1、BS ISO 9298:2017 Rubber compounding ingredients Zinc oxide Test methods BSI Standards Publication WB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 9298:2017 BRITISH STANDARD National foreword This British Standard is the UK implementation of ISO 9298:2017. The UK participation in its p
2、reparation was entrusted to Technical Committee PRI/50, Raw materials (including latex) for use in the rubber industry. 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 a co
3、ntract. Users are responsible for its correct application. The British Standards Institution 2017. Published by BSI Standards Limited 2017 ISBN 978 0 580 92856 7 ICS 83.040.20 Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under
4、the authority of the Standards Policy and Strategy Committee on 31 March 2017. Amendments/corrigenda issued since publication Date T e x t a f f e c t e dBS ISO 9298:2017 ISO 2017 Rubber compounding ingredients Zinc oxide Test methods Ingrdients de mlange du caoutchouc Oxyde de zinc Mthodes dessai I
5、NTERNATIONAL STANDARD ISO 9298 Second edition 2017-03 Reference number ISO 9298:2017(E)BS ISO 9298:2017ISO 9298:2017(E)ii ISO 2017 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in Switzerland All rights reserved. Unless otherwise specified, no part of this publication may be r
6、eproduced 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 member body in the country of the reque
7、ster. ISO copyright office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.orgBS ISO 9298:2017ISO 9298:2017(E)Foreword iv 1 Scope . 1 2 Normative references 1 3 T erms and definitions . 1 4 Sampling 2 5 Methods of te
8、st for the determination of physical and chemical properties 2 5.1 General . 2 5.2 Matter volatile at 105 C . 2 5.3 Water-soluble matter 2 5.4 Acidity/alkalinity 2 5.5 Residue on sieve 2 5.6 Nitrogen-adsorption surface area 2 6 Classification and typical v alues of zinc o xides 3 7 Test report . 3 A
9、nnex A (normative) Det ermination of zinc o xide c ont ent 4 Annex B (normative) Determination of lead, cadmium, copper and manganese contents .7 Annex C (normative) Determination of acid-insoluble matter 10 Annex D (informative) Zinc o xides used as rubber c ompounding mat erial Classification and
10、typical values .12 ISO 2017 All rights reserved iii Contents PageBS ISO 9298:2017ISO 9298:2017(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 ca
11、rried 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
12、. 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 diffe
13、rent 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
14、 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/
15、 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 conformit y assessment, as well as information about ISOs adherence to the Worl
16、d Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www . i s o .org/ iso/ foreword .html. 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 rubb
17、er industry. This second edition cancels and replaces the first edition (ISO 9298:1995), which has been technically revised. The main change is the reference to ISO 18852 as the method for the nitrogen adsorption to determine the surface area.iv ISO 2017 All rights reservedBS ISO 9298:2017INTERNATIO
18、NAL ST ANDARD ISO 9298:2017(E) Rubber compounding ingredients Zinc oxide Test methods WARNING Persons using this document should be familiar with normal laboratory practice. This document does not purport to address all of the safety problems, if any, associated with its use. It is the responsibilit
19、y of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. 1 Scope This document specifies the methods to be used for the evaluation of zinc oxide for use in the rubber industry. The analytical methods are applicable to all co
20、mmercial zinc oxides, for example: direct type (American process); indirect type (French process); other types produced by different chemical methods, i.e. precipitation and calcination. Zinc oxide can also be coated with organic materials, such as fatty acids, oil, wetting agents, etc., in order to
21、 improve the dispersion in rubber. 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
