BS ISO 501-2012 Hard coal Determination of the crucible swelling numbe《硬煤 坩埚膨胀指数的测定》.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 501:2012Hard coal Determination ofthe crucible swelling numberBS ISO 501:2012 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 501:20

2、12. Itsupersedes BS 1016-107.1:1991 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PTI/16, Solid mineral fuels.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include

3、 all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2012. Published by BSI StandardsLimited 2012ISBN 978 0 580 73550 9ICS 73.040Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Sta

4、ndard was published under the authority of theStandards Policy and Strategy Committee on 31 August 2012.Amendments issued since publicationDate T e x t a f f e c t e dBS ISO 501:2012 ISO 2012Hard coal Determination of the crucible swelling numberHouille Dtermination de lindice de gonflement au creus

5、etINTERNATIONAL STANDARDISO501Fourth edition2012-09-01Reference numberISO 501:2012(E)BS ISO 501:2012ISO 501:2012(E)ii ISO 2012 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2012All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any for

6、m or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-

7、mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 501:2012ISO 501:2012(E) ISO 2012 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Principle 14 Preparation of the test sample . 15 Apparatus . 16 Preparation of apparatus 37 Procedure. 58 Expression

8、 of results 79 Precision of the method 79.1 Repeatability . 79.2 Reproducibility . 710 Test report . 7BS ISO 501:2012ISO 501:2012(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Inter

9、national 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 committee. International organizations, governmental and non-governmental, in liaison wit

10、h 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 accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical

11、committees is to prepare International Standards. 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 drawn to th

12、e 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.ISO 501 was prepared by Technical Committee ISO/TC 27, Solid mineral fuels, Subcommittee SC 5, Methods of analysis.This fourth

13、 edition cancels and replaces the third edition (ISO 501:2003), which has been technically revised.iv ISO 2012 All rights reservedBS ISO 501:2012INTERNATIONAL STANDARD ISO 501:2012(E)Hard coal Determination of the crucible swelling numberWARNING Use of this International Standard can involve hazardo

14、us materials, operations and equipment. This International Standard does not purport to address all of the safety issues associated with its use. It is the responsibility of the user of this International Standard to establish appropriate safety and health practices and determine the applicability o

15、f regulatory limitations prior to use.1 ScopeThis International Standard specifies a method for determining the swelling properties of hard coal when heated in a covered crucible. NOTE The “crucible swelling number” (CSN) is also known as the “free swelling index” (FSI).2 Normative referencesThe fol

16、lowing 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 13909-4, Hard coal and coke Mechanical sampling Part

17、4: Coal Preparation of test samplesISO 18283, Hard coal and coke Manual sampling3 PrincipleA sample of coal is heated in a covered crucible under standard conditions of time and temperature. The shape of the coke button obtained is classified by comparison with the outlines of a set of standard prof

18、iles.4 Preparation of the test sampleThe test sample shall be the general analysis test sample prepared in accordance with ISO 13909-4 and ISO 18283. Ensure that the moisture content of the sample is in equilibrium with the laboratory atmosphere, exposing it, if necessary, in a thin layer for the mi

19、nimum time required to achieve equilibrium.The sample used for the crucible swelling number (CSN) test should be ground to pass a 212 m sieve. Avoid very fine grinding, as CSN can be adversely affected with pulverization level. Once the sample is prepared to this size specification, the test should

20、be performed within 24 h in order to avoid oxidation and a potentially misleading CSN result.5 Apparatus5.1 Crucible and lid (see Figure 1): silica crucible, squat form, and silica lid with ring handle. ISO 2012 All rights reserved 1BS ISO 501:2012ISO 501:2012(E)The crucible shall conform to the fol

21、lowing specifications:External height: 26 1,0 mmExternal diameter at top: 41 1,0 mmInternal diameter at base: 14 3,0 mmMass: 12 1,0 gCapacity: 16 ml to 17,5 mlDimensions in millimetresKey1 flat surface required2 lid3 crucibleFigure 1 Crucible with lid for swelling test2 ISO 2012 All rights reservedB

