1、BSI Standards Publication WB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06 Brown coals and lignites Determination of the yields of tar, water, gas and coke residue by low temperature distillation BS ISO 647:2017 ISO 2017 Brown coals and lignites Determination of the yields of tar, water, gas
2、 and coke residue by low temperature distillation Charbons bruns et lignites Dtermination des rendements en goudron, en eau, en gaz et en rsidu de coke par distillation basse temprature INTERNATIONAL STANDARD ISO 647 Second edition 2017-07 Reference number ISO 647:2017(E) National foreword This Brit
3、ish Standard is 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 inc
4、lude all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017 Published by BSI Standards Limited 2017 ISBN 978 0 580 93624 1 ICS 73.040 Compliance with a British Standard cannot confer immunity from legal obligations. This
5、British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 July 2017. Amendments/corrigenda issued since publication Date Text affected BRITISH STANDARD BS ISO 647:2017 ISO 2017 Brown coals and lignites Determination of the yields of tar, water, gas and c
6、oke residue by low temperature distillation Charbons bruns et lignites Dtermination des rendements en goudron, en eau, en gaz et en rsidu de coke par distillation basse temprature INTERNATIONAL STANDARD ISO 647 Second edition 2017-07 Reference number ISO 647:2017(E) BS ISO 647:2017 ISO 647:2017(E)ii
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9、22 749 09 47 copyrightiso.org www.iso.org BS ISO 647:2017 ISO 647:2017(E)Foreword iv Introduction v 1 Scope . 1 2 Normative references 1 3 T erms and definitions . 1 4 Principle 1 5 Reagents 1 6 Apparatus . 2 7 Preparation of test sample . 5 8 Procedure. 5 9 Expression of result . 7 10 Precision . 7
10、 10.1 Repeatability limit 7 10.2 Reproducibility limit 8 11 Test report . 8 ISO 2017 All rights reserved iii Contents Page BS ISO 647:2017 ISO 647:2017(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The
11、 work of preparing International 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-gove
12、rnmental, in liaison with ISO, also take part in the work. ISO collaborates 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 i
13、n the ISO/IEC Directives, Part 1. In particular the different approval 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 t
14、he 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. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO
15、 list of patent declarations received (see www .iso .org/ patents). Any 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 expression
16、s related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: w w w . i s o .org/ iso/ foreword .html. This document was prepared by Technical Committee ISO/TC 27, Solid
17、 minerals fuels, Subcommittee SC 5, Methods of analysis. This second edition cancels 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
18、All rights reserved BS ISO 647:2017 ISO 647:2017(E) Introduction The yield of distillation 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 v
19、BS ISO 647:2017BS ISO 647:2017 Brown coals and lignites Determination of the yields of tar, water, gas and coke residue by low temperature distillation 1 Scope This document specifies a method for the determination of the yields of tar, water, gas and coke residue obtained from brown coal and lignit
20、e by distillation to a final temperature of 520 C. 2 Normative references The following 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 l
21、atest edition of the referenced document (including any amendments) applies. ISO 5068-2, Brown coals and lignites Determination of moisture content Part 2: Indirect gravimetric method for moisture in the analysis sample ISO 1170, Coal and coke Calculation of analyses to different bases 3 T erms a nd
22、 definiti ons No terms and definitions are listed in this document. ISO and IEC maintain terminological 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 .o
23、rg/ obp 4 Principle The sample is heated in an aluminium retort to a temperature of 520 C during a 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
24、 weighed. The receiver and its contents are also weighed and the mass of the water in it determined 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.