22、 the referenced document (including any amendments) applies. ISO 787-2, General methods of test for pigments and extenders Part 2: Determination of matter volatile at 105 C ISO 787-4, General methods of test for pigments and extenders Part 4: Determination of acidity or alkalinity of the aqueous ext
23、ract ISO 787-7, General methods of test for pigments and extenders Part 7: Determination of residue on sieve Water method Manual procedure ISO 787-8, General methods of test for pigments and extenders Part 8: Determination of matter soluble in water Cold extraction method ISO 1124, Rubber compoundin
24、g ingredients Carbon black shipment sampling procedures ISO 18852, Rubber compounding ingredients Determination of multipoint nitrogen surface area (NSA) and statistical thickness surface area (STSA) 3 T erms a nd definiti ons No terms and definitions are listed in this document. ISO and IEC maintai
25、n terminological databases for use in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp ISO 2017 All rights reserved 1BS ISO 9298:2017ISO 9298:2017(E) 4 Sampling Sampl
26、ing shall be carried out in accordance with ISO 1124 for dry powders. 5 Methods of test for the determination of physical and chemical properties 5.1 General Surface-coated zinc oxides shall be evaluated by the methods specified in Table 1. This evaluation shall be done without prior calcination or
27、extraction, since there is little purpose in determining volatile-matter content, content of water-soluble matter or acidity if the coating is removed. T a b l e 1 M e t h o d s f o r t h e e v a l u a t i o n o f s u r f a c e - c o a t e d z i n c o x i d e s Property Units Test method Matter vola
28、tile at 105 C % (m/m) ISO 787-2 Water-soluble matter % (m/m) ISO 787-8 Acidity/alkalinity (H 2 SO 4equiv.) g H 2 SO 4 /100 g ISO 787-4 Residue on sieve % (m/m) ISO 787-7 Nitrogen-adsorption surface area m 2 /g ISO 18852 Zinc oxide % (m/m) Annex A Lead % (m/m) Annex B Cadmium % (m/m) Annex B Copper %
29、 (m/m) Annex B Manganese % (m/m) Annex B Acid-insoluble matter % (m/m) Annex C 5.2 Matter volatile at 105 C Determine the loss on heating at 105 C in accordance with ISO 787-2. 5.3 Water-soluble matter Determine the percentage of water-soluble matter in accordance with ISO 787-8. 5.4 Acidity/alkalin
30、ity Determine the acidity/alkalinity, in cm 3o f 0 , 1 m o l / d m 3standard volumetric solution per 100 g of sample, in accordance with ISO 787-4. The result shall be expressed in grams of sulfuric acid per 100 g (g H 2 SO 4 /100 g) by multiplying the result by 4,9 10 -3 . 5.5 Residue on sieve Dete
31、rmine the sieve residue in accordance with ISO 787-7. 5.6 Nitrogen-adsorption surface area Determine the surface area in accordance with ISO 18852. The test portion shall be 0,7 g to 1,0 g, or more if indicated by the initial test or past experience.2 ISO 2017 All rights reservedBS ISO 9298:2017ISO
32、9298:2017(E) 6 Classific ation and typical v alues of zinc o xides Three types of zinc oxide are used in the rubber industry and are described in Annex D. Typical values for some of the various types of zinc oxide are given in Annex D. 7 Test report The test report shall include the following: a) a
33、reference to this document, i.e. ISO 9298; b) all details necessary for the identification of the sample; c) the zinc oxide content of the sample; d) the lead, cadmium, copper and manganese contents of the sample; e) the water-soluble matter content of the sample; f) the acidity/alkalinity of the sa
34、mple; g) the residue on sieve; h) the surface area by nitrogen adsorption; i) the acid-insoluble matter; j) the dates of the tests; k) details of any deviation from the procedures specified in this document. ISO 2017 All rights reserved 3BS ISO 9298:2017ISO 9298:2017(E) Annex A (normative) Det ermin
35、ation of zinc o xide c ont ent A.1 Reagents Use only reagents of recognized analytical grade and distilled, deionized or distilled/deionized water for sample preparation and required dilutions. A.1.1 Nitric acid, 65 % (m/m), d 1,4 Mg/m 3 . A.1.2 Hydrochloric acid, 20 % (m/m), d 1,1 Mg/m 3 . A.1.3 Am
36、monia solution, 25 % (m/m), d 0,91 Mg/m 3 . A.1.4 Hydrogen peroxide solution, 3 % (m/m). A.1.5 Iron(III) solution. Dissolve 86 g of iron(III) ammonium sulfate in water and dilute to 1 000 cm 3 . A.1.6 Ammonium chloride solution. Dissolve 250 g of ammonium chloride in water and dilute to 1 000 cm 3 .