22、S ISO 501:2012ISO 501:2012(E)5.2 Pierced silica lid (see Figure 2), similar to that described in 5.1 but with a 6 mm hole through which the thermocouple (5.7) can pass.Dimensions in millimetresFigure 2 Pierced crucible lid5.3 Triangle, consisting of silica tubing of 6 mm to 6,5 mm external diameter,

23、 mounted on nickel/chromium wire, or formed of solid silica, the length of each side being approximately 55 mm to 60 mm.5.4 Burner, capable of giving the required standard heating conditions.For coal gas with a calorific value of approximately 20 MJ/m3, a Teclu-type burner having a burner tube with

24、an internal diameter of approximately 12,5 mm has been found satisfactory. For natural gas or LPG with a calorific value of approximately 30 MJ/m3to 40 MJ/m3, a Teclu- or Meker-type burner could be used. For these types of gases, the diameter of the burner tube or burner grid should be approximately

25、 30 mm.Alternatively, an electrical heating system may be used, provided that it has been shown to give results within 1/2 unit of that obtained with the gas heating method over the whole range of swelling numbers.5.5 Gauge, for measuring gas pressure.5.6 Draught shield, made from refractory piping

26、approximately 150 mm in length, of 100 mm internal diameter and 110 mm external diameter. At one end, the piping shall have three slots 25 mm deep in which the wire portions of the silica triangle rest (5.3) (see Figure 3).5.7 Thermocouple, sheathed, of fine wire of diameter not greater than 0,5 mm

27、if made of noble metals, or 0,8 mm if made of base metal.5.8 Weight, of mass 500 g 10 g.5.9 Sight tube, made of any rigid and opaque material, for viewing the coke buttons, to avoid the effect of parallax (see Figure 4).6 Preparation of apparatusAssemble the apparatus as shown in Figure 3. Place an

28、empty crucible (5.1) on the silica triangle (5.3) and support the crucible in the draught shield (5.6). Adjust the gas and air supplies to the burner (5.4), so that the temperature of the inner surface of the base of the crucible reaches 800 C 10 C in 1,5 min and 820 C 5 C in 2,5 min from first igni

29、ting the gas. Finally, heat a crucible in the apparatus for at least 5 min. Replace the crucible and check the temperatures again. Make any minor adjustments that are necessary to meet the standard conditions. ISO 2012 All rights reserved 3BS ISO 501:2012ISO 501:2012(E)If a Teclu-type burner is used

30、, a flame approximately 300 mm long, with the crucible positioned just above the tip of the blue cone, will generally be found to give the standard temperature conditions.If a Meker-type burner is used, place the crucible approximately 10 mm above the burner grid and adjust the flame so that the sta

31、ndard temperature conditions are attained.Measure the temperature using a thermocouple (5.7) inserted through the pierced lid (5.2) and having its unprotected junction and a portion of each wire in contact with the centre of the base of the empty crucible. A temperature of 800 C 10 C should be attai

32、ned after 1,5 min and one of 820 C 5 C after 2,5 min.Check the apparatus at frequent intervals to ensure that the standard conditions apply.Dimensions in millimetresKey1 pressure gauge graduated in kilopascalsFigure 3 Apparatus for the gas heating method4 ISO 2012 All rights reservedBS ISO 501:2012I

33、SO 501:2012(E)Dimensions in millimetresKey1 standard profile templateFigure 4 Sight tube apparatus7 ProcedurePreheat the apparatus for approximately 5 min.Weigh 1,00 g to 1,01 g of the freshly ground sample (see Clause 4) into a clean, dry crucible (5.1) and rotate the crucible if necessary while li

34、ghtly tapping it 12 times on the bench to level the surface of the coal. Cover the crucible with the unpierced lid and place the crucible upright on the silica triangle (5.3), supported in the draught shield (5.6). Light the gas and heat at the predetermined rate for such time as is required for the

