1、BS ISO5794-1:2010ICS 83.040.20NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDRubber compoundingingredients Silica,precipitated, hydratedPart 1: Non-rubber testsThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on
2、 30 June2010 BSI 2010ISBN 978 0 580 70218 1Amendments/corrigenda issued since publicationDate CommentsBS ISO 5794-1:2010National forewordThis British Standard is the UK implementation of ISO 5794-1:2010. Itsupersedes BS ISO 5794-1:2005 which is withdrawn.The UK participation in its preparation was e
3、ntrusted to TechnicalCommittee PRI/23, Test methods for rubber and non-black compoundingingredients.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are respo
4、nsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.BS ISO 5794-1:2010Reference numberISO 5794-1:2010(E)ISO 2010INTERNATIONAL STANDARD ISO5794-1Fourth edition2010-03-15Rubber compounding ingredients Silica, precipitated, hydrated Part 1:
5、 Non-rubber tests Ingrdients de mlange du caoutchouc Silices hydrates prcipites Partie 1: Essais sur le produit brut BS ISO 5794-1:2010ISO 5794-1:2010(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but sh
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8、 ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2010 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any
9、form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address 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
10、09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2010 All rights reservedBS ISO 5794-1:2010ISO 5794-1:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Terms and definitions .2 4 Sampling.2 5 Methods of test 2 6 Test rep
11、ort3 Annex A (normative) Determination of total copper content .4 Annex B (normative) Determination of total manganese content .7 Annex C (normative) Determination of total iron content 10 Annex D (normative) Determination of specific surface area 13 Annex E (normative) Determination of the specific
12、 surface area by multipoint nitrogen adsorption test (BET test) 20 Annex F (normative) Determination of granule size fractions of granulated precipitated silica21 Annex G (normative) Determination of CTAB surface area .23 Annex H (informative) Classification of silicas and typical physical and chemi
13、cal properties29 Bibliography31 BS ISO 5794-1:2010ISO 5794-1:2010(E) iv ISO 2010 All rights reservedForeword 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
14、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 wo
15、rk. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare Inte
16、rnational Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of t
17、he 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. ISO 5794-1 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the r
18、ubber industry. This fourth edition cancels and replaces the third edition (ISO 5794-1:2005), of which it constitutes a minor revision comprising the following changes: the distilled or deionized water used for the tests has been replaced throughout the document by grade 3 water as defined in ISO 36
19、96; the way in which the silica content is calculated (see Table 1) has been simplified; for the sieve specified in F.3.2, an alternative sieve height (45 mm) has been included in addition to the sieve height of 25 mm originally specified. This fourth edition also incorporates the Technical Corrigen
20、da ISO 5794-1:2005/Cor.1:2006 and ISO 5794-1:2005/Cor.2:2007. ISO 5794 consists of the following parts, under the general title Rubber compounding ingredients Silica, precipitated, hydrated: Part 1: Non-rubber tests Part 2: Evaluation procedures in styrene-butadiene rubber BS ISO 5794-1:2010INTERNAT
21、IONAL STANDARD ISO 5794-1:2010(E) ISO 2010 All rights reserved 1Rubber compounding ingredients Silica, precipitated, hydrated Part 1: Non-rubber tests WARNING Persons using this part of ISO 5794 should be familiar with normal laboratory practice. This part of ISO 5794 does not purport to address all