37、 A.1.7 Masking solution. Dissolve 30 g of ammonium fluoride, 100 g of ammonium thiosulfate and 250 g of ammonium acetate in water and dilute to 1 000 cm 3 . A.1.8 Bromothymol blue solution. Dissolve 0,1 g of bromothymol blue in 100 cm 3of ethanol. A.1.9 Xylenol orange solution. Dissolve 0,2 g of xyl
38、enol orange, tetrasodium salt, in 100 cm 3of water. A.1.10 EDTA, standard volumetric solution, c(EDTA) = 0,1 mol/dm 3 . Dissolve 37,225 g of ethylenedinitrilotetraacetic acid, disodium salt (Na 2 EDTA), in water in a 1 000 cm 3one-mark volumetric flask, dilute to the mark and mix well. Alternatively
39、, commercially available standard solutions may be used. A.1.11 Zinc metal, of minimum purity 99,995 % (m/m). A.2 Apparatus The usual laboratory apparatus and, in particular, the following.4 ISO 2017 All rights reservedBS ISO 9298:2017ISO 9298:2017(E) A.2.1 V olumetric flasks, class A, of capacity 2
40、50 cm 3 , 500 cm 3and 1 000 cm 3 . A.2.2 Pipettes, class A, of capacity 50 cm 3and 100 cm 3 . A.2.3 Burette, class A, of capacity 50 cm 3 . A.2.4 Balance, of capacity 250 g, weighing to an accuracy of at least 1 mg. A.2.5 Heating device, e.g. a hotplate. A.2.6 Filter paper, acid-washed and fluted. A
41、.2.7 Beakers, of capacity 600 cm 3and 1 000 cm 3 . A.2.8 C onical flasks, of capacity 500 cm 3and 1 000 cm 3 . A.3 Sampling Take a representative sample in accordance with ISO 1124. A.4 Procedure A.4.1 Suspend 20 g of the zinc oxide sample, weighed to 0,01 g, in 100 cm 3of water in a 1 000 cm 3beake
42、r (A.2.7) and dissolve carefully with approximately 90 cm 3of nitric acid (A.1.1). When the zinc oxide has dissolved, boil for a short time, cool down the solution and transfer it to a 500 cm 3volumetric flask (A.2.1). Carefully dilute the solution to the mark with water and shake. A.4.2 Pipette 50
43、cm 3of this solution into a 250 cm 3volumetric flask (A.2.1). Add 10 cm 3of iron(III) solution (A.1.5). Shake and then add successively 5 cm 3of hydrogen peroxide solution (A.1.4), 60 cm 3of ammonium chloride solution (A.1.6) and 30 cm 3of ammonia solution (A.1.3). A.4.3 Shake briefly and cool down.
44、 Make up to the mark and filter through a dry folded filter paper (A.2.6) into a dry 500 cm 3conical flask (A.2.8). Pipette 50 cm 3of this solution into a 600 cm 3beaker and dilute with water to about 300 cm 3 . A.4.4 Add four drops of bromothymol blue solution (A.1.8) and neutralize with hydrochlor
45、ic acid (A.1.2). The colour changes from blue to light yellow. Add two drops of hydrochloric acid in excess. After addition of 20 ml of masking solution (A.1.7) and seven drops of xylenol orange solution (A.1.9), titrate with EDTA solution (A.1.10) until the colour changes from purple-red to orange-
46、yellow. A.4.5 After further dropwise addition of 0,5 cm 3to 1 cm 3of EDTA solution, the colour changes sharply to pale yellowish-green. Let the total volume of EDTA solution added be V 1 . A.5 Standar dization p r oc edur e Dilute concentrated nitric acid to a concentration of approximately 30 % (m/
47、m), d 1,2 Mg/m 3 . WARNING Acid should be added carefully to water. Then dissolve 20 g of refined zinc (A.1.11), weighed to 0,01 g, by heating in a beaker with 40 cm 3of the diluted nitric acid. Allow the solution to cool, transfer to a 1 000 cm 3volumetric flask and dilute to the mark. Proceed acco
48、rding to A.4.2 to A.4.5 to obtain the titration volume V 2 . ISO 2017 All rights reserved 5BS ISO 9298:2017ISO 9298:2017(E) 1 cm 3of 0,1 mol/dm 3EDTA solution corresponds to 0,006 537 g of zinc or 0,008 138 g of zinc oxide. A.6 Expression of results Calculate the total zinc oxide content w ZnO , exp
49、ressed as a percentage by mass, using Formula (A.1): (A.1) where V 1 is the volume, in cubic centimetres, of EDTA solution required for titration of the zinc in the test portion (A.4); V 2 is the volume, in cubic centimetres, of EDTA solution required for titration of the zinc in the standardization procedure (A.5); 1,245 is the ratio of the relative molecular mass of zinc oxide to the relative atomic mass of zinc. A.7 Interference Lead and iron are
