【AS澳大利亚标准】AS 1038.21.1.1-2008 Coal and coke-Analysis and testing Part 21.1.1 Higher rank coal and coke-Relative.doc

as 102008as 102008australian standardcoal and cokeanalysis and testingpart 21.1.1: higher rank coal and coke relative densityanalysis sample/density bottle methodthis australian standard was prepared by committee mn-001, coal and coke. it was approved on behalf of the council of standards australia on 7 october 2008.this standard was published on 30 october 2008.the following are represented on committee mn-001:australasian institute of mining and metallurgyaustralian coal associationaustralian coal preparation societyaustralian institute of energycsiro, energy technologydepartment of natural resources and mines, qldinstitution of engineers, australiaminerals council of australianational generators forumuniversity of newcastleuniversity of new south walesuniversity of queenslandthis standard was issued in draft form for comment as dr 08161.standards australia wishes to acknowledge the participation of the expert individuals that contributed to the development of this standard through their representation on the committee and through the public comment period.keeping standards up-to-dateaustralian standards are living documents that reflect progress in science, technology and systems. to maintain their currency, all standards are periodically reviewed, and new editions are published. between editions, amendments may be issued.standards may also be withdrawn. it is important that readers assure themselves they are using a current standard, which should include any amendments that may have been published since the standard was published.detailed information about australian standards, drafts, amendments and new projects can be found by visiting .austandards australia welcomes suggestions for improvements, and encourages readers to notify us immediately of any apparent inaccuracies or ambiguities. contact us via email at .au, or write to standards australia, gpo box 476, sydney, nsw 2001.as 102008australian standardcoal and cokeanalysis and testingpart 21.1.1: higher rank coal and coke relative densityanalysis sample/density bottle methodoriginated as part of as 1038.211983. previous edition as 102002. third edition 2008.copyright standards australiaall rights are reserved. no part of this work may be reproduced or copied in any form or by any means, electronic or mechanical, including photocopying, without the written permission of the publisher.published by standards australia gpo box 476, sydney, nsw 2001, australiaisbn 0 7337 8945 5prefacethis standard was prepared by the standards australia subcommittee on coal evaluation, under the supervision of the committee mn-001, coal and coke, as a revision of as 102002, coal and cokeanalysis and testing, part 21.1.1: higher rank coal and cokerelative densityanalysis sample/density bottle method.the objective of this standard is to provide those responsible for testing coal and coke with a standardized method for measuring the relative density using a density bottle, so that disputes can be minimized.this revision makes changes to the temperature of the water bath.the term informative has been used in this standard to define the application of the appendix to which it applies. an informative appendix is for information and guidance only.7as 102008contentspage1scope . .4 2referenced documents . 43definitions . 44principle . 45safety . 46reagents . 47apparatus . 58sample. 59calibration of density bottle . 510procedure . 611calculation . 612reporting of result. 613precision . 614test report . 7appendix a alternative methods for de-aerating the analysis sample. 8standards australiaaustralian standardcoal and cokeanalysis and testingpart 21.1.1: higher rank coal and cokerelative densityanalysis sample/density bottle method1 scopethis standard sets out a method for the determination of the relative density of higher rank coal and coke by a relative density bottle.2 referenced documentsthe following documents are referred to in this standard: as1038coal and cokeanalysis and testing1038.3part 3:proximate analysis of higher rank coal1038.4part 4:cokeproximate analysis1038.16 part 16:assessment and reporting of results2378density bottles2418coal and cokeglossary of terms2706numerical valuesrounding and interpretation of limiting values4264coal and cokesampling4264.1part 1:higher rank coalsampling procedures4264.2part 2:cokesampling proceduresas/nzs2243safety in laboratories (series)3 definitionsfor the purpose of this standard, the definitions given in as 2418 apply.4 principlethe mass of water displaced by a known mass of air-dry coal or coke is determined in a density bottle.5 safetyfor information on laboratory safety, reference should be made to the relevant parts ofas/nzs 2243.6 reagents6.1 distilled waterdistilled water or water of equivalent purity. standards a.au6.2 wetting agent solutiona solution of non-ionic liquid wetting agent prepared in either distilled or deionized water with a concentration of between 10 ml/l and 15 ml/l.7 apparatus7.1 density bottlea density bottle of 50 ml capacity, and conforming to as 2378 (see figure 1).7.2 water batha water bath with stirrer, thermostatically controlled to maintain a bath temperature of 30 1c.note: the water temperature should be kept constant throughout both stages of the procedure described in clauses 9 and 10. the actual temperature need not be reported with the result, as differences within this range are not significant.7.3 vacuum desiccator7.4 vacuum pumpcapable of evacuating the desiccator to 8 kpa.7.5 weighing devicea balance having a minimum capacity of 100 g and readable to the nearest 0.001 g.8 sample8.1 generalthe sample shall be the analysis sample prepared to a nominal top size of 212 m. sample preparation procedures are described in as 4264.1 and as 42 equilibrationthe moisture content of the sample shall be equilibrated with the laboratory atmosphere by exposure in a thin layer on a tray.the sample shall be thoroughly mixed immediately before analysis.9 calibration of density bottlethe density bottle shall be calibrated regularly as follows:(a)fill the density bottle (7.1) to within 5 mm of the top with wetting agent solution(6.2).