1、BRITISH STANDARD CONFIRMED September 1997 BS 1016-6: 1977 Incorporating Amendment Nos. 1 and2 Methods for Analysis and testing of coal and coke Part 6: Ultimate analysis of coal UDC 662.66 + 662.74:543.84BS1016-6:1977 This British Standard, having been prepared under the directionof the Solid Fuel S
2、tandards Committee, was published under the authority ofthe Executive Boardon 29April1977 BSI 11-1999 First published March 1942 First revision December 1958 Second revision April 1969 Third revision April 1977 The following BSI references relate to the work on this standard: Committee references SF
3、C/45 andSFC/45/8 Draft for comment 73/42187DC ISBN 0 580 09173 2 Cooperating organizations The Solid Fuel Standards Committee, under whose supervision this British Standard was prepared, consists of representatives from the following Government departments and scientific and industrial organizations
4、: Association of Consulting Engineers British Carbonization Research Association* British Cast Iron Research Association British Ironfounders Association British Mechanical Engineering Confederation Central Electricity Generating Board* Chamber of Coal Traders Coke Oven Managers Association* Combust
5、ion Engineering Association* Council of Ironfoundry Associations Department of Energy Domestic Solid Fuel Appliances Approval Scheme Greater London Council Health and Safety Executive Heating and Ventilating Contractors Association Institute of British Foundrymen* Institute of Fuel Institution of He
6、ating and Ventilating Engineers Low Temperature Coal Distillers Association of Great Britain Ltd. National Coal Board* Society of British Gas Industries Solid Fuel Advisory Service Water-tube Boilermakers Association Womens Solid Fuel Council The organizations marked with an asterisk in the above li
7、st, together with the following, were directly represented on the committee entrusted with the preparation of this British Standard: British Coal Exporters Federation British Gas Corporation British Steel Corporation Cement Makers Federation Chemical Industries Association Electricity Supply industr
8、y in England and Wales Institute of Trading Standards Administration London Coal Exporters Association Scientific Instruments Manufacturers Association of Great Britain Society of Chemical Industry Solid Smokeless Fuels Federation Independent experts Amendments issued since publication Amd. No. Date
9、 of issue Comments 6982 May 1992 7689 May 1993 Indicated by a sideline in the marginBS1016-6:1977 BSI 11-1999 i Contents Page Cooperating organizations Inside front cover Foreword ii 1 Scope 1 2 References 1 3 Definitions 1 4 Introduction 1 5 Sample 1 6 Carbon and hydrogen 2 7 Nitrogen 6 8 Total sul
10、phur 8 9 Carbon dioxide 11 10 Reporting of results 13 11 Precision of the determinations 13 Figure 1 Temperature distribution curve for the carbon andhydrogenfurnace 3 Figure 2 Absorption train for carbon and hydrogen determination 4 Figure 3 Nitrogen distillation apparatus 7 Figure 4 Absorption tra
11、in and furnace for sulphur (high temperaturemethod) 10 Figure 5 Apparatus for carbon dioxide (titrimetric method) 11 Figure 6 Apparatus for carbon dioxide (gravimetric method) 14 Publications referred to Inside back coverBS1016-6:1977 ii BSI 11-1999 Foreword BS 1016 comprises a series of Parts deali
12、ng with methods for the analysis and testing of coal and coke. It is gradually being restructured and Parts in the new series have been allocated numbers from100onwards. The current Parts are as follows, with new Part numbers (which will be given to revisions when they are published) in parentheses
13、where appropriate. Part 1: Total moisture of coal (Part 101); Part 2: Total moisture of coke (Part 102); Part 6: Ultimate analysis of coal (Part 106); Part 7: Ultimate analysis of coke (Part 106); Part 8: Chlorine in coal and coke (Part 106); Part 9: Phosphorus in coal and coke (Part 106); Part 10:
14、Arsenic in coal and coke (Part 106); Part 11: Forms of sulphur in coal (Part 106); Part 14: Analysis of coal ash and coke ash (Part 114); Part 15: Fusibility of coal ash and coke ash (Part 113); Part 16: Methods for reporting results (Part 100); Part 17: Size analysis of coal (Part 109); Part 18: Si
15、ze analysis of coke (Part 110); Part 20: Determination of Hardgrove grindability index of hard coal (Part112); Part 21: Determination of moisture-holding capacity of hard coal (Part 103); Part 104: Proximate analysis; Part 105: Determination of gross calorific value; Part 107: Caking and swelling pr
16、operties of coal; Part 108: Tests special to coke; Part 111: Determination of abrasion index of coal. The methods given in BS1016are specified for the analysis of coal or of coke or, in some instances, for the analysis of both coal and coke. Experience has shown that, in general, the methods may als
