1、 Reference numberISO 10329:2009(E)ISO 2009INTERNATIONAL STANDARD ISO10329First edition2009-02-01Coal Determination of plastic properties Constant-torque Gieseler plastometer method Charbon Dtermination des proprits plastiques Mthode du plastomtre Gieseler couple constant ISO 10329:2009(E) PDF discla
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5、TED DOCUMENT ISO 2009 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs mem
6、ber body in the country of the requester. ISO copyright office Case postale 56 CH-1211 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 reservedISO 10329:2009(E) ISO 2009 All rights reserved iiiContents Pag
7、e Foreword iv 1 Scope . 1 2 Normative references . 1 3 Terms and definitions. 1 4 Principle. 2 5 Apparatus 2 6 Calibration . 3 7 Sample . 4 8 Procedure 4 9 Cleaning of the apparatus 10 10 Calculation and expression of results 10 11 Precision of the method. 11 ISO 10329:2009(E) iv ISO 2009 All rights
8、 reservedForeword 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 technical committees. Each member body interested in a subject for
9、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 closely with the International Electrotechnical Commission (IEC) on al
10、l 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 International Standards. Draft International Standards adopted by the technical committees are
11、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 document may be the subject of patent rights. ISO shall not be held res
12、ponsible for identifying any or all such patent rights. ISO 10329 was prepared by Technical Committee ISO/TC 27, Solid mineral fuels, Subcommittee SC 5, Methods of analysis. INTERNATIONAL STANDARD ISO 10329:2009(E) ISO 2009 All rights reserved 1Coal Determination of plastic properties Constant-torqu
13、e Gieseler plastometer method 1 Scope This International Standard specifies a method for obtaining a relative measure of the plastic behaviour of coal when heated under prescribed conditions. The method may be used to obtain values of the plastic properties of coals and blends used in carbonization
14、and in other situations where determination of plastic behaviour of coals is of practical importance. NOTE The empirical nature of this test requires proper equipment calibration to produce fluidity readings which are a true indication of the relative plastic behaviour of the coal. 2 Normative refer
15、ences 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 18283, Hard coal and coke Manual sampli
16、ng ISO 13909-1, Hard coal and coke Mechanical sampling Part 1: General introduction ISO 13909-2, Hard coal and coke Mechanical sampling Part 2: Coal Sampling from moving streams ISO 13909-3, Hard coal and coke Mechanical sampling Part 3: Coal Sampling from stationary lots 3 Terms and definitions For
17、 the purposes of this document, the following terms and definitions apply 3.1 dial division per minute measure of stirrer rotation rate, as used in this method NOTE There are 100 dial divisions for each full 360 rotation of the stirrer. The fluidity result is expressed as total dial divisions turned
18、 by the stirrer in a 1 min time period, i.e. dd/min. 3.2 initial softening temperature temperature at which dial movement or electronic readout indicates a stirring shaft movement of one dial division per minute (dd/min), with continued indication of movement of at least 1 dd/min thereafter 3.3 maxi
19、mum fluidity temperature temperature at which stirring shaft rotation reaches the maximum rate 3.4 plastic range difference between the initial softening temperature and the solidification temperature ISO 10329:2009(E) 2 ISO 2009 All rights reserved3.5 final fluidity temperature temperature at which
20、 the last 1 dd/min stirrer rotation rate is reached 3.6 solidification temperature temperature at which the stirring shaft stops 3.7 maximum fluidity maximum rate of rotation for the stirring shaft in dial divisions per minute 3.8 jamming swelling up of coal into the retort tube during the test, whi
21、ch may produce a lower fluidity result than expected and can only be noted after visual inspection of the disassembled crucible and retort at the conclusion of the test 3.9 breaking free spinning behaviour of coal, either by rotating at maximum motor speed or by abrupt changes in rotation, which occ
22、urs as a result of a molten ball of coal forming around the base of the stirrer, and which makes reporting of the true maximum fluidity of the coal difficult 4 Principle Measurements of the plastic properties of coals are made by applying a constant torque to a stirrer placed in a crucible into whic
23、h the coal is charged. The crucible is immersed in a bath and the temperature increased uniformly. The rotation of the stirrer is recorded in relation to increase in temperature. 5 Apparatus 5.1 Gieseler plastometer retort, composed of the following component parts (see Figure 1). 5.1.1 Retort cruci
24、ble, cylindrical, with (21,4 0,1) mm inside diameter, and (35,0 0,3) mm in depth with exterior threads for joining the crucible to the barrel. The crucible shall have a (2,38 0,02) mm diameter notch with an included angle of 70 in the centre of its inside base to serve as a seat for the stirrer. 5.1
25、.2 Retort crucible cover, with interior threads for joining the crucible cover to the crucible and exterior threads for joining the crucible cover to the barrel. The inside diameter of the hole which accommodates the stirrer shall be (9,5 0,1) mm. 5.1.3 Guide sleeve, provided near the upper end of t
26、he stirrer to guide the latter within the barrel with a clearance of between 0,05 mm and 0,10 mm. 5.1.4 Gas exit hole, provided on the barrel to afford an exit for the volatile products during a test, placed, for example, at the midpoint of the barrel; a tube may be fitted if desired. 5.1.5 Barrel,
27、(121,0 2,5) mm long, having an inside diameter of (9,5 0,1) mm. The top end of the barrel shall be 12,7 mm in inside diameter to a depth sufficient to allow the fitting of a guide sleeve through which the axle of the stirrer passes when the apparatus is assembled. ISO 10329:2009(E) ISO 2009 All righ
28、ts reserved 35.1.6 Steel stirrer, provided with a straight shaft (3,95 0,05) mm in diameter and equipped with four rabble arms. The lower end of the stirrer shall be tapered to a point having an included angle of 60. The rabble arms on the stirrer shall be (1,6 0,05) mm in diameter, (6,4 0,05) mm in
