1、BRITISH STANDARD CONFIRMED SEPTEMBER 1989 BS 1016-1: 1973 Methods for The analysis and testing of coal and coke Part 1: Total moisture of coal UDC 662.66 + 662.74:543 + 662.66:543.712.2BS1016-1:1973 This British Standard, having been approved by the Solid FuelIndustry Standards Committee, was publis
2、hed underthe authority of the Executive Board on 15October1973 BSI 07-1999 First published, March 1942 First revision, February 1957 Second revision, October 1973 The following BSI references relate to the work on this standard: Committee reference SFE/45 and SFE/45/8 Draft for comment 72/40657 ISBN
3、 0 580 076873 Co-operating organizations The Solid Fuel Industry Standards Committee, under whose supervision this British Standard was prepared, consists of representatives from the following Government departments and scientific and industrial organizations: A British Standard does not purport to
4、include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, p
5、ages i and ii, pages 1 to 6, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Association of Consulting Engineers Electricity Council, the Cent
6、ral Electricity British Cast Iron Research Association Generating Board and Area Boards in British Coke Research Association* England and Wales* British Ironfounders Association Greater London Council British Mechanical Engineering Heating and Ventilating Contractors Confederation Association Britis
7、h Steel Industry* Institute of British Foundrymen* Chamber of Coal Traders Institute of Fuel* Chemical Industries Association* Institution of Heating and Ventilating Coal Utilisation Council Engineers Coke Oven Managers Association* Institution of Mechanical Engineers* Combustion Engineering Associa
8、tion* Low Temperature Coal Distillers Association Council of Ironfoundry Associations of Great Britain Ltd. Department of the Environment National Coal Board* Department of Trade and Industry Society of British Gas Industries Domestic Solid Fuel Appliances Approval Water-tube Boilermakers Associatio
9、n* Scheme Womens Advisory Council on Solid Fuel The scientific and industrial organizations marked with an asterisk in the above list, together with the following, were directly represented on the committee entrusted with the preparation of this British Standard: British Coal Exporters Federation Sc
10、ientific Instrument Manufacturers British Gas Corporation Association of Great Britain Cement Makers Federation Society of Chemical Industry Institute of Trading Standards Solid Smokeless Fuels Federation Institution of Electrical Engineers South Wales Institute of Engineers London Coal Exporters As
11、sociation Independent experts Amendments issued since publication Amd. No. Date of issue CommentsBS1016-1:1973 BSI 07-1999 i Contents Page Co-operating organizations Inside front cover 1 Scope 1 2 Definitions 1 3 Coal sample 1 4 Moisture in the 13 mm coal sample 1 5 Moisture in the 3 mm coal sample
12、2 6 Calculation and reporting 4 7 Precision of the determination 4 8 Notes 4 Figure 1 Suitable nitrogen oven 5 Publications referred to Inside back coverii blankBS1016-1:1973 BSI 07-1999 1 1 Scope This British Standard describes alternative methods of determining the total moisture on samples of coa
13、l taken and prepared by the procedures given in BS1017-1. NOTEThe titles of the British Standards referred to in this standard are listed on the inside back cover. 2 Definitions For purposes of this British Standard, the following definitions apply: 2.1 total moisture the moisture in the coal as sam
14、pled 2.2 free moisture the moisture that is lost by the coal sample in attaining approximate equilibrium with the air to which it is exposed 2.3 moisture in air-dried coal the moisture in the coal sample after it has attained approximate equilibrium with the air to which it is exposed 2.4 high rank
15、coal a coal containing (arbitrarily) less than4% of moisture (in air-dried coal) and more than84% of carbon (dry, ash free basis) 2.5 low rank coal any coal other than a high rank coal. If the rank of the coal is not known it is treated as a low rank coal 2.6 repeatability the maximum acceptable dif
16、ference between single determinations carried out in one laboratory on two separate moisture samples taken simultaneously in accordance with the principles laid down in BS1017 1) 2.7 reproducibility the maximum acceptable difference between single determinations carried out in different laboratories
17、 on two separate moisture samples taken simultaneously in accordance with the principles laid down in BS1017 1) 3 Coal sample The sample for the determination of total moisture shall have been taken and prepared according to BS1017-1. It will be received in the laboratory in a sealed, air-tight cont
18、ainer and will consist either of1kg of coal having a maximum particle size of13mm or of not less than300g of air-dried coal having a maximum particle size of3mm. All samples, other than a1kg sample prepared from a coal having an initial top size of less than13mm or from a visibly dry high rank coal
19、of any top size, will have been air-dried before receipt and details of the loss in mass on air-drying, i.e.the free moisture, will be recorded on the label of the sample container (but see final paragraph of Foreword). 4 Moisture in the 13 mm coal sample 4.1 Distillation with toluene 4.1.1 Principl
20、e. This method is suitable for all coals. The whole of the1kg sample of coal is heated with toluene under reflux conditions. The toluene distils into a graduated receiver, carrying with it the water from the coal. The water then separates to form the lower layer. The excess toluene overflows from th
21、e receiver and returns to the flask. The moisture in the coal is calculated from the masses of the sample taken and of the water collected. 4.1.2 Special reagent. The following reagent is required: Toluene. Boiling point110 C, dry 2) . 4.1.3 Special apparatus. The following apparatus is required: De
22、an and Stark apparatus complying with BS756 and comprising: 1) a copper flask, capacity two litres. 2) a receiver, capacity100ml. 3) a condenser and spray tube, as specified in BS756. 4) heating apparatus: the flask may be heated directly by gas or electricity, or by immersion in a heated oil bath.
