1、BRITISH STANDARDBS ISO 11345:2006Rubber Assessment of carbon black and carbon black/silica dispersion Rapid comparative methodsICS 83.060g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g
2、38g50g51g60g53g44g42g43g55g3g47g36g58BS ISO 11345:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 22 February 2006 BSI 22 February 2006ISBN 0 580 47864 5National forewordThis British Standard reproduces verbatim ISO 11345:2006 and impleme
3、nts it as the UK national standard. It supersedes BS ISO 11345:1997 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/22, Physical testing of rubber, which has the responsibility to:A list of organizations represented on this committee can be obtaine
4、d on request to its secretary.Cross-referencesThe British Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electr
5、onic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to und
6、erstand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK.Summary of pagesThis document comprises a
7、front cover, an inside front cover, the ISO title page, pages ii to v, a blank page, pages 1 to 26, an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsReference
8、 numberISO 11345:2006(E)INTERNATIONAL STANDARDISO11345Second edition2006-02-01Rubber Assessment of carbon black and carbon black/silica dispersion Rapid comparative methods Caoutchouc valuation de la dispersion du noir de carbone et du noirde carbone/silice Mthodes comparatives rapides BS ISO 11345:
9、2006iiiiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references . 13 Terms and definitions. 14 Principle. 15 Number of tests. 26 Method A Visual microscopic or photographic microscopic inspection with u 30 magnification. 27 Method B Split-field microscopic inspection with u 30 magni
10、fication . 38 Method C Visual microscopic or photographic microscopic inspection with u 100 magnification. 69 Method D Split-field microscopic inspection with u 100 magnification . 710 Method E Large-agglomerate count with u 100 magnification 811 Test report . 10Annex A (normative) Visual dispersion
11、 rating vs dispersion classification at u 30 magnification (methods A and B) 11Annex B (normative) Visual dispersion rating vs dispersion classification at u 100 magnification Carbon black (CB) . 12Annex C (normative) Visual dispersion rating vs dispersion classification at u 100 magnification Reinf
12、orcing carbon black (RCB) 15Annex D (informative) Visual dispersion rating vs dispersion classification at u 100 magnification Reinforcing carbon black with silica (RCB/Silica) . 18Annex E (normative) Visual dispersion rating vs dispersion classification at u 100 magnification Semi-reinforcing carbo
13、n black (SRCB) . 21Annex F (informative) Dispersion in rubber 24Bibliography . 26BS ISO 11345:2006ivForeword 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 11345 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 2, Testing and analysis.This second edition cancels
18、and replaces the first edition (ISO 11345:1997), which has been technically revised. BS ISO 11345:2006vIntroduction The degree of filler dispersion in a rubber compound is important because certain physical properties, e.g. tensile strength, hysteresis and abrasion resistance, are influenced by disp
19、ersion. The methods described in this International Standard make use of the well known fact that, in a compound in which the ingredients are well dispersed, light is reflected from a freshly cut surface, revealing a smooth, unblemished texture. The presence of improperly dispersed ingredients is sh
20、own by irregularities which usually take the form of circular, convex “bumps” or concave pockmarks on the surface, and their presence indicates a less-than-perfect dispersion of the compounding ingredients. The size and frequency of these irregularities may be used to judge the degree to which the c
21、ompound falls short of an optimum dispersion. A set of four standards each comprising ten photographs based on size and frequency of these irregularities has been established to which numerical ratings have been assigned. This scheme provides a means of evaluating dispersion in a rubber compound and
22、 assigns numerical designations to the degrees of dispersion. This International Standard describes test procedures for assessing the degree of macrodispersion of carbon black and silica in rubber. The methods are primarily intended to be used as rapid factory controls during mixing and subsequent p
23、rocessing stages to assure adequate carbon black dispersion. Five alternative methods are described. The addition of a higher magnification and photographic reference standards for silica was in response to a request from tyre manufacturers and filler producers. Method E was specially requested by m
24、anufacturers of extruded profiles for the automotive industry. Equipment with electronically stored standards may be supplied by: TechPro, Inc 121 East Ascot Lane, Cuyahoga Falls, OH 44223, USATelephone +1 330 923 3546 Telefax +1 330 923 6335 www.techpro- BS ISO 11345:2006blank1Rubber Assessment of
25、carbon black and carbon black/silica dispersion Rapid comparative methods WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibil
26、ity of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. 1 Scope This International Standard specifies qualitative visual methods for the rapid and comparative assessment of the degree of macrodispersion of carbon black an
27、d carbon black/silica in rubber. Ratings are made relative to a set of standard reference photographs, and the results are expressed on a numerical scale from 1 to 10. In addition, a method is given for rating the presence of large agglomerates on a numerical scale (ratings 1 to 10). 2 Normative ref
28、erences 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) applies. ISO 1382, Rubber Vocabulary3 Terms and de
29、finitions For the purposes of this document, the terms and definitions given in ISO 1382 apply. 4 Principle The carbon black or carbon black/silica filled rubber compound is cut to expose a fresh surface for examination under magnification. Five methods are described: Method A: Visual microscopic or
