1、BRITISH STANDARD BS 6043-1-1:2002 ISO 6257:2002 Methods of sampling and test for carbonaceous materials used in aluminium manufacture Part 1: Electrode pitch Section 1.1: Sampling ICS 71.100.10 Licensed Copy: Wang Bin, na, Thu Jun 07 02:39:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSIBS 6043-1-1:200
2、2 This British Standard, having been prepared under the direction of the Materials and Chemicals Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 14 November 2002 BSI 14 November 2002 ISBN 0 580 40737 3 National foreword This B
3、ritish Standard reproduces verbatim ISO 6257:2002 and implements it as the UK national standard. It supersedes BS 6043-1-1:1981 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee CII/24, Raw materials for the aluminium industry, which has the responsibil
4、ity to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standa
5、rds Correspondence Index”, or by using the “Search” facility of the BSI Electronic 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
6、does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European de
7、velopments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to v, a blank page, pages 1 to 21 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Ame
8、ndments issued since publication Amd. No. Date Comments Licensed Copy: Wang Bin, na, Thu Jun 07 02:39:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSIINTERNATIONAL STANDARD ISO 6257 Second edition 2002-10-01 Reference number ISO 6257:2002(E) Carbonaceous materials used in the production of aluminium Pi
9、tch for electrodes Sampling Produits carbons utiliss pour la production de laluminium Brais pour lectrodes chantillonnageBS604311:2002Licensed Copy: Wang Bin, na, Thu Jun 07 02:39:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSIBS604311:2002ii Licensed Copy: Wang Bin, na, Thu Jun 07 02:39:05 GMT+00:00
10、2007, Uncontrolled Copy, (c) BSIISO 5262002:7)E( ISO 2002 r llAithgs reservde iii Contents Page 1 Scope . 1 2 Normative references . 1 3 Terms and definitions 1 4 General procedures and precautions . 3 5 Sampling of solid pitch 5 6 Soft pitches . 9 7 Hot liquid pitch 10 8 Sample size reduction 17 9
11、Sample containers 19 10 Sampling report 19 Bibliography. 21 BS604311:2002iii Licensed Copy: Wang Bin, na, Thu Jun 07 02:39:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSIISO :7526(2002)E vi ISO 2002 Ar llithgr seresvde Foreword ISO (the International Organization for Standardization) is a worldwide fe
12、deration 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 been established has the right to be represented on that com
13、mittee. 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 standardization. International Standards are drafted in accord
14、ance with the rules given in the ISO/IEC Directives, Part 3. 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
15、 drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 6257 was prepared by Technical Committee ISO/TC 47, Chemistry, Subcommit
16、tee SC 7, Aluminium oxide, cryolite, aluminium fluoride, sodium fluoride, carbonaceous products for the aluminium industry. This second edition cancels and replaces the first edition (ISO 6257:1980), which has been technically revised. BS604311:2002iv Licensed Copy: Wang Bin, na, Thu Jun 07 02:39:05
17、 GMT+00:00 2007, Uncontrolled Copy, (c) BSIISO 5262002:7)E( ISO 2002 r llAithgs reservde v Introduction Sampling is a vital step in analysis and testing. Its importance is recognized in this International Standard which specifies comprehensive methods of sampling the grades of pitch used for the ele
18、ctrolytic production of aluminium. Such samples should be as representative as possible of the materials sampled (whether from the whole or part of a batch or consignment) and in a form that facilitates the determination of the distribution of values of properties. BS604311:2002v Licensed Copy: Wang
19、 Bin, na, Thu Jun 07 02:39:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSILicensed Copy: Wang Bin, na, Thu Jun 07 02:39:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSIANRETNIITOTS LANDNADRA ISO 5262002:7)E( ISO 2002 r llAithgs reservde 1 Carbonaceous materials used in the production of aluminium Pitch f
20、or electrodes Sampling WARNING This International Standard may involve the use of hazardous materials, operations and equipment. This International Standard cannot address all the safety implications associated with its use. It is the responsibility of the user of this International Standard to esta
21、blish appropriate health and safety practices and assess the applicability of regulatory limitations prior to use. 1 Scope This International Standard specifies methods for sampling and preparing samples prior to testing of binder pitch used in the manufacture of electrodes for the electrolytic prod
22、uction of aluminium. These methods are applicable to grades of pitch in liquid or solid form, the latter having softening points higher than(determined according to the method specified in ISO 5940), in bulk, or in a number of containers making up one batch at sites of manufacture, storage, or deliv
23、ery. Sampling methods and sampling plans for large consignments, or lots, of pitch in liquid form during the loading and unloading of ships are included. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this I
24、nternational Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative docu
25、ments indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 3165, Sampling of chemical products for industrial use Safety in sampling ISO 5940, Carbonaceous
26、materials for the production of aluminium Pitch for electrodes Determination of softening point by the ring-and-ball method 3 Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 3.1 sampling unit defined quantity of material having a boun
27、dary which may be physical, for example a container, or hypothetical, for example a particular time or time interval in the case of a stream of material NOTE 1 A number of sampling units may be gathered together, for example in a package or box. NOTE 2 In French, the term “individu” is sometimes use
28、d, a synonym of “unit dchantillonnage”. In English, the terms “individual”, “unit” and “item” are sometimes used in practice as synonyms of “sampling unit”. ISO 6206 30 C BS604311:20021 Licensed Copy: Wang Bin, na, Thu Jun 07 02:39:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSIISO :7526(2002)E 2 ISO
