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1、International Standard 740412 0 +Qii 4 INTERNATIONAL ORGANIZATION FOR STANDARDIZATION*MEXKnYHAPOnHAR OPrAHMJAUMR I-IO CTAH,lAPTH3AUW4*ORGANlSATlON INTERNATIONALE DE NORMALISATION Methods for the petrographic analysis of bituminous coal and anthracite - Part 2: Method of preparing coal samples Mthode
2、s danalyse pktrographique des charbons bitumineux et de lanthracite - Partie 2: Pkparation dkchantillons de charbon First edition - 1985-04-15 G UDC 662.66 : 552 : 620.11 z Ref. No. IS0 7404/2-1985 (E) 1 Descriptors : minerals and ores, solid fuels, coal, bituminous coal, anthracite, tests, petrogra
3、phy, microscopic analysis, specimen preparation. k!? Price based on 8 pages Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 00:34:03 MDTNo reproduction or networking permitted wi
4、thout license from IHS -,-,- Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technical committees. Each member body interest
5、ed in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, govern- mental and non-governmental, in liaison with ISO, also take part in the work. Draft International Standards adopted by the technical committees
6、 are circulated to the member bodies for approval before their acceptance as International Standards by the IS0 Council. They are approved in accordance with IS0 procedures requiring at least 75 % approval by the member bodies voting. International Standard IS0 74C4/2 was prepared by Technical Commi
7、ttee ISO/TC 27, Solid mineral fuels. 0 International Organization for Standardization, 1999 0 Printed in Switzerland Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 00:34:03 MDTN
8、o reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD IS0 7404/2-1985 (El Methods for the petrographic analysis of bituminous coal and anthracite - Part 2: Method of preparing coal samples 0 Introduction 0.1 Petrographic analyses have been recognized inter- nat
9、ionally as important in the context of the genesis, vertical and lateral variation, continuity, metamorphism and usage of coal. The International Committee for Coal Petrology (ICCP) has made recommendations concerning nomenclature and analytical methods and has published an extensive handbook descri
10、bing in detail the characteristics of a wide range of coals. The text of this International Standard agrees substantially with the text of the handbook and incorporates many useful com- ments made by members of the ICCP and by member bodies of ISOITC 27, Solid mineral fuels. Petrographic analyses of
11、 a single coal provide information about the rank, the maceral and microlithotype compositions and the distribution of mineral matter in the coal. The reflec- tance of vitrinite is a useful measure of coal rank and the distribution of the reflectance of vitrinife in a coal blend, together with a mac
12、eral group analysis, can provide infor- mation about some important chemical and technological properties of the blend. This International Standard is concerned with the methods of petrographic analysis currently employed in characterizing bituminous coal and anthracite in the context of their techn
13、ological use. It establishes a system for petrographic analysis and comprises five parts, as follows: Part 1: Glossary of terms. Part 2: Method of preparing coal samples. Part 3: Method of determining maceral group composition. Part 4: Method of determining microlithotype compo- sition.) Part 5: Met
14、hod of determining microscopically the reflec- tance of vitrinite. For information on the nomenclature and analysis of brown coals and Iignites, reference should be made to the lnter- national Handbook of Coal Petrography published by the ICCP.2) 0.2 The varied petrographic composition and hardness
15、of coal and the type and amount of included mineral matter does not permit the formulation of a precise procedure which can be applied with equal success to.all types and ranks of coal. Within these limits, therefore, this part of IS0 7404 allows the operator to apply his individual skill and experi
16、ence to the preparation of a satisfactory polished surface. At the same time a recommended procedure, which has been found applicable to a wide variety of coals, is given in the annex. Many processes are involved between the mining of the coal and its preparation for industrial use. Petrographic ana
17、lysis may be required at any stage on samples from the coal seam in situ or from borehole cores, the raw product from the colliery, the products from the preparation plant or the final product. The amount and size distribution of the coal being investigated thus varies widely and it is important to
18、ensure that the sample obtained for petrographic analysis is fully representative. 1 Scope and field of application This part of IS0 7404 specifies a method for preparing a polished particulate block from a sample of crushed coal, for analysis by reflectance microscopy using white light. It does not