30、 photographic microscopic inspection with u 30 magnification (for carbon black). Method B: Split-field microscopic inspection with u 30 magnification (for carbon black). Method C: Visual microscopic or photographic microscopic inspection with u 100 magnification (for carbon black or carbon black/sil
31、ica). Method D: Split-field microscopic inspection with u 100 magnification (for carbon black or carbon black/silica). Method E: Large-agglomerate count with u 100 magnification (for carbon black). BS ISO 11345:20062In methods A to D, the dispersion level is compared with a series of ten hard-copy o
32、r electronically stored standard references under oblique illumination at 30 (to accentuate detail) and with an effective magnification of u 30 for methods A and B (see Annex A) and u 100 for methods C and D (see Annexes B to E), and then rated numerically from 10 (excellent) to 1 (very poor). A rat
33、ing of 10 indicates a state of dispersion resulting in near optimum physical properties while a rating of 1 would indicate structural flaws causing considerably inferior physical properties. Normally, the visual dispersion ratings indicate the following levels of compound quality. Visual dispersion
34、rating Dispersion classification 9 to 10 Excellent 8 Good 7 Acceptable 5 to 6 Doubtful 3 to 4 Poor 1 to 2 Very poor In method E, the presence of agglomerates is analysed using an image-processing system under oblique illumination at 30 and with an effective magnification of u 100, and then rated num
35、erically from 10 (excellent) to 1 (very poor). The rating 10 is based on the absence of clusters with a diameter of 23 m or larger, indicating that the agglomerates are much smaller than this. The rating 1 corresponds to the maximum number of large agglomerates which can be achieved in practice. 5 N
36、umber of tests A minimum of five tests on different parts of each test piece shall be carried out. 6 Method A Visual microscopic or photographic microscopic inspection with u 30 magnification 6.1 General Method A is a test method which determines the degree of dispersion of carbon black in rubber co
37、mpounds by means of visual microscopic or photographic microscopic inspection, which is used to rate the test piece against a set of transparencies or electronically stored standard references. 6.2 Apparatus 6.2.1 Razor blade, with a single edge, attached to a sample cutter. 6.2.2 Sample cutter, com
38、prising a razor blade holder and a lever mechanism which provides a vertical cutting action. 6.2.3 Binocular microscope (u 30), or 6.2.4. 6.2.4 Binocular microscope (u 30), equipped with a standard self-developing or digital camera with at least 2 megapixel resolution. 6.2.5 Illuminator, microscope
39、type, with high luminous intensity. BS ISO 11345:200636.3 Test piece 6.3.1 Vulcanized compound Using the sample cutter, cut out a test piece with a cross-section of approximately 8 mm thickness and 10 mm width. Do not touch the surface to be used for rating. The razor blade shall be replaced before
40、the edge wears to the extent that the cut becomes lined. 6.3.2 Unvulcanized compound The compound shall first be compressed to remove most of the air holes since, even in small amounts, they can have the appearance of poorly dispersed carbon black and can therefore affect the rating. To accomplish t
41、his, press the rubber into a slab between thin sheets of plastic in a mould at a pressure of about 1 kPa for 5 min at 105 C. Take care to avoid excessive flow during this step. The surface to be examined shall, as far as possible, be free from distortion and blemishes. To achieve this, the cutting e
42、dge of the tool shall be free from defects and the distortion of the sample shall be minimized by applying the cutting pressure evenly and slowly with the sharp razor blade heated to approximately 100 C. However, even with all these precautions, the evaluation of a cured test piece of the same compo
43、und may give a different result. 6.4 Procedure Examine the prepared test piece under the binocular microscope with oblique illumination (at an angle of incidence of 30) to accentuate surface detail. The illuminator should preferentially be placed parallel to the direction of cutting since any cuttin
44、g lines will show less. Compare the size and frequency of any any carbon black agglomerates in the test piece (showing up as surface bumps or depressions) with those in the reference photographs (see Annex A). NOTE If a microscope with a self-developing or digital camera is used, the dispersion can
45、be assessed by side-by-side comparison with the reference photographs using the photograph obtained. This provides a permanent record of the test piece appearance in a matter of minutes. Assign to each compound being assessed the most closely matching numerical rating, using whole numbers. For close
46、r matching, use fractional ratings: 5 1/2 would indicate a rating between 5 and 6. A rating of 10 indicates a state of dispersion representing near-optimum physical properties while a rating of 1 indicates the presence of structural flaws, resulting in inferior physical properties. 7 Method B Split-
47、field microscopic inspection with u 30 magnification 7.1 General Method B determines the degree of dispersion of carbon black in rubber compounds by means of a split-field viewing technique which is used to rate the test piece against a set of transparencies or electronically stored standard referen
48、ce images. The assessment of the degree of carbon black dispersion using the split-field optical-microscopic technique is accomplished by co-projection of the reference images and the test piece image on a TV monitor using a black-and-white video camera or a CCD camera. The reference images are iden
49、tical to the photographic references used in method A. 7.2 Apparatus 7.2.1 Razor blade, with a single edge, attached to a sample cutter. 7.2.2 Sample cutter, comprising a razor blade holder and a lever mechanism which provides a vertical cutting action. BS ISO 11345:200647.2.3 Equipment for split-field representation. The instrument is based on the so-called split-field optical-microscope technique in which each of the 10 references can be projected side by side with the reflected image of the tes