29、2002 Ar llithgr seresvde 3.2 sample one or more sampling units taken from a larger number of sampling units, or one or more increments taken from a sampling unit ISO 6206 3.3 representative sample sample assumed to have the same composition as the material sampled when the latter is considered as ho
30、mogeneous whole ISO 6206 3.4 sampling plan planned procedure of selection, withdrawal and preparation of a sample or samples from a lot (see 3.6) to yield the required knowledge of the characteristic(s) from the final sample (see 3.10) so that a decision can be made regarding the lot NOTE Considerat
31、ions of cost, effort and delay usually determine an acceptable sampling error. ISO 6206 3.5 consignment quantity of material covered by a particular consignment note or shipping document ISO 6206 3.6 lot total quantity of material to be sampled using a particular sampling plan NOTE A lot may consist
32、 of consignments, batches or items. ISO 6206 3.7 batch definite quantity of material that may be one item or a number of items which belong together because of their manufacture or production under conditions which are presumed to be uniform ISO 6206 3.8 bulk sample collected set of samples which do
33、 not maintain their individual identity ISO 6206 3.9 incremental sample one of a series of samples taken during the sampling process NOTE Incremental samples may or may not retain their individual identity depending on the sampling instructions. BS604311:20022 Licensed Copy: Wang Bin, na, Thu Jun 07
34、 02:39:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSIISO 5262002:7)E( ISO 2002 r llAithgs reservde 3 3.10 final sample sample obtained or prepared under the sampling plan for possible subdivision into identical portions for testing reference or storage ISO 6206 3.11 laboratory sample sample as prepar
35、ed for sending to the laboratory and intended for inspection or testing ISO 6206 3.12 reference sample sample prepared at the same time as, and identical with, the laboratory sample, which is acceptable to the parties concerned and retained for use as a laboratory sample if a disagreement occurs ISO
36、 6206 3.13 spot sample sample of specified number or size taken from a specified place in the material or at a specified place and time in a stream of material and representative of its own immediate or local environment NOTE In English, the term “snap sample” is sometimes used as a synonym for “spo
37、t sample”. ISO 6206 4 General procedures and precautions 4.1 Sampling methods Manual and automated sample-taking are equally acceptable. Details of the methods employed shall be described in the sampling report (see clause 10). 4.2 Contamination of sample or of pitch being sampled The sampling proce
38、dure shall not cause contamination of the sample or of the pitch being sampled. Sample containers, sampling apparatus and any ancillary gear shall be dry. Sample containers, sampling apparatus, any ancillary gear, the hands and gloves and the protective clothing of the sampler shall be clean. Pitch
39、undergoes slow surface oxidation in the presence of air. Finely divided products, because of their large surface area per unit mass, may show a significant rise in softening point even if stored for only a short time. It is recommended therefore that finely divided reference samples be prepared for
40、storage by melting and resolidifying as follows. a) Place a sufficient amount of the powdered sample in a suitable container with a loose-fitting lid in an oven controlled at approximately above the expected softening point of the pitch. Leave in the oven for at this temperature. After heating, the
41、surface of the melt should be smooth, shiny and free of skin. b) If the surface of the melt is covered with froth, suggesting the presence of water, discard it and prepare another melt using a further portion of the sample which has first been dried by allowing it to stand in an evacuated desiccator
42、 in the presence of a suitable desiccant for approximately . 50 C2 h 2h BS604311:20023 Licensed Copy: Wang Bin, na, Thu Jun 07 02:39:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSIISO :7526(2002)E 4 ISO 2002 Ar llithgr seresvde c) Pour the molten pitch without turbulence, so as to avoid entrapping air
43、 bubbles, into an air-tight metal container, allowing it to solidify and seal the container. d) Note any froth formation during melting in the sample report and, in such cases; retain a separate portion of the finely-divided sample, stored in a sealed air-tight container, for the determination of wa
44、ter content. If a sample container is opened, it shall be securely closed again as soon as possible and any damaged sealing rings shall be replaced. 4.3 Sampling for the determination of water content of pitch in solid form For bulk shipments of solid pitch, a series of spot samples shall be taken f
45、or determination of water content, either from the conveying system during charge or discharge, or from the hold or compartment, or lorry at the top, middle or bottom during charge or discharge. The individual samples shall be sealed immediately in air-tight containers and tested promptly to avoid l
46、oss of moisture. 4.4 Mass of laboratory and reference samples The mass of the laboratory and reference samples shall be at least three times the amount required for testing and shall never be less than unless otherwise agreed in accordance with an established quality procedure. The sample mass shall
47、 be included in the sampling report (see clause 10). The minimum recommended sample mass is . 4.5 Safety precautions Comprehensive safety instructions are given in ISO 3165. Attention is drawn in particular to the following. When sampling hot liquid pitch from large containers such as ships, road or
48、 rail tanks, the sampler shall closely follow the safety procedures laid down for that site or location. These procedures typically include protective equipment and guidelines on safe working practice. Avoid inhalation of pitch vapour and dust. Sampling from ships, road or rail vehicles shall be str
49、ongly discouraged when in motion or when motion is likely to begin. 4.6 Suspect consignment A consignment shall be considered suspect if: a) a container is damaged or defective; b) there is any doubt as to the nature of the contents of a container, for example because of the presence of an old label or incorrect markings; c) there is evidence of an unexpected lack of uniformity; d) there are ob
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