19、 apply to the preparation of polished particulate blocks for analysis using fluorescence microscopy techniques nor to the preparation of polished orientated lumps of coal. 2 References IS0 1988, Hard coal - Sampling. IS0 331011, Test sieves - Technicalrequiremants and testing - Part 1: Test sieves o
20、f metal wire cloth. IS0 740411, Methods for the petrographic analysis of bituminous coal and anthracite - Part 1: Glossary of terms. 1) At present at the stage of draft. 2) The second edition (19631, together with the supplement issued in 1971, may be obtained from Professor D.G. Murchison, Organic
21、Geochemistn/ Unit, Department of Geology, University of Newcastle, Newcastle-upon-Tyne, NE1 7RU, United Kingdom. The supplement issued in 1973 may be obtained from Centre national de la recherche scientifique, 15, quai Anatole-France, F-75997 Paris, France. 1 Copyright International Organization for
22、 Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 00:34:03 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 7404/Z-1985 (E) 3 Definitions For the purpose of this part of IS0 7404, the definit
23、ions of IS0 7404/l apply. It is recommended that aluminium oxide powders be used throughout and that an abrasive having a maximum particle size of 0,3 pm be used for the penultimate polishing stage. 5.5 Lap cloths: cotton, silk or synthetic fabric with a minimum of nap. 4 Principle The mixing of a r
24、epresentative sample of air-dried coal, crushed to a specified particle size, with a suitable binder. Formation of the mixture into a particulate block, one face of which is ground and polished to give a relief-free and scratch-free sur- face for analysis by reflectance microscopy. 5 Materials 5.1 B
25、inder, used to hold the particles of crushed coal together as a particulate block. The properties of the binder shall be such that: 6 Apparatus 6.1 Test sieve, of aperture 1,OO mm complying with the re- quirements of IS0 3310/l, with a suitable lid and receiver. 6.2 Grinding mill or pestle and morta
26、r, suitable for crushing 0,3 to 0,45 kg of coal to pass through the test sieve (6.1) with the minimum production of fines. The grinding mill may be manually or electrically operated. 6.3 Press, capable of producing a pressure of up to 17 MPa.” a) there shall be no chemical reaction with the coal or
27、This may be a simple hand operated lever, a torque-wrench or a immersion oil; hydraulic press. b) the temperature required to make the particulate block shall not exceed 100 OC and a temperature less than 60 OC is preferable; c) the surfaces of the coal particles shall be easily wetted and there sha
28、ll be good penetration of pores and cracks; d) the coal particles shall be held securely during grinding and polishing; e) there shall be a marked contrast with the coal particles when immersed in oil and focused under the microscope; f) the hardness shall be comparable with that of the coal so that
29、 a flat, relief-free and scratch-free surface can bdob- tained by grinding and polishing; g) there shall be no large volume changes during curing which might cause possible damage to the coal particles. 5.2 Mould release agent, which does not damage the mould or affect the coal or binder. 5.3 Grindi
30、ng abrasives. Silicon carbide papers of decreas- ing grain size. 5.4 Polishing abrasives. Metal oxide powders or diamond pastes of decreasing grain size. A metal oxide powder having a maximum particle size not exceeding 0.05 pm shall be used for the final polishing stage. NOTE - The number of polish
31、ing stages will depend on the grain size of the abrasive used at the final stage of grinding and on the grain size of the polishing abrasives available. 6.4 Metal mould, to hold the mixture of coal and binder during the curing process, with an ejector ring and plunger or other means of removing the
32、block from the mould after curing. (See note I.) The mould shall be capable of withstanding double the pressure normally applied in making the particulate block. The internal dimensions of the mould shall be such that the face of the block to be polished has a surface area of at least 600 mm*. NOTES
33、 1 The interior of the mould and the surface of the plunger should have a ground finish. 2 For reflectance analysis two blocks of minimum size may be necessary if the coal is deficient in vitrinite. The mould may be either cuboid or cylindrical provided that the block produced fits the holder of the
34、 grinding and polishing apparatus being used. 3 Figure 1 gives an example of the dimensions of a mould, plunger and ejector ring used to produce a block 40 mm in diameter. 6.5 Disposable containers, suitable for mixing the required amounts of coal and binder. NOTE - Wax coated containers are unsuita
35、ble 6.6 Grinding and polishing machine, with interchangeable lapping discs for each of the grinding and polishing stages. NOTE - The machine should be fitted with a contrarotating specimen holder of the type in which the specimen is held rigidly and is not free to rotate independently of the holder.