(b)place the bottle in the water bath (7.2), maintain the temperature as specified in clause 7.2, and allow to stand for at least 30 min or until air bubbles cease to rise through the liquid. tap the bottle gently to help to disperse any trapped air bubbles.(c)when the surface of the liquid is free from air bubbles, fill the density bottle with wetting agent solution.note: a beaker of wetting agent solution should be kept in the water bath.carefully insert the density bottle stopper, ensuring that no air bubbles remain trapped beneath the stopper. remove the drop of water from the top of the stopper with a piece of filter paper. (this should be done only once.) remove the density bottle and contents from the bath, and carefully wipe the bottle with a clean, dry cloth.(d)weigh, and record the mass (m1) of the density bottle with stopper and wetting agent solution.note: to avoid losses due to evaporation, this weighing should be carried out within 5 min of removal from the water bath.the initial calibration should be carried out in triplicate. the spread of the triplicate values shall be not greater than 0.005 g; otherwise, the entire calibration shall be repeated. regular verification of this calibration should be carried out. if there has been no change to the apparatus or concentration of the wetting agent, the initial calibration mass (m1) should continue to be used.10 procedurethe procedure shall be as follows:(a)weigh, to the nearest milligram, approximately 2 g of the sample and transfer it to the clean density bottle. record the mass (m) of the sample. concurrently, weigh out a sample for moisture determination by the method of as 1038.3 or as 1038.4.(b)add 10 ml to 15 ml of wetting agent to the density bottle and mix to ensure that the sample is wet. continue to add wetting agent to wash down the sides of the bottle (approximately 20 ml).(c)transfer the bottle and contents to the vacuum desiccator (7.3). connect the desiccator to the vacuum pump (7.4) and reduce the pressure in the desiccator to about 8 kpa, absolute. do not evacuate to below 7 kpa, as boiling and violent frothing may occur.note: other methods of de-aerating, such as boiling or vibrating with ultrasonic waves, may be used. these methods are described in appendix a.(d)remove the density bottle and contents from the desiccator and repeat steps 9(b)and 9(c).(e)weigh and record the mass (m2) of the density bottle with stopper, wetting agent solution, and sample.11 calculationthe result for relative density shall be calculated using the following equation:wherer elative density =mm + m1 m2. . . (1)m= mass of sample, in gramsm1 = mass of stoppered density bottle, completely filled with wetting agent solution, in grams (mean of triplicate results determined during calibration)m2 = mass of stoppered density bottle, plus wetting agent solution, plus sample, in grams12 reporting of resultthe result, the mean of duplicate determinations, for relative density, shall be reported to the nearest 0.01, rounded in accordance with as 2706.13 precisionthe values of repeatability and reproducibility should not exceed those give in table 1. otherwise reference shall be made to as 1038.16.14 test reportthe test report shall contain the following information: (a)complete identification of the sample tested.(b)reference to this australian standard, i.e. as 10.(c)the result of the determination including the basis of reporting, i.e. air-dry. (d)the moisture content of the sample.table 1precision data for relative density determinationrelative densityrepeatabilityrreproducibilityr30.030.080.08figure 1 typical density bottleappendix aalternative methods for de-aerating the analysis sample(informative)a1 method 1boiling a1.1 apparatusthe following apparatus is required:(a)glycerine batha suitable vessel in which sufficient glycerine can be heated for the lower two-thirds of the density bottle to be immersed.(b)air condensera glass tube of approximate length 1 m which may be attached to the top of the density bottle.a1.2 procedurethe procedure is as follows:(a)attach the air condenser (a1.1(b) to the neck of the bottle with rubber tubing, and immerse the bottle in a glycerine bath (a1.1(a).(b)heat the bath so that the water in the bottle begins to boil vigorously. (c)wash down any scum with a few millilitres of the hot, air-free water.(d)after 30 min boiling, remove the bottle from the glycerine bath, detach the air condenser and allow the bottle to cool.a2 method 2ultrasonic vibrating a2.1 apparatusan ultrasonic bath with timer.a2.2 procedurethe procedure is as follows:(a)add sufficient water to the ultrasonic bath to immerse the density bottle to the bottom of its neck.(b)place the density bottles in the bath, and vibrate until free of air bubbles. (c)remove the density bottles and allow to cool.standards australiastandards australia develops australian standards and other documents of public benefit and national interest. these standards are developed through an open process of consultation and consensus, in which all interested parties are invited to participate. through a memorandum of understanding with the commonwealth government, standards australia is recognized as australias peak non-government national standards body. standards australia also supports excellence in design and innovation through the australian design awards.for further information visit .auaustralian standardscommittees of experts from industry, governments, consumers and other relevant sectors prepare australian standards. the requirements or recommendations contained in published standards are a consensus of the views of representative interests and also