25、A separate determination of moisture in the coal is made so that the decomposition water can be calculated. 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
26、 on the “dry” basis. 5 Reagents 5.1 Graphite paste. Ground dry and made into suitable paste with water or thick lubricating oil. INTERNATIONAL ST ANDARD ISO 647:2017(E) ISO 2017 All rights reserved 1 BS ISO 647:2017 ISO 647:2017(E) 5.2 Xylene. Boiling point 135 C to 140 C. 5.3 Toluene. Boiling point
27、 110 C. 6 Apparatus 6.1 Retort. Made of aluminium, with the dimensions shown in Figure 1. With the cover fitted, 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
28、for 20 min before use. If, through wear, the upper edge of the conical portion of the cover is below the top surface 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
29、 less than 7 mm above the top surface of the retort. This will ensure that the free volume of the retort does not exceed 180 ml.2 ISO 2017 All rights reserved BS ISO 647:2017 ISO 647:2017(E) Dimensions in millimetres Materials: Aluminium retort, aluminium content 99 % Volume of retort: 170 ml 10 ml
30、Outlet tube: Brass Key A screw thread B bearer bar C depth of hole for the thermometer D cover E as in Figure 2 a) F as in Figure 2 b) Figure 1 Retort 6.2 Furnace. Heated either electrically or by gas. For electrical heating, a resistance wire furnace or a silicon carbide rod furnace may be used. IS
31、O 2017 All rights reserved 3 BS ISO 647:2017 ISO 647:2017(E) 6.3 Thermoc ouple and m illi v oltmet er or nitr ogen-filled mer cury thermomet 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 int
32、ervals of one month by comparing it with a standard thermometer in a manner approved by a national testing authority. 6.4 Receiver. Round-bottomed 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 Figur
33、e 2), provided with a rubber or glass stopper. Dimensions in millimetres Key 1 retort with gas outlet tube 7 cooling bath 2 extent of heating furnace 8 outlet 3 gas outlet tube 9 cold water 4 heat resistant stopper 10 glass adapter tube 5 level of cooling water 11 ground joint 6 receiver Figure 2 Ar
34、rangement of the receiver in the cooling bath4 ISO 2017 All rights reserved BS ISO 647:2017 ISO 647:2017(E) 6.5 Cooling bath. The distance between the receiver 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
35、 bath. 6.6 Distillation apparatus. Composed of condenser, graduated tube for measurement of water and distillation flask. All parts are connected by means of ground glass joints. 7 Preparation of test sample Spread the laboratory sample on a tray and allow it to attain approximate moisture equilibri
36、um 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 of 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 r
37、educe 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 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 th
38、an 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 be considerably greater. 8 Procedure Weigh, to the nearest 0,05 g, about 50 g of the test sample and transfer it completely to the retort.
39、 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 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 t
40、he 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 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
41、 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 receiver in the cooling bath and ensure that the apparatus is gastight. It is necessary to pre-heat certain types of furnaces in order to
42、 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 joint shall not touch the water. Start the flow of water through the cooling bath and heat the retort according to the specification of
43、Table 1. T a b l e 1 S p e c i f i c a t i o n o f h e a t i n g t h e r e t o r t Time from start min Temperature C 10 220 20 310 30 380 40 440 50 480 60 505 70 520 80 520 Maintain the rate of heating within the limits shown in Figure 3. ISO 2017 All rights reserved 5 BS ISO 647:2017 ISO 647:2017(E
44、) Key X time, minutes Y temperature, C 1 temperature graph against time 2 limits NOTE 1 Total time for low temperature distillation between 20 C and 520 C: 80 min. NOTE 2 Effective time for low temperature distillation between 310 C and 520 C: 60 min. Figure 3 Schedule of heating At the end of the a
45、bove 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. Disconnect the receiver from the retort and, if necessary, transfer the remaining tar fr
46、om 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 retort to room temperature. Remove the coke residue carefully and weigh it to the ne
47、arest 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 receiver and determine the total water content by entrainment using the distillatio
48、n apparatus (6.6).6 ISO 2017 All rights reserved BS ISO 647:2017 ISO 647:2017(E) 9 Expression of result The yields on the “as analysed” basis are given by Formulae (1) to (4): (1) (2) (3) (4) wherem 0 is the mass of sample, in grams;m 1 is the mass of empty receiver and stopper, in grams;m 2 is the
49、mass of receiver and stopper, plus tar, plus total water, in grams;m 3 is the mass of total water determined by entrainment, in grams;m 4 is the mass of coke residue, in grams;M is the moisture content of the sample, in mass percent; is the coke residue yield of the sample, in mass percent; is the tar yield of the sample, in mass p