22、 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 ensure compliance with any national regulatory conditions. 1 Scope This part of ISO 5794 specifies methods of test for characterizing precipitated h
23、ydrated silica for use as a rubber compounding ingredient. A definition of precipitated hydrated silica is given. ISO 5794-2 specifies the test formulation, mixing equipment, mixing procedure and methods of test for use in determining the physical properties of styrene-butadiene rubber compounded wi
24、th precipitated hydrated silica. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) ap
25、plies. ISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings ISO 787-2, General methods of test for pigments and extenders Part 2: Determination of matter volatile at 105 C ISO 787-8, General methods of test for pigments and extenders Part 8:
26、 Determination of matter soluble in water Cold extraction method ISO 787-9, General methods of test for pigments and extenders Part 9: Determination of pH value of an aqueous suspension ISO 787-10, General methods of test for pigments and extenders Part 10: Determination of density Pyknometer method
27、 ISO 787-18, General methods of test for pigments and extenders Part 18: Determination of residue on sieve Mechanical flushing procedure ISO 1124, Rubber compounding ingredients Carbon black shipment sampling procedures ISO 3262-1:1997, Extenders for paints Specifications and methods of test Part 1:
28、 Introduction and general test methods ISO 3262-19:2000, Extenders for paints Specifications and methods of test Part 19: Precipitated silica BS ISO 5794-1:2010ISO 5794-1:2010(E) 2 ISO 2010 All rights reservedISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 15528
29、, Paints, varnishes and raw materials for paints and varnishes Sampling ISO 18852, Rubber compounding ingredients Determination of multipoint nitrogen surface area (NSA) and statistical thickness surface area (STSA) 3 Terms and definitions For the purposes of this document, the following terms and d
30、efinitions apply. 3.1 precipitated hydrated silica material composed of amorphous particles obtained from soluble silicates by precipitation from aqueous solution 4 Sampling Sampling shall be carried out in accordance with ISO 15528. 5 Methods of test The properties of precipitated hydrated silica s
31、hall be determined by the methods of test referred to in Table 1. Table 1 Methods of test Property Method of test Silica content of ignited sample, % (by mass) ISO 3262-19:2000, Clause 6 Colour ISO 3262-1:1997, 5.1 Residue on sieve (nominal aperture size 45 m) for silica in powder form for silica in
32、 other forms ISO 3262-19:2000, Clause 8 ISO 787-18 Volatile matter at 105 C (loss on heating) ISO 787-2 (Use a test portion of 2 g weighed to the nearest 0,1 mg.) Density, Mg/m3ISO 787-10 Loss on ignition at 1 000 C of dried sample ISO 3262-1:1997, 5.2 pH of slurry ISO 787-9 Water-soluble matter ISO
33、 787-8 Total copper content, mg/kg See Annex A Total manganese content, mg/kg See Annex B Total iron content, mg/kg See Annex C Specific surface area, m2/g See Annexes D, E Granule size distribution, % See Annex F CTAB surface area, m2/g See Annex G BS ISO 5794-1:2010ISO 5794-1:2010(E) ISO 2010 All
34、rights reserved 36 Test report The test report shall include the following information: a) a reference to this part of ISO 5794; b) all details necessary for complete identification of the material tested; c) the results of the tests: 1) silica content, 2) colour, 3) residue on sieve (and the test m
35、ethod used), 4) volatile matter at 105 C, 5) density, 6) loss on ignition at 1 000 C, 7) pH of slurry, 8) water-soluble matter, 9) total copper content, 10) total manganese content, 11) total iron content, 12) specific surface area by nitrogen adsorption (and the test method used), 13) granule size
36、distribution (fraction retained on the 75 m and 300 m screens, and the fines content), 14) specific surface area by CTAB adsorption, d) any unusual observations noted during the test; e) any deviations from the test method and the reason for them; f) any tests performed not covered by this part of I