36、 The specimen holder should have a means of varying the load on the specimen. 1) 1 MPa = 106N/m2 2 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 00:34:03 MDTNo reproduction or
37、networking permitted without license from IHS -,-,- IS0 7404/2-1985 (El 6.7 Sample cleaner. Some means of cleaning the surface of the particulate block between the successive stages of grinding and polishing shall be available. Jets of tap water and distilled water are essential and, in addition, an
38、 ultrasonic cleaning bath, if available. NOTE - If necessary a cleaning filter should be used to remove solid particulates from the water supply before use in cleaning and polishing. 6.8 Desiccator. 2 The precise procedure for preparing a particulate block will depend on the type of binder, mould an
39、d press used. Provided that the materials and apparatus comply with the requirements of clauses 5 and 6, the steps in the procedure may be chosen by experiment. 3 An elevated temperature is used to speed the rate of cure of the binder. When rapid curing is not required, curing may be carried out at
40、ambient temperature provided that adequate time is allowed and all voids are eliminated. 4 A recommended procedure is given in the annex. 7.3 Preparation of polished surface of particulate block 7 Procedure 7.1 Preparation of coal sample for making particulate block 7.1.1 Subsample Obtain a represen
41、tative subsample of the coal to be examined. For most purposes it will be convenient to take this sample after the first stage in the preparation of the laboratory sample for general analysis in accordance with the requirements of IS0 1968. 7.1.2 Drying Air dry the subsample (7.1.1) in accordance wi
42、th the re- quirements of IS0 1988 to facilitate crushing and sample div- ision and to avoid interference with the curing of the binder in the preparation of the particulate block. 7.1.3 Size reduction Reduce the size of the particles to an upper limit of 1 mm. NOTE - The reduction in the size of the
43、 coarse particles should be car- ried out using a grinding mill (6.2) adjusted to give a product crushed to an upper size of I,00 mm with minimum production of fines. If a pestle and mortar (6.2) is used, sieve and grind the oversize repeatedly until all the coal just passes the specified size. 7.1.
44、4 Sample division Divide the subsample using a riffle or small rotary sample divider to obtain a laboratory sample of 50 to 100 g of coal in accordance with the requirements of IS0 1968. The laboratory sample may be stored in a screw-topped jar prior to analysis. 7.2 Preparation of particulate block
45、 The object is to prepare a particulate block of suitable thickness in which particles of coal are evenly dispersed in the resin such that at least 60 % of the cross-sectional area of the polished surface is coal. NOTES 1 This percentage will reduce the time of analysis and any tendency towards the
46、segregation of particles due to size and density. Grind and polish one end face of the particulate block using a grinding and polishing machine (6.6) and a series of abrasives of decreasing particle size. The block may be held manually or by means of the specimen holder. Suitable materials for both
47、grinding and polishing are described in 5.3 to 5.5, and A.2.3 to A.2.5. Carry out the final polish with a metal oxide powder having a maximum particle size not exceeding 0,05 pm. Thoroughly wash the surface of the block under a strong jet of water (6.7) after each stage of grinding and polishing. Im
48、mer- sion of the block in distilled water in an ultrasonic cleaning bath (6.7) is recommended for removing the debris remaining after the grinding stages. The removal of all traces of polishing abrasive from the block is essential and this may be achieved by wiping the surface with clean lens tissue
49、 or cotton wool whilst washing the surface under a strong jet of water. After the final washing rinse with a jet of distilled water. Dry the particulate block in a stream of clean air. NOTES 1 An electric hair-drier or fan assisted warm air chamber are suitable for this purpose. 2 A recommended polishing and grinding procedure is given in the annex. 7.4 Examination of the polished surface Examine the polished surface with a dry object