23、The receiver and condenser shall be cleaned before each determination by treating them with a suspension of potassium dichromate in sulphuric acid, or other suitable cleansing agent. 1) It should be noted that this definition differs from those in Parts 3 to 16 of BS 1016. 2) The residual toluene in
24、 the flask after a determination may be filtered and dried for re-use.BS1016-1:1973 2 BSI 07-1999 4.1.4 Procedure. Weigh the sample and container (seeNote1) as received to the nearest gram. Transfer the coal as completely as possible to the flask, carefully clean all traces of the sample from the so
25、cket in the neck of the flask and connect to the glass portion of the apparatus. Add400ml of the toluene through the top of the reflux condenser. Heat the flask so that brisk distillation occurs and continue to distil until no more water collects in the graduated receiver (seeNote2). This normally t
26、akes6to8h. During distillation wash down any drops of water adhering to the inner surface of the condenser and upper walls of the receiver with toluene, using the spray tube. Record the volume of water collected. Weigh the wet container with any coal left adhering to it and dry completely at105 C to
27、110 C. Cool and reweigh. Empty out the residual coal and reweigh the dry empty container (seeNote3). 4.1.5 Calculation of result. Calculate the result as follows: 4.2 Drying at105 C to 110 C in air 4.2.1 Principle. This method shall be used only for high rank coals. The whole of the1kg sample of coa
28、l is heated to constant mass in an air oven at105 C to110 C and its moisture calculated from the loss in mass of the sample. 4.2.2 Special apparatus. The following apparatus is required: 1) Air oven. An oven capable of maintaining a temperature within the range105 C to110 C and in which the atmosphe
29、re changes three to five times per hour. The number of atmosphere changes in the oven shall be determined by one of the methods described in BS2648. 2) Tray. Non-corrodible metal tray approximately0.1m 2in area by25mm deep. 4.2.3 Procedure. Weigh the sample and container (seeNote1) as received to th
30、e nearest gram. Weigh the dry empty tray, transfer the coal as completely as possible to the tray and spread evenly. Place the charged tray in the oven at a temperature of105 C to110 C. Dry the wet container with any coal adhering to it by warming, transfer the remaining coal to the tray and weigh t
31、he dry empty container (seeNote4). Heat the tray and its contents until constant in mass. The time required is normally5to6h. The loss in mass of the hot sample shall be checked at the end of the fourth hour and at hourly intervals thereafter. Weigh hot to avoid absorption of moisture during cooling
32、. 4.2.4 Calculation of result. Calculate the result as follows: 5 Moisture in the3mm coal sample 5.1 Distillation with toluene 5.1.1 Principle. This method is suitable for all coals. A known mass of coal is heated in a distillation flask with toluene under reflux conditions. The toluene distils into
33、 a graduated receiver, carrying with it the water from the coal. The water then separates to form the lower layer. The excess toluene overflows from the receiver and returns to the flask. The moisture in the coal is calculated from the masses of the sample taken and of the water collected. 5.1.2 Spe
34、cial reagent. The following reagent is required: Toluene. Boiling point110 C, dry 3) . 5.1.3 Special apparatus. The following apparatus is required: Dean and Stark apparatus complying with BS756 and comprising: 1) A glass flask, capacity500ml. 2) A receiver, capacity10ml (25ml for samples expected t
35、o contain more than10% of moisture). 3) A condenser and spray tube, as in BS756. m 1 = Mass of container plus sample as received (g), m 2 = Mass of water collected (g) (numerically equal to the volume of water collected ml), m 3 = Mass of wet container plus adhering wet coal (g), m 4 = Mass of dry c
36、ontainer plus dry coal (g), m 5 = Mass of dry empty container (g), M = Percentage of moisture in the sample analysed, thenM m 2 m 3 m 4 () + m 1 m 5 -100 = If m 1 = Mass of container plus sample as received (g), m 2 = Mass of empty tray (g), m 3 = Mass of tray plus sample after heating (g), m 4 = Ma