35、 flame of the burning volatile matter to die out, and in any case for at least 2,5 min. Turn off the gas and allow the crucible to cool.Remove the residue carefully from the crucible.Perform the test in triplicate.If the residue is non-coherent, for example mostly loose powder, no further examinatio

36、n is needed and this result shall be designated as swelling number 0.If the residue is a coherent coke button but is not swollen, place the button onto a flat surface and rest the 500 g weight (5.8) on the button. If the button supports the 500 g weight without breaking into more ISO 2012 All rights

37、 reserved 5BS ISO 501:2012ISO 501:2012(E)than two hard pieces, designate the result as swelling number 1. If the button crumbles, disintegrates or breaks into more than two pieces, then designate the result as swelling number 1/2.If the coke button is swollen, compare the button with the standard nu

38、mbered profiles shown in Figure 5. The button can be examined through the sight tube apparatus (Figure 4) (optional) in order to avoid the effect of parallax. Rotate the button about the buttons vertical axis so that the largest profile of the button is presented for comparison; designate the result

39、 by the swelling number inscribed in the outline of the profile in Figure 5 which the button most nearly matches. For coke buttons that do not conform in shape to the standard profiles, the overlapping areas may be fitted by estimation into the uncovered areas of the standard profiles.IMPORTANT If p

40、rinting a copy of Figure 5 from an electronic version of this International Standard, ensure that no scaling or magnification is applied by selecting the print option “Actual size”, or “None” under page scaling. To verify that the printed copy is sized correctly, measure the 30 mm scale bar.Figure 5

41、 Determination of crucible swelling number Standard profiles (actual size) and corresponding swelling numbers (courtesy of British Standards)After each test, burn off the carbon residue, cool, and wipe the crucible and lid with a clean cloth.If the spread of values for an initial three determination

42、s is 1/2 or less, average the three values and report the average value. If the spread of values for an initial three determinations exceeds 1/2, carry out two more single determinations. If the five results agree to within one unit, average the five values and report the average value. If the five

43、results do not agree to within one unit, repeat the five determinations. From the 10 determinations, throw out the lowest value and the highest value, average the remaining eight values and report the average value.6 ISO 2012 All rights reservedBS ISO 501:2012ISO 501:2012(E)8 Expression of resultsRe

44、port the swelling number of the coal sample as follows:Swelling number 0: non-coherent residueSwelling number 1/2: non-swollen coke button that crumbles, disintegrates or breaks into more than two pieces under the 500 g weightSwelling number 1: non-swollen coke button that supports the 500 g weight

45、without breaking into more than two hard, coherent piecesSwelling number 1 1/2 to 9: number of the profile in Figure 5 that a swollen coke button most nearly matchesSwelling number greater than 9: profile exceeds that for swelling number 9Report the mean swelling number to the nearest 1/2 unit.NOTE

46、It is acceptable to report 1/2 as 0,5, and profiles greater than 9 as 9 or 9+.9 Precision of the method9.1 RepeatabilityThe range of the results of either three or five tests, carried out in the same laboratory by the same operator using the same apparatus on the same analysis sample, shall not exce

47、ed the values given in Table 1.9.2 ReproducibilityThe means of the five results obtained in each of two different laboratories on representative portions taken from the same sample after the last stage of sample preparation shall not differ by more than the values given in Table 1.Table 1 Precision

48、values for crucible swelling numberNumber of determinationsMaximum acceptable difference between resultsSame laboratory (Repeatability)Different laboratory (Reproducibility)3 determinations 1/2 5 determinations 1 110 Test reportThe test report shall include the following particulars:a) identificatio

49、n of the sample tested;b) a reference to this International Standard, i.e. ISO 501;c) result of the determination. ISO 2012 All rights reserved 7BS ISO 501:2012ISO 501:2012(E) ISO 2012 All rights reservedICS 73.040Price based on 7 pagesThis page deliberately left blankBSI is the independent national body responsible for preparing British Standards and other standards-related publications, information and services. It presents the UK view on standards in Europe and at the international