1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Brown coals and lignites Determination of the yields of tar, water, gas and coke residue by low temperature distillationBS ISO 647:2017 ISO 2017Brown coals and lignites Determination of the yields of tar, water, gas and
2、 coke residue by low temperature distillationCharbons bruns et lignites Dtermination des rendements en goudron, en eau, en gaz et en rsidu de coke par distillation basse tempratureINTERNATIONAL STANDARDISO647Second edition2017-07Reference numberISO 647:2017(E)National forewordThis British Standard i
3、s the UK implementation of ISO 647:2017.The UK participation in its preparation was entrusted to Technical Committee PTI/16, Solid mineral fuels.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the nece
4、ssary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017 Published by BSI Standards Limited 2017ISBN 978 0 580 93624 1ICS 73.040Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was
5、published under the authority of the Standards Policy and Strategy Committee on 31 July 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS ISO 647:2017 ISO 2017Brown coals and lignites Determination of the yields of tar, water, gas and coke residue by low tempera
6、ture distillationCharbons bruns et lignites Dtermination des rendements en goudron, en eau, en gaz et en rsidu de coke par distillation basse tempratureINTERNATIONAL STANDARDISO647Second edition2017-07Reference numberISO 647:2017(E)BS ISO 647:2017ISO 647:2017(E)ii ISO 2017 All rights reservedCOPYRIG
7、HT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, witho
8、ut prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS I
9、SO 647:2017ISO 647:2017(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Reagents 16 Apparatus . 27 Preparation of test sample . 58 Procedure. 59 Expression of result . 710 Precision . 710.1 Repeatability limit 710.2 Reproducibility limit 811 Te
10、st report . 8 ISO 2017 All rights reserved iiiContents PageBS ISO 647:2017ISO 647:2017(E)ForewordISO (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
11、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 with ISO, also take part in the work. ISO coll
12、aborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approv
13、al criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).Attention is drawn to the possibility that some of the elements of this document may be the
14、subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www .iso .org/ patents).An
15、y trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs a
16、dherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .html.This document was prepared by Technical Committee ISO/TC 27, Solid minerals fuels, Subcommittee SC 5, Methods of analysis.This second edition c
17、ancels and replaces the first edition (ISO 647:1974), of which it constitutes a minor revision. The changes compared to previous edition are as follows: dated references and other minor items have been changed.iv ISO 2017 All rights reservedBS ISO 647:2017ISO 647:2017(E)IntroductionThe yield of dist
18、illation products by low temperature distillation, especially the yield of tar, forms the basis for the classification of brown coal and lignite for use in low temperature carbonization. ISO 2017 All rights reserved vBS ISO 647:2017BS ISO 647:2017Brown coals and lignites Determination of the yields
19、of tar, water, gas and coke residue by low temperature distillation1 ScopeThis document specifies a method for the determination of the yields of tar, water, gas and coke residue obtained from brown coal and lignite by distillation to a final temperature of 520 C.2 Normative referencesThe following
20、documents are referred to in the text in such a way that some or all of their content constitutes requirements 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 5068-2,
21、Brown coals and lignites Determination of moisture content Part 2: Indirect gravimetric method for moisture in the analysis sampleISO 1170, Coal and coke Calculation of analyses to different bases3 Terms and definitionsNo terms and definitions are listed in this document.ISO and IEC maintain termino
22、logical databases for use in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp4 PrincipleThe sample is heated in an aluminium retort to a temperature of 520 C during a
23、 period of 80 min. The products of decomposition pass into a water-cooled receiver. The tar and water are condensed while gaseous products pass to atmosphere. The coke residue remaining in the retort is weighed. The receiver and its contents are also weighed and the mass of the water in it determine
24、d by entrainment with toluene or xylene. The mass of tar is obtained by difference.The total water in the receiver includes the moisture in the coal as well as that from the decomposition of the coal. A separate determination of moisture in the coal is made so that the decomposition water can be cal
25、culated.The percentage of gas (plus errors) is obtained by subtracting from 100 the sum of the percentages of coke residue, tar and total water. The results are reported on the “as analysed” basis and on the “dry” basis. 5 Reagents5.1 Graphite paste.Ground dry and made into suitable paste with water
26、 or thick lubricating oil.INTERNATIONAL STANDARD ISO 647:2017(E) ISO 2017 All rights reserved 1BS ISO 647:2017ISO 647:2017(E)5.2 Xylene.Boiling point 135 C to 140 C.5.3 Toluene.Boiling point 110 C.6 Apparatus6.1 Retort.Made of aluminium, with the dimensions shown in Figure 1. With the cover fitted,
27、its capacity with the outlet tube shall be 170 ml 10 ml. The outlet tube shall be made of brass and its internal wall shall be clean and polished. A new assembly shall be heated at 520 C for 20 min before use.If, through wear, the upper edge of the conical portion of the cover is below the top surfa
28、ce of the retort, its free volume will be less than 160 ml and a new cover is required. The new oversize cover shall be ground so that when fitted, the upper edge of the round portion is less than 7 mm above the top surface of the retort. This will ensure that the free volume of the retort does not
29、exceed 180 ml.2 ISO 2017 All rights reservedBS ISO 647:2017ISO 647:2017(E)Dimensions in millimetresMaterials: Aluminium retort, aluminium content 99 %Volume of retort: 170 ml 10 mlOutlet tube: BrassKeyA screw threadB bearer barC depth of hole for the thermometerD coverE as in Figure 2 a)F as in Figu
