferred method is method B (potentiometric titration).2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document an
23、d are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 385, Laboratory glassware BurettesISO 648, Laboratory glassware Single-volume pipettesISO 1042,
24、Laboratory glassware One-mark volumetric flasksISO 1126, Rubber compounding ingredients Carbon black Determination of loss on heating3 PrincipleA test portion of carbon black is dried, weighed and mixed vigorously with a measured volume of standard iodine solution. The mixture is then centrifuged. A
25、 measured volume of the clear iodine solution is titrated with a standard solution of sodium thiosulfate. From this titration value and the mass of the test portion, the iodine adsorption number of the carbon black is calculated. ISO 2016 All rights reserved 1BS ISO 1304:2016ISO 1304:2016(E)4 Appara
26、tusOrdinary laboratory equipment (beakers, funnels, porcelain spoon, weighing bottles, etc.), plus the following:4.1 Analytical balance, with sensitivities:a) 0,01 g (for 6.1.5 and 7.3.5);b) 0,1 mg (for other paragraphs).4.2 Oven, preferably of the gravity-convection type, capable of temperature reg
27、ulation to within 1 C at 125 C and temperature uniformity to within 5 C.4.3 Stoppered one-mark volumetric flasks, preferably class A in accordance with ISO 1042, of capacities:a) 2 000 cm3, with a tolerance of 0,60 cm3;b) 1 000 cm3, with a tolerance of 0,40 cm3.4.4 Repetitive dispenser, 25 cm3capaci
28、ty, calibrated to within 0,03 cm3accuracy, or one-mark pipettes, high precision, of capacities:a) 20 cm3, with a tolerance of 0,03 cm3;b) 25 cm3, with a tolerance of 0,03 cm3.If class A pipettes in accordance with ISO 648 are used, no calibration is necessary. In other cases, pipettes shall be calib
29、rated to the nearest 0,01 cm3with distilled water, a temperature correction being made if necessary to show the true delivery at any volume used to within 0,01 cm3. The true delivered volume is the read volume plus (or minus) the calibration correction at that volume. For high-precision volume deter
30、mination (see 7.2.2, 7.3.2, 8.3.3, 8.3.6 and 8.3.8), it is recommended that the 20 cm3and 25 cm3pipettes have calibration corrections of the same magnitude and in the same sense.4.5 Digital burettes, with 0,01 cm3increment counter and zero-reset control, calibrated to within 0,05 cm3accuracy, or bur
31、ettes (for method A only), high precision, side-arm filling, graduated in 0,05 cm3and with automatic zero, of capacities:a) 25 cm3, with a tolerance of 0,05 cm3;b) 50 cm3, with a tolerance of 0,05 cm3.If class A burettes in accordance with ISO 385 are used, no calibration is necessary. In other case
32、s, burettes shall be calibrated to the nearest 0,01 cm3with distilled water, a temperature correction being made if necessary to show the true delivery at any volume used to within 0,01 cm3. The true delivered volume is the read volume plus (or minus) the calibration correction at that volume.4.6 St
33、oppered bottles, with ground-glass stoppers, of capacities 250 cm3and 500 cm3.4.7 Glass bottle, with ground-glass stopper, of capacity 2 000 cm3.4.8 Amber-glass bottles, with ground-glass stoppers, of capacities 1 000 cm3and 2 000 cm3.2 ISO 2016 All rights reservedBS ISO 1304:2016ISO 1304:2016(E)4.9
34、 Centrifuge tubes, of capacity 50 cm3, with screw cap and polyethylene liner.Cork, rubber or metal stoppers shall not be used.4.10 Mechanical shaker, capable of 240 strokes/min, with 25 mm stroke length.4.11 Centrifuge, minimum speed 105 rad/s (1 000 r/min).4.12 Desiccator, with silica gel as desicc
35、ant.4.13 Magnetic stirrers and spin bars.4.14 Automatic titrator (for method B only), equipped with a combined electrode for potentiometric titration.5 ReagentsUnless otherwise stated, all chemicals shall be of reagent grade.5.1 Water, deionized or distilled.5.2 Iodine (I2).5.3 Potassium iodide (KI)
36、.5.4 Potassium iodate (KIO3).5.5 Sodium thiosulfate pentahydrate (Na2S2O35H2O).5.6 n-Amyl alcohol (C5H11OH).5.7 Sulfuric acid (H2SO4), mass fraction 98 %, = 1,84 Mg/m3.5.8 Soluble starch (for method A only).5.9 Salicylic acid (C7H6O3) (for method A only).6 Preparation of solutions6.1 Iodine solution
