1、BRITISH STANDARD BS ISO 18553:2002 Incorporating amendment no. 1 Method for the assessment of the degree of pigment or carbon black dispersion in polyolefin pipes, fittings and compounds ICS 23.040.20; 23.040.45 BS ISO 18553:2002 This British Standard was published under the authority of the Standar
2、ds Policy and Strategy Committee on 24 May 2002 BSI 2007 ISBN 978 0 580 60467 6 National foreword This British Standard is the UK implementation of ISO 18553:2002, incorporating amendment 1:2007. It supersedes BS 2782-11:Method 1106A:1983 which is withdrawn. The start and finish of text introduced o
3、r altered by amendment is indicated in the text by tags !“. Tags indicating changes to ISO text carry the number of the ISO amendment. For example, text altered by ISO amendment 1 is indicated by !“. The UK participation in its preparation was entrusted by Technical Committee PRI/88, Plastic piping
4、systems and components, to Subcommittee PRI/88/4, Method of test for thermoplastic piping systems and components. A list of organizations represented on this subcommittee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contr
5、act. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Amendments issued since publication Amd. No. Date Comments 17424 31 October 2007 See national foreword Reference number ISO 18553:2002(E)INTERNATIONAL STANDARD IS
6、O 18553 First edition 2002-03-01 Method for the assessment of the degree of pigment or carbon black dispersion in polyolefin pipes, fittings and compounds Mthode destimation de la dispersion du pigment et du noir de carbone dans les tubes, raccords et compositions base de polyolfines ISO 18553:2002(
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11、ctnuoo yrf ttseuqer ehe.r ISO cirypothg fofice saCe tsopale 65 eneG 1121-HC 02 av leT. 4 + 10 947 22 1 11 xaF0 947 22 14 + 9 74 E-mail coirypthgiso.c h Web ww.wiso.ch Prnietdi nS wztierland ii ISO 2002 Allr ithgsr ese devrISO 18553:2002(E) iiiContents Page Foreword.iv Introduction.v 1 Scope 1 2 Prin
12、ciple1 3 Apparatus .1 4 Procedure .2 5 Expression of results 3 6 Test report 3 Annex A (normative) Grading table for particles and agglomerates.4 Annex B (normative) Photomicrographs for evaluation of the appearance of the dispersion.5 Annex C (informative) Examples of grading of particles and agglo
13、merates 8 Annex D (informative) Basic specification .9 ISO 18553:2002(E) iv 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 carried out through ISO
14、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. ISO collaborates clo
15、sely 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 3. The main task of technical committees is to prepare International Standards. Dra
16、ft 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 the elements of this Inte
17、rnational Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 18553 was prepared by Technical Committee ISO/TC 138, Plastics pipes, fittings and valves for the transport of fluids, Subcommittee SC 5, General properties of
18、 pipes, fittings and valves of plastic materials and their accessories Test methods and basic specifications. This International Standard cancels and replaces ISO 11420:1996, Method for the assessment of the degree of carbon black dispersion in polyolefin pipes, fittings and compounds, and ISO 13949
19、:1997, Method for the assessment of the degree of pigment dispersion in polyolefin pipes, fittings and compounds, which have been combined into a single document. Annexes A and B form a normative part of this International Standard. Annexes C and D are for information only. ISO 18553:2002(E) vIntrod
20、uction Thermoplastic products manufactured for pipeline systems are normally coloured. Typically fine carbon black particles or coloured pigments are used. These are normally incorporated into the raw material prior to either extrusion of pipe or injection moulding of pipe fittings. The purpose of c
21、olouring is to allow identification of the pipeline in service and also, in the case of carbon black, to act as protection of the polymer from degradation by ultra-violet light if the product is stored externally or used for external service. It is important that the carbon black or pigment particle
22、s are correctly dispersed in the polymer, and hence the final product, to ensure that the physical, mechanical and surface protection properties are maintained. Correct dispersion may also be an indication that anti-oxidants and ultra-violet stabilizers are correctly dispersed, and that the size of
23、agglomerates of particles is not excessive. This method provides procedures for assessing the degree of dispersion by physical measurement of the size of the dispersed particles and arithmetically grading the particle size distribution. It also provides photographs for comparison with microscopic im
24、ages of samples taken from raw-material compound or products in order to judge subjectively the acceptability of carbon black or pigment dispersion. A recommended limit of grading of particles/agglomerate size and a list of the photographs from annex B for an acceptable rating of appearance is given
25、 in annex D. It is noted that this method supersedes and merges previously published individual methods for assessment of carbon black and pigment dispersion (see the foreword). INTERNATIONAL STANDARD ISO 18553:2002(E)1Method for the assessment of the degree of pigment or carbon black dispersion in
26、polyolefin pipes, fittings and compounds 1 Scope This International Standard describes a method with two procedures for the assessment of pigment or carbon black particle and agglomerate size and degree of dispersion in polyolefin pipes, fittings and compounds. The method is applicable to polyolefin
27、 pipes and fittings, as well as raw material in pellet form, with the choice of procedure to be determined by the referring specification. The method is applicable to carbon black pigmented polyolefin pipes, fittings and compounds with a carbon black content of less than 3 %. 2 Principle Small sampl
28、es of raw-material pellet or material removed from the pipe or fitting are heated and compressed between microscope slides. Alternatively, a microtome slice can be taken. The specimens produced are examined microscopically and the sizes of particles and agglomerates are measured, recorded and graded