37、SO 5794; g) the date of the test. BS ISO 5794-1:2010ISO 5794-1:2010(E) 4 ISO 2010 All rights reservedAnnex A (normative) Determination of total copper content A.1 Principle A test portion is digested with hydrofluoric acid and sulfuric acid and the silicon is volatilized as silicon tetrafluoride. An
38、y metals in the digested test portion are dissolved in hydrochloric acid, then the solution is diluted and aspirated into the flame of an atomic absorption spectrometer set at a wavelength of 324,7 nm. The method is applicable to the determination of copper contents up to 125 mg/kg, and there is pro
39、vision for extending the range to 1 250 mg/kg. WARNING All recognized health and safety precautions should be taken when performing this method of analysis. A.2 Reagents and materials All reagents shall be of recognized analytical grade. The water used shall be grade 3 water as defined in ISO 3696:1
40、987. A.2.1 Acetylene, compressed-gas supply. A.2.2 Air, compressed-gas supply. A.2.3 Hydrochloric acid, 10 % (by mass) solution. Dilute 20 cm3of 35 % (by mass) hydrochloric acid solution (20= 1,18 Mg/m3) with 50 cm3of water. A.2.4 Hydrofluoric acid, 40 % (by mass) solution (20= 1,13 Mg/m3). A.2.5 Su
41、lfuric acid, 98 % (by mass) solution (20= 1,84 Mg/m3). A.2.6 Nitric acid, 68 % (by mass) solution (20= 1,42 Mg/m3). A.2.7 Copper, standard solution corresponding to 1 g of Cu per cubic decimetre. Dissolve 1,000 g 0,001 g of high-purity copper turnings in a mixture of 10 cm3of water and 5 cm3of nitri
42、c acid (A.2.6) in a 100 cm3beaker. Boil under a fume hood to expel oxides of nitrogen. Cool, transfer to a 1 dm3volumetric flask, make up to the mark with water and mix. 1 cm3of this standard solution contains 1 000 g of copper. A.2.8 Copper, standard solution corresponding to 50 mg of Cu per cubic
43、decimetre. Pipette 50,0 cm3of the 1 g/dm3standard copper solution (A.2.7) into a 1 dm3volumetric flask, add 5 cm3of nitric acid (A.2.6), make up to the mark with water and mix. 1 cm3of this standard solution contains 50 g of copper. BS ISO 5794-1:2010ISO 5794-1:2010(E) ISO 2010 All rights reserved 5
44、A.2.9 Copper, standard solution corresponding to 10 mg of Cu per cubic decimetre. Pipette 50,0 cm3of the 50 mg/dm3standard copper solution (A.2.8) into a 250 cm3volumetric flask, add 1 cm3of nitric acid (A.2.6), make up to the mark with water and mix. 1 cm3of this standard solution contains 10 g of
45、copper. NOTE Commercially available standard copper solutions may be used, if preferred, instead of the solutions described in A.2.7, A.2.8 and A.2.9. A.3 Apparatus Usual laboratory equipment, plus the following: A.3.1 Platinum dish, of capacity approximately 35 cm3. A.3.2 Atomic absorption spectrom
46、eter, fitted with an air/acetylene burner. A.3.3 Analytical balance, capable of weighing to 0,1 mg. A.4 Procedure A.4.1 Test portion Weigh, to the nearest 0,1 mg, approximately 2 g of sample into the platinum dish (A.3.1). A.4.2 Blank test Carry out a blank test simultaneously with the determination
47、, using the same reagents and same procedures, but omitting the test portion. A.4.3 Preparation of the calibration graph A.4.3.1 Preparation of standard calibration solutions Into a series of six 50 cm3volumetric flasks, transfer the volumes of 10 mg/dm3standard copper solution (A.2.9) indicated in
48、Table A.1, dilute to the mark with water and mix. Table A.1 Standard calibration solutions for determination of copper Volume of standard copper solution (A.2.9) cm3Corresponding copper content g/cm30,5 0,1 2,5 0,5 5,0 1,0 10,0 2,0 15,0 3,0 25,0 5,0 BS ISO 5794-1:2010ISO 5794-1:2010(E) 6 ISO 2010 Al
49、l rights reservedA.4.3.2 Spectrometric measurements Aspirate in turn each of the standard calibration solutions prepared in A.4.3.1 into the flame of the atomic absorption spectrometer (A.3.2) and record their absorbances at a wavelength of 324,7 nm, following the instructions of the instrument manufacturer. Aspirate water into the flame after each measurement. A.4.3.3 Plotting the graph Plot a graph having, for example, the copper contents, in micrograms p