37、ss of dry empty container (g), M = Percentage of moisture in the sample analysed, 3) The residual toluene in the flask after a determination may be filtered and dried for re-use. thenM m 1 m 4 ()m 3 m 2 () m 1 m 4 () -100 =BS1016-1:1973 BSI 07-1999 3 4) Heating apparatus: the flask may be heated dir
38、ectly by gas or electricity, or by immersion in a heated oil bath. The receiver and condenser shall be cleaned before each determination by treating them with a suspension of potassium dichromate in sulphuric acid, or other suitable cleansing agent. 5.1.4 Procedure. Before opening the container, tho
39、roughly mix the sample, preferably by mechanical means, for at least1min. Weigh to the nearest0.1g about100g of the sample and transfer to the dry distillation flask. Add200ml of the toluene in such a way that any coal adhering to the neck or sides of the distillation flask is washed down by the rea
40、gent. Fill the receiver with the toluene and assemble the apparatus. Heat the distillation flask and keep the contents boiling briskly. Continue the distillation until no further water collects in the graduated receiver. During distillation wash down any drops of water adhering to the inner surface
41、of the condenser, or to the upper walls of the receiver, with toluene, using the spray tube. Continue the distillation for a sufficient time to ensure that any water washed back into the distillation flask has been carried over into the receiver. Record the volume of water collected. Calibrate the a
42、pparatus by distilling a series of known volumes of water, accurately measured, e.g.by a microburette, covering the range of moisture contents in the fuels likely to be encountered. Plot a graph, showing the mass of water added (assuming1ml has a mass of1g) against the scale reading of the water in
43、the receiver and use it to correct the mass of water obtained in each test. 5.1.5 Calculation of result. Calculate the result as follows: 5.2 Drying in nitrogen 5.2.1 Principle. This method is suitable for all coals. A known mass of coal is heated to constant mass in a current of nitrogen in an oven
44、 maintained at105 C to110 C and its percentage moisture calculated from the loss in mass of the coal. 5.2.2 Special reagents. The following reagents are required: 1) Nitrogen. Dry and containing less than10p.p.m. of oxygen; this is commercially available in cylinders. 2) Desiccant. Either fresh or f
45、reshly regenerated, self-indicating activated alumina, silica gel or anhydrous calcium sulphate. 5.2.3 Special apparatus. The following apparatus is required: 1) Oven. A minimum-free-space oven capable of maintaining a temperature within the range105 C to110 C and with provision for the nitrogen to
46、pass through it at about15oven volumes per hour. A suitable oven is illustrated in Figure 1. Arrangements should be made for measuring the flow of nitrogen through the oven. 2) Weighing vessels. Shallow vessels, of glass with ground-on covers, or of corrosion-resistant metal with well-fitting covers
47、, of such a size that the loading of the coal layer does not exceed0.3g/cm 2 . Circular dishes65mm in diameter are suitable for10g of coal sample. 5.2.4 Procedure. Before opening the container, thoroughly mix the sample, preferably by mechanical means, for at least1min. Weigh a clean dry weighing ve
48、ssel with its cover to the nearest milligram, spread into it about10g of the sample in an even layer and replace the cover. Reweigh to determine the mass of sample taken. Place the cover on a metal plate in a desiccator and heat the uncovered vessel in the oven at a temperature of105 C to110 C in a
49、stream of nitrogen (seeNote5) until constant in mass (1 to3h is normally sufficient). Remove the vessel and dry sample from the oven, replace the cover and set to cool on a metal plate for10min. Transfer to the metal plate in the desiccator and weigh after a further10min. 5.2.5 Calculation of result. Calculate the result as follows: If m 1 = mass of coal taken (g), m 2 = mass of water collected (g), M = percentage of moisture