29、 length, and shall be placed so as to be perpendicular to the shaft at 90 intervals around the shaft and (3,2 0,05) mm apart centre to centre along the shaft. The middle two rabble arms shall be set at 180 to each other, and likewise, the remaining two arms at 180 to each other. The lowest rabble ar
30、m shall be set to give (1,6 0,05) mm clearance between it and the bottom of the crucible when the stirrer is in place. The upper end of the stirrer shall be cut to fit into a slot on the lower end of the axle in the plastometer head. The rabble arms should be checked before each test to ensure that
31、they are clean and free from distortion or other visual damage. It is essential that the dimensions of the rabble arms on the stirrer meet the requirements in this clause and in Figure 2, and it is important that these dimensions are checked on a regular basis, e.g. every 50 determinations. If after
32、 use it is found by accurate measurement that any of the dimensions are outside the specified limits, the rabble arms should be replaced or the stirrer discarded. 5.2 Plastometer head. The plastometer head, shown schematically in Figure 3, shall consist of a fixed-speed motor (approximately 300 r/mi
33、n to 500 r/min) connected directly to a magnetic clutch or hysteresis brake capable of adjustment over a reasonable range either side of a torque value of 101,6 gcm (9,66 Nm). A dial drum, attached to the clutch brake output shaft, shall be graduated into 100 divisions for 360 degrees. Each complete
34、 drum revolution or 100 dial divisions shall be recorded on a counter actuated by an electric eye or other suitable method. As an alternative, an electronic device capable of measuring rotation rates between 0,01 and 300 r/min may be attached to the clutch or brake output shaft. Using this latter te
35、chnique, rotation rates can be converted directly to dial divisions per minute (dd/min) and can be displayed or recorded once a minute on a suitable electronic readout or printer. NOTE Care is needed in the maintenance and lubrication of all bearings, particularly after the instrument has been used
36、with a coal high in volatile matter. Using bearings with a closed race is undesirable due to the increased friction of the closed race compared to bearings with an open race. When using open race bearings, clean and replace on a regular basis. 5.3 Electric Furnace. An electrically heated furnace sha
37、ll be used (see Figure 4) with suitable controls so that a heating rate of (3,0 0,1) C/min, on an overall basis, with not more than (3,0 1,0) C for any given minute, can be maintained over a temperature range from 300 C to 550 C with a (15 1) C rise over any given 5 min period. The furnace shall con
38、tain a molten solder bath of approximately 50 percent lead and 50 percent tin composition. The temperature in the bath shall be measured with a suitable thermocouple in a protection tube of approximately 6 mm in outside diameter immersed in the bath so that the tube touches the outside wall of the c
39、rucible and the hot junction of the thermocouple is at the same height as the centre of the coal charge. A stirrer shall be used to agitate the solder. 5.4 Loading device. The loading device shall be provided to pack the coal uniformly in the crucible under a total load of 10 kg and designed in such
40、 a manner that, after compression, the crucible and its contents can be removed easily from the device without disturbing the contents. A suitable device, such as shown in Figure 5, has a static weight of 9 kg together with a drop weight of 1 kg which is dropped twelve times from a height of 115 mm.
41、 NOTE The static weight of 9 kg is the combined mass of the cage, packing head, dropping mass shaft and the static mass. 6 Calibration Torque shall be checked with the string and pulley method shown in Figure 6. In the string and pulley method, a pulley is screwed onto the spindle and a string attac
42、hed to this pulley is placed over a second vertical pulley, with the required weight attached. A 25,4 mm (1 in) radius pulley and a 40 g weight have been used for that purpose. With the plastometer motor turned on, the brake or clutch suspension, or the torque gauge or ISO 10329:2009(E) 4 ISO 2009 A
43、ll rights reservedtransducer, reads (101,6 5,1) gcm (40,0 2,0) gin. All instruments should be checked in this manner as required, at a predetermined frequency based on the laboratorys experimentation on stability or torque setting. Alternatively, torque can be checked with a suitable gauge or transd
44、ucer provided it has been validated against the string and pulley method. If this method is used, the torque applied to the shaft is checked as a minimum at two positions at 90 to each other to check that the drive shaft alignment and bearings running is correct. If the torque values are different,
45、this indicates a problem that must be repaired, otherwise lower fluidity values will be recorded. NOTE A pulley/weight assembly is the only one capable of reliably evaluating the torque over a complete 360 rotation. 7 Sample Collect a representative gross sample of coal in accordance with ISO 18283,
46、 ISO 13909-1, ISO 13909-2 and ISO 13909-3. Approximately 4 kg of coal crushed to pass a 4,75 mm sieve shall constitute the laboratory sample. This sample should be representative of the batch being tested. Spread the laboratory sample on a tray and allow it to equilibrate with the laboratory atmosph
47、ere. Drying shall not be continued beyond this point so that the plastic properties of the coal are not altered by oxidation. The drying temperature shall not exceed 40 C. After air drying to equilibration, divide the sample representatively to about 500 g. Representatively subsample one quarter fro
48、m this 500 g portion then crush this one quarter in successive steps to pass a 425 m sieve in such a manner as to minimize the production of fines. This is done by alternatively screening and crushing the oversize material until no oversize material remains. The size reduction process should aim at
49、keeping the fines of less than 212 m in diameter to less than 50 % of the final sample. Thoroughly mix the sample, preferably by mechanical means, and withdraw not less than 5 g of this sample by increments. Test the coal for plastic properties by duplicate determinations within 8 h after preparing the sample passing a 425 m sieve. Avoid delays in performing the analysis so far as possible because the plastic properties of coal may be significantly affected by deteri
