1、BS ISO7404-5:2009ICS 73.040NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDMethods for thepetrographic analysisof coalsPart 5: Method of determiningmicroscopically the reflectance ofvitriniteThis British Standard was published under the authority of the Standard
2、s Policy and Strategy Committee on 30 November 2009. BSI 2009ISBN 978 0 580 56505 2Amendments/corrigenda issued since publicationDate CommentsBS ISO 7404-5:2009National forewordThis British Standard is the UK implementation of ISO 7404-5:2009. Itsupersedes BS 6127-5:1995 which is withdrawn.The UK pa
3、rticipation in its preparation was entrusted to TechnicalCommittee PTI/16, Solid mineral fuels.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 responsibl
4、e for its correct application. Compliance with a British Standard cannot confer immunityfrom legal obligations.BS ISO 7404-5:2009Reference numberISO 7404-5:2009(E)ISO 2009INTERNATIONAL STANDARD ISO7404-5Third edition2009-10-01Methods for the petrographic analysis of coals Part 5: Method of determini
5、ng microscopically the reflectance of vitrinite Mthodes danalyse ptrographique des charbons Partie 5: Dtermination au microscope du pouvoir rflecteur de la vitrinite BS ISO 7404-5:2009ISO 7404-5:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing
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10、Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2009 All rights reservedBS ISO 7404-5:2009ISO 7404-5:2009(E) ISO 2009 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3 Defi
11、nitions 1 4 Principle .1 5 Reagents and materials 2 6 Apparatus.3 7 Preparation of coal sample 7 8 Procedure.7 9 Reporting of results 10 10 Precision 12 11 Test report13 Bibliography14 BS ISO 7404-5:2009ISO 7404-5:2009(E) iv ISO 2009 All rights reservedForeword ISO (the International Organization fo
12、r Standardization) is a worldwide federation 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
13、 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 closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Internati
14、onal 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 International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication
15、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 document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
16、ISO 7404-5 was prepared by Technical Committee ISO/TC 27, Solid mineral fuels. This third edition cancels and replaces the second edition (ISO 7404-5:1994), which has been technically revised. ISO 7404 consists of the following parts, under the general title Methods for the petrographic analysis of
17、coals: Part 1: Vocabulary1) Part 2: Methods of preparing coal samples Part 3: Method of determining maceral group composition Part 4: Method of determining microlithotype, carbominerite and minerite composition1) Part 5: Method of determining microscopically the reflectance of vitrinite 1) Parts 1 a
18、nd 4 of this International Standard will be available under the original title, Methods for the petrographic analysis of bituminous coal and anthracite, until the revisions of these documents have reached the stage at which they are publicly available. BS ISO 7404-5:2009ISO 7404-5:2009(E) ISO 2009 A
19、ll rights reserved vIntroduction Petrographic analyses have been recognized internationally as important in the context of the genesis, vertical and lateral variation, continuity, metamorphism and usage of coal. The International Committee for Coal and Organic Petrology (ICCP) has made recommendatio
20、ns concerning nomenclature and analytical methods and has published a comprehensive handbook that is continuously updated. The text of this part of ISO 7404 agrees substantially with the text of the handbook and incorporates many useful comments made by members of the ICCP and by member bodies of IS
21、O/TC 27, Solid mineral fuels. Petrographic analyses of single seam coals provide information about the rank, the maceral and microlithotype compositions and the distribution of minerals in the coal. The reflectance of vitrinite is a useful measure of coal rank and can provide information on the dist
22、ribution of coals of different rank in a coal blend. Together with a maceral group analysis, it provides information about some important chemical and technological properties of the coal and the coal blend. The reflectance of vitrinite has various other applications, such as the characterization of
23、 bulk samples and cargoes. For coal blends, the measurement of the vitrinite reflectance profile can permit the identification of the component coals and permit the estimation of the relative abundance of the component coals within the blend. ISO 7404 (all parts) is concerned with the methods of pet
24、rographic analysis currently employed in characterizing coal in the context of their technological use. The method of determining the reflectance of vitrinite is applicable for low-, medium- and high-rank coals7. The properties of a given coal are determined by the proportions and associations of th
25、e macerals and minerals present (see ISO 7404-33) and by the rank of the coal and thus its type, grade and rank. The reflectance of the vitrinite in the coal can be used as an indicator of rank, independent of the petrographic composition. Vitrinite reflectance increases progressively with rank. The
26、 reflectances of the macerals of the vitrinite group can vary significantly in a single coal seam and therefore the value of the reflectance obtained depends also on the choice of the macerals used for measurement. Reflectance measurements are made on one or more of the macerals of vitrinite and, in
27、 reporting the results, it is necessary to specify the macerals on which the measurement were made and the proportions of the overall value contributed by each of the macerals measured. Consequently, a vital step in the measurement of vitrinite reflectance is the identification of vitrinite and its
28、various macerals or maceral varieties. For this purpose, reference can be made to ISO 7404-1 and the ICCP1handbook. For rank determination of single-seam coals, normally the reflectance of collotelinite (eu-ulminite6in lignites, the equivalent of low-rank B and C6) is determined. In cases where coll