37、, 0,023 64 mol/dm3(0,047 28 N), containing 9,5 parts of potassium iodide to 1 part of iodine.NOTE Since the test result depends on the concentration of both iodine and potassium iodide in the solution, the instructions for the preparation and the standardization of the solution (7.3) have to be foll
38、owed precisely.6.1.1 Weigh, to the nearest 0,01 g, 114,00 g of potassium iodide (5.3) into a 100 cm3beaker.6.1.2 Place about three-quarters of the KI in a clean 2 000 cm3volumetric flask (4.3) through a large-diameter funnel.6.1.3 Add enough water (5.1) to cover the KI. Swirl to dissolve, and allow
39、to stand until the solution attains ambient temperature. ISO 2016 All rights reserved 3BS ISO 1304:2016ISO 1304:2016(E)6.1.4 Place the remainder of the KI in a 250 cm3beaker with enough water (5.1) to dissolve it.6.1.5 Weigh, to the nearest 0,01 g, 12,00 g of iodine on the balance 4.1 a) in a weighi
40、ng bottle fitted with a ground-glass stopper. Use only a porcelain spoon to transfer the iodine crystals, and close the weighing bottle when making weighings.6.1.6 Transfer the iodine through a funnel to the potassium iodide solution prepared in 6.1.3.6.1.7 Wash thoroughly the weighing bottle with p
41、ortions of the KI solution prepared in 6.1.4 until no colour remains, and transfer the washings through the funnel to the 2 000 cm3volumetric flask.6.1.8 Wash the funnel with the rest of the KI solution prepared in 6.1.4.6.1.9 Add water (5.1) to almost fill the volumetric flask, cap it with the grou
42、nd-glass stopper, invert it 2 or 3 times to homogenize and let it stand for about one hour.6.1.10 Open the flask, make up to the mark with water (5.1), insert a spin bar in the flask, place it on the magnetic stirrer (4.13) and stir for 2 h at least at medium speed.At medium speed, the depth of the
43、vortex should be about 5 mm.6.1.11 Transfer the solution to an amber-glass bottle (4.8) and let it stand overnight prior to any use.6.2 Sodium thiosulfate solution, 0,05 mol/dm3(0,05 N).NOTE Previous editions of this International Standard required a thiosulfate concentration of 0,039 4 mol/dm3(0,03
44、9 4 N). Since the concentration of the thiosulfate solution does not have any impact on the iodine adsorption number, this International Standard now includes a more commonly used solution of 0,05 mol/dm3(0,05 N). The advantage is that such a solution is readily available commercially. If preferred,
45、 it can be prepared from solid sodium thiosulfate as described below.Use of sodium thiosulfate solution of 0,039 4 mol/dm3(0,039 4 N) is still permitted. In this case, the instructions for the preparation of the solution, the formulae used in its standardization and the formulae used in the calculat
46、ion of the iodine adsorption number will have to be modified accordingly.6.2.1 Weigh, to the nearest 0,005 g, 24,817 g of sodium thiosulfate pentahydrate (5.5) into a suitable container.6.2.2 With the help of a funnel, transfer the weighed sodium thiosulfate to a 2 000 cm3volumetric flask (4.3).6.2.
47、3 Add through the funnel about 1 litre of water (5.1). Wash carefully.6.2.4 Add 10 cm3of n-amyl alcohol (5.6) to the flask, and shake the solution in the flask vigorously until all crystals are dissolved.6.2.5 Make up to the mark with water (5.1), insert a spin bar in the flask, place it on the magn
48、etic stirrer and stir for about 2 h at medium speed (see 6.1.10).6.2.6 Transfer the solution to a glass bottle (4.7).4 ISO 2016 All rights reservedBS ISO 1304:2016ISO 1304:2016(E)6.3 Potassium iodate/iodide solution, c(KIO3) = 0,008 33 mol/dm3(0,05 N).6.3.1 Dry an adequate quantity of potassium ioda
49、te (5.4) in the oven (4.2) at 125 C for 1 h. Allow to cool to ambient temperature in the desiccator (4.12).6.3.2 In a 1 000 cm3volumetric flask (see 4.3), dissolve 57,0 g (weighed to the nearest 0,1 g) of potassium iodide (5.3) in about 200 cm3of water (5.1). Allow to stand until the solution attains ambient temperature.6.3.3 Weigh out, to the nearest 0,1 mg, 1,783 3 g of the freshly dried potassium iodate (5.4) and transfer to the iodide solution in the volumetric flask.6.3.4 Make up to the mark with