30、re 2 b)Figure 1 Retort6.2 Furnace.Heated either electrically or by gas. For electrical heating, a resistance wire furnace or a silicon carbide rod furnace may be used. ISO 2017 All rights reserved 3BS ISO 647:2017ISO 647:2017(E)6.3 Thermocouple and millivoltmeter or nitrogen-filled mercury thermomet
31、er.Calibrated and capable of indicating temperatures up to 550 C.A new thermometer shall be aged and then calibrated before use and shall be rechecked at intervals of one month by comparing it with a standard thermometer in a manner approved by a national testing authority.6.4 Receiver.Round-bottome
32、d glass flask, capacity 750 ml, with conical ground joint and with either long or short neck depending on the method of connection to the retort (see Figure 2), provided with a rubber or glass stopper.Dimensions in millimetresKey1 retort with gas outlet tube 7 cooling bath2 extent of heating furnace
33、 8 outlet3 gas outlet tube 9 cold water4 heat resistant stopper 10 glass adapter tube5 level of cooling water 11 ground joint6 receiverFigure 2 Arrangement of the receiver in the cooling bath4 ISO 2017 All rights reservedBS ISO 647:2017ISO 647:2017(E)6.5 Cooling bath.The distance between the receive
34、r and the walls of the bath is not less than 20 mm. The water flow shall be adjusted to maintain a temperature of between 10 C and 15 C in the bath.6.6 Distillation apparatus.Composed of condenser, graduated tube for measurement of water and distillation flask. All parts are connected by means of gr
35、ound glass joints.7 Preparation of test sampleSpread the laboratory sample on a tray and allow it to attain approximate moisture equilibrium with the atmosphere. Carefully crush the sample so that at least 90 % passes through a sieve of 1 mm aperture while not more than 50 % passes through a sieve o
36、f 0,2 mm aperture. If the moisture content of the crushed sample is still greater than 20 %, further air-drying should be carried out to reduce the moisture content to between 10 % and 20 %. The test sample may be stored in a hermetically sealed container. Alternatively, the sample may be kept for a
37、 period not longer than 1 week in a stoppered container filled to more than 80 % of its capacity.NOTE When samples are kept for longer than 1 week in containers which are not hermetically sealed or are not entirely filled, the loss of tar yield can be up to 0,5 % and in certain cases, the loss can b
38、e considerably greater.8 ProcedureWeigh, to the nearest 0,05 g, about 50 g of the test sample and transfer it completely to the retort. Lightly smear the conical portion of the cover with the graphite paste, replace the cover and seal by rotating it. Determine the moisture content of the test sample
39、 at the same time by the method given in ISO 5068-2.Weigh the receiver and stopper to the nearest 0,05 g and connect the receiver to the outlet tube of the retort by means of either a heat resistant stopper see Figure 2 a) or a glass adapter tube see Figure 2 b). In the latter case, insert the brass
40、 outlet tube about 8 mm into the glass adapter tube and seal it to it by means of a short length of rubber tubing. Wind the joint with cotton, asbestos, linen, filter paper or similar material and cool by a stream of water while the retort is being heated. Place the retort in the furnace and the rec
41、eiver in the cooling bath and ensure that the apparatus is gastight. It is necessary to pre-heat certain types of furnaces in order to reach 220 C within 10 min of inserting the retort, and the receiver shall be immersed in the cooling bath as far as possible, but the rubber stopper or the ground jo
42、int shall not touch the water. Start the flow of water through the cooling bath and heat the retort according to the specification of Table 1.Table 1 Specification of heating the retortTime from startminTemperatureC10 22020 31030 38040 44050 48060 50570 52080 520Maintain the rate of heating within t
43、he limits shown in Figure 3. ISO 2017 All rights reserved 5BS ISO 647:2017ISO 647:2017(E)KeyX time, minutesY temperature, C1 temperature graph against time2 limitsNOTE 1 Total time for low temperature distillation between 20 C and 520 C: 80 min.NOTE 2 Effective time for low temperature distillation
44、between 310 C and 520 C: 60 min.Figure 3 Schedule of heatingAt the end of the above period, stop the heating and remove the retort from the furnace with the receiver still connected. Allow to stand for 10 min to enable the tar collected in the outlet tube to trickle down into the receiver. Disconnec
45、t the receiver from the retort and, if necessary, transfer the remaining tar from the outlet tube into the receiver with a small spatula. Only a very small residue of tar will be found in a clean smooth brass tube. Close the receiver and the outlet tube of the retort with stoppers and cool the retor
46、t to room temperature. Remove the coke residue carefully and weigh it to the nearest 0,05 g in a previously counterpoised weighing bottle.Wipe off adhering water from the outside of the receiver and re-weigh to obtain the mass of the tar plus total water. Add 200 ml of toluene or xylene to the recei
47、ver and determine the total water content by entrainment using the distillation apparatus (6.6).6 ISO 2017 All rights reservedBS ISO 647:2017ISO 647:2017(E)9 Expression of resultThe yields on the “as analysed” basis are given by Formulae (1) to (4):CRmm=40100 (1)Tarmmmm=()2130100 (2)DWmmM=30100 (3)G
48、asCRTar DWMmmmmm= +()=+10010012400(4)wherem0is the mass of sample, in grams;m1is the mass of empty receiver and stopper, in grams;m2is the mass of receiver and stopper, plus tar, plus total water, in grams;m3is the mass of total water determined by entrainment, in grams;m4is the mass of coke residue
49、, in grams;M is the moisture content of the sample, in mass percent;CRis the coke residue yield of the sample, in mass percent;Taris the tar yield of the sample, in mass percent;DWis the decomposition water yield of the sample, in mass percent;Gasis the gas yield of the sample, in mass percent.The result, preferably the mean of duplicate determinations (see Clause 10), should be reported to the nearest 0,1 %. Values for tar, coke residue, decomposition water and