29、otelinite (or in low-rank coals, eu-ulminite) is not present in sufficient amounts, reflectance analysis on other vitrinite macerals is performed. Reflectance analysis on various vitrinite macerals can also be applied for technological purposes and to coal blends; see 8.3.1. The reflectance value ob
30、tained also depends on whether maximum or random reflectance measurements are made, so it is necessary to specify the type of measurement. All of these analysis procedures are applicable to single-coal seams or to blends providing that adequate (see 8.3.1) reflectance measurements are made in compli
31、ance with an unbiased sampling procedure on a representative sample. An accreditation programme for vitrinite reflectance analysis of single-seam coals (SCAP) is run regularly by the ICCP for accrediting petrologists. NOTE As this edition of ISO 7404 covers coals of all rank, the term “vitrinite” as
32、 used in this part of ISO 7404 includes vitrinite as well as huminite. Reference can be made to ISO 7404-1 for details. The equivalent to collotelinite in lignites is ulminite B. Reflectance measurement on lignites is performed on huminite. BS ISO 7404-5:2009BS ISO 7404-5:2009INTERNATIONAL STANDARD
33、ISO 7404-5:2009(E) ISO 2009 All rights reserved 1Methods for the petrographic analysis of coals Part 5: Method of determining microscopically the reflectance of vitrinite 1 Scope This part of ISO 7404 specifies the methods for determining the reflectance of vitrinite of coals microscopically on the
34、polished surfaces, immersed in oil. The methods are applicable to coals from single seams or coal blends covering the whole range of low-, medium- and high-rank coal. Vitrinite reflectance measurements can be used to characterize the components within blends. Measures can be taken to correct for the
35、 vitrinite percentage within each of the components of the blend or to determine the proportion of components in a blend, particularly when the components have dissimilar vitrinite contents. This method necessitates the identification of vitrinite by the analyst. Reflectance measurements on vitrinit
36、e obtained by interpreting the results from an automated system, are outside the scope of this part of ISO 7404. 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 referen
37、ces, the latest edition of the referenced document (including any amendments) applies. ISO 7404-1, Methods for the petrographic analysis of bituminous coal and anthracite Part 1: Vocabulary ISO 7404-2, Methods for the petrographic analysis of coals Part 2: Methods of preparing coal samples 3 Definit
38、ions For the purposes of this document, the definitions given in ISO 7404-1 apply. 4 Principle The intensity of light reflected at near-normal incidence from a specified area of well polished vitrinite under oil immersion, measured at 546 nm using a photomultiplier (or similar device), is compared w
39、ith the intensity of light reflected under identical conditions from a number of standards of known reflectance. Different vitrinite particles within a single-coal seam invariably differ slightly from one another in optical properties. Therefore, an adequate number (see 8.3.1) of readings on differe
40、nt particles is taken to ensure that the results are representative of the coal or coal blend. BS ISO 7404-5:2009ISO 7404-5:2009(E) 2 ISO 2009 All rights reserved5 Reagents and materials 5.1 Immersion oil, non-drying, non-corrosive type, with a refractive index of 1,518 0 0,000 4 at 23 C and a wavel
41、ength of 546 nm. Oil from a bottle opened more than one year ago should not be used. In attempts to produce oils that are chemically and physically stable, toxic compounds such as polychlorinated bi-phenyls were used in some older products. Some more recent oils have been associated with allergies.
42、The composition of the oil should, therefore, be checked to ensure that no toxic or other undesirable properties are associated with it. 5.2 Calibration standards 5.2.1 Reflectance standards, consisting of polished surfaces of materials that a) are isotropic (or basal sections of uniaxial minerals);
43、 b) are durable and resistant to corrosion; c) have a reflectance that is stable over a long period; d) are free from inclusions, grain boundaries, discontinuities, internal flaws and fractures; e) have negligibly low absorptance. To avoid significant amounts of light other than that reflected from
44、the top surface returning to the objective, the body of the standard shall be either thicker than 5 mm or wedge-shaped. The lower surface shall be matt if it makes an angle of less than 10 with the upper polished surface. The sides shall be shielded from external light. The reflectance of the standa
45、rds shall be of an order similar to that of the coal being measured. Use at least two such standards with well spaced reflectances. If a coal with a reflectance greater than 2,0 % is being measured, use one or more additional standards with reflectance greater than 2,0 %. Table 1 gives approximate m
46、ean values for reflectance standards or reflectance ranges as found between different standards, as calibrated against an ICCP Master Standard (see Note 2) in common use. NOTE 1 For measuring a vitrinite reflectance of about 1,0 %, a standard with reflectance below and a standard with reflectance ab
47、ove 1% are used. NOTE 2 An ICCP round robin exercise on reflectance standards demonstrated that variations between standards of nominally identical reflectances can be significant9; since then, the ICCP has offered the calibration of standards against ICCP master standards. NOTE 3 It is necessary th
48、at standards be carefully cleaned to avoid scratching the polished surface. If solvents are used to remove old oil, it is necessary to take care that the evaporation of the solvent does not leave a residue on the surface of the standard. Tarnishing can also occur with some standard materials, partic
49、ularly glasses. When the surface becomes scratched, or when comparison with the other standards shows that the reflectance value has changed, polishing is necessary. 5.2.2 Calculation of reflectance standards Some sources4recommend calculating the reflectance, R, of a standard as given in Equation (1): ()()2222221,5181001,518nnRnn+=+(1) where BS ISO 7404-5:2009ISO 7404-5:2009(E) ISO 2009 All rights reserved 3n is the known refractive index of the standard material at a wavelength of 546 nm; is the known