29、 by comparison with a tabulated grading system (see Table A.1). A particle/agglomerate size grading is determined from an average of the gradings determined for six specimens. If required, a rating of the appearance of the dispersion is determined by comparison with photomicrographs (see annex B). 3
30、 Apparatus 3.1 General 3.1.1 Microscope, capable of producing suitable magnification, see 4.2 and 5.2, with orthogonal travel, a standard calibrated graticule capable of measuring the particle and agglomerate size, and lighting adequate to avoid optical effects. 3.1.2 Glass microscope slides: 1 mm t
31、hickness is suitable, with a thin cover slip. 3.2 For the compression procedure (see 4.1.1) 3.2.1 Oven or hotplate or other type of heating device, capable of operating at a controlled temperature between 150 C and 210 C. 3.2.2 Scalpel, for cutting out specimens. 3.2.3 Press, weights or spring clips
32、, to maintain pressure. ISO 18553:2002(E) 2 3.3 For the microtome procedure (see 4.1.2) 3.3.1 Microtome, capable of producing a slice of the required thickness (see 4.1.2). 4 Procedure 4.1 Specimen preparation Two methods of preparation of test specimens are described: a compression procedure and a
33、microtome procedure. 4.1.1 Compression procedure 4.1.1.1 Using a scalpel (3.2.2), cut six specimens, each of mass 0,6 mg 0,2 mg for assessing pigment dispersion, or each of mass 0,20 mg 0,10 mg for assessing carbon black dispersion, from different parts of the product to be analysed (see notes 1, 2,
34、 and 3). Place the six specimens on one or more clean microscope slides (3.1.2), with each specimen approximately equidistant from its neighbour and from adjacent edges of the slide (see note 4). Cover with another (or other) clean microscope slide(s) or cover slip(s) (see note 5). NOTE 1 It should
35、be noted that difficulty will be encountered with the microscopic examination of specimens which are too thick. NOTE 2 The specimens are preferably cut along different axes of the product. NOTE 3 It is recommended that cutting out the specimens take place on a clean surface to minimize the possibili
36、ty of extraneous contamination. NOTE 4 Adherence of the specimens may be improved by heating the slide or using a drop of immersion oil or Canada balsam. NOTE 5 Shims made of metal or another suitable material may be used to ensure that uniform thickness is obtained. For the specimen mass and thickn
37、ess given, a film at least 4 mm across is obtained (see note 1). 4.1.1.2 If an oven (see 3.2.1) is to be used, clamp the two slides together with spring clips (see 3.2.3). Place the clamped slides in the oven, for instance (see 3.2.1) maintained at a temperature between 150 C and 210 C and leave for
38、 at least 10 min until each specimen is pressed out to a film of thickness of at least 60 m 20 m for assessment of pigment dispersion or to a thickness of 20 m 10 m for assessment of carbon black dispersion (see note 1 to 4.1.1.1). Remove the slides from the oven and, when they are cool enough to be
39、 handled, remove the clips. 4.1.1.3 Alternatively place the slides on a hotplate or other heating device (see 3.2.1) at a temperature between 150 C and 210 C, and apply pressure using a press or a weight sufficient to produce uniform thickness film according to 4.1.1.2. Cool before removing the slid
40、es for the microscopic examination (see 4.2). 4.1.2 Microtome procedure Cut six specimens from different parts of the product (see note 2 to 4.1.1.1) to produce films of a thickness of 60 m 20 m for assessment of pigment dispersion or of a thickness of 20 m 10 m for assessment of carbon black disper
41、sion, and at least 4 mm across in any direction (see note 1 to 4.1.1.1). Place the six specimens on one or more clean microscope slides (3.1.2), with each specimen approximately equidistant from its neighbour and from adjacent edges of the slide (see note 4 to 4.1.1.1). Cover with another (or other)
42、 clean microscope slide(s) or cover slip. ISO 18553:2002(E) 34.2 Microscopic examination 4.2.1 Examination for assessment of degree of dispersion Examine the particles and agglomerates in each of the six specimens in turn through the microscope (3.1.1) under transmitted light with a recommended magn
43、ification of 100 (see note). Measure and record the largest dimension of each particle and agglomerate, ignoring those less than 5 m. Grade according to the size categories given in Table A.1. NOTE Some pigments may be more visible in polarized light or light of a different intensity. If possible, c
44、heck that the agglomerates are pigment by varying the light intensity and by using different light sources, for instance transmitted, reflected, or polarized light. 4.2.2 Examination for rating of appearance If a rating of the appearance is required, examine each specimen in turn through the microsc
45、ope (3.1.1) under transmitted light with a magnification of at least 70. Note the appearance of each specimen in comparison with the photomicrographs (see annex B). 5 Expression of results 5.1 Grading of particle and agglomerate size Using Table A.1, determine the highest particle/agglomerate size g
46、rade for each specimen. Calculate the arithmetic mean of the six grades obtained and express the result to a single decimal point, rounded up to the next higher value (see the examples given in annex C). 5.2 Rating of appearance Note the appearance of each specimen and the overall dominant appearanc
47、e of the set of specimens. 6 Test report The test report shall include the following information: a) all details necessary for complete identification of the material or product tested, including sample type, origin, manufacturers code number and previous history; b) a reference to this Internationa
48、l Standard; c) the method of preparation of the film specimens (i.e. compression or microtome) and the thickness of the specimens; d) the average grading and the individual film gradings of the specimens, in accordance with 5.1; e) if required, the value of the dominant appearance of the set of spec
49、imens and the individual appearance of each film specimen, in accordance with 5.2; f) details of any deviation from the test method, as well as any incident which may have influenced the results; g) the date of the test. For grades 2,5 and above, it is not necessary to measure particles falling into the lower size categories. To avoid unnecessary work, the largest particles should be measured initially, and compared with the requirements for the maximum n