17、o be used for the analysis of manufactured smokeless fuels other than coke made by a conventional process. However, as no systematic survey has been made of their applicability to all such fuels, it is not possible to state whether the ultimate analysis methods for coal or those for coke (see Part 7
18、) will be more appropriate for a particular fuel; usually the former are likely to be satisfactory for fuels prepared at temperatures below800 C. The revision of Part6has been undertaken in order to complete the introduction of metric units and to adopt a uniform presentation. No technical changes h
19、ave been made to the methods retained from the previous edition of this Part, but the Liebig method has been deleted as it is now little used for the determination of carbon and hydrogen in coal. The high temperature method for the determination of carbon and hydrogen is technically equivalent to IS
20、O 609. Similarly, the method for nitrogen, the method for sulphur and the gravimetric method for carbon dioxide correspond technically with those specified in ISO 333, ISO 351 and ISO 925 respectively. There is no ISO titrimetric method for the determination of carbondioxide.BS1016-6:1977 BSI 11-199
21、9 iii In the foreword to the last revision of Part6it was stated that it might shortly be possible to specify a satisfactory procedure for the direct determination of oxygen in coal. Since then, ISO1994has been published on the basis of international collaborative work in which a number of UK labora
22、tories took part. It has been decided that it is unnecessary to issue a British Standard on this subject but that, where a direct oxygen determination is needed, a reference should be made to ISO1994. The definition of ultimate analysis of a coal consequently includes oxygen as one of its chemical c
23、onstituents, this being identical with the ISOdefinition. A British Standard does not purport to 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 le
24、gal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i to iv, pages1to 14, 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 tab
25、le on the inside front cover.iv blankBS1016-6:1977 BSI 11-1999 1 1 Scope This Part of BS1016describes methods of determining carbon, hydrogen, nitrogen, sulphur and carbon dioxide in the analysis sample of coal. In order to quote the ultimate analysis of coal a value for oxygen is required; this may
26、 be determined by the method specified in ISO1994or estimated as a difference figure and reported as “oxygen plus errors”. 2 References The titles of the publications referred to in this standard are listed on the inside back cover. 3 Definitions For the purposes of this Part of BS 1016 the followin
27、g definitions apply. 3.1 ultimate analysis the analysis of coal expressed in terms of its carbon, hydrogen, nitrogen, sulphur and oxygen contents 3.2 moisture in the analysis sample the moisture in the analysis sample of coal after it has attained approximate equilibrium with the laboratory atmosphe
28、re to which it has been exposed 3.3 ash the inorganic matter remaining after the coal has been incinerated to constant mass under standardized conditions 3.4 repeatability the maximum acceptable difference between duplicate determinations carried out at different times in the same laboratory on the
29、same analysis sample by the same operator using the same apparatus 3.5 reproducibility the maximum acceptable difference between the mean of duplicate determinations carried out in one laboratory and the mean of duplicate determinations carried out in any other laboratory on representative samples t
30、aken from the same gross sample after the last stage of the reduction process 4 Introduction The determination of the total amounts of carbon, hydrogen, nitrogen and sulphur, regardless of their origin, is described. The carbon includes that present in the mineral carbonates and the hydrogen include
31、s that present both in the moisture and in the water of constitution of the argillaceous constituents of the mineral matter. All the nitrogen is assumed to be present in the coal substance. Sulphur is normally present in three forms: as iron pyrites (FeS 2 ), as inorganic sulphates associated with t
32、he mineral matter, and as organic sulphur compounds in the coal substance. Oxygen in the coal substance may be determined by one of the procedures given in ISO 1994. Alternatively, an estimate of the percentage of oxygen can be obtained on the air-dried basis by subtracting the sum of the determined
33、 percentages of moisture, ash, carbon, hydrogen, nitrogen and sulphur from 100. The value so obtained for oxygen may be inaccurate because it includes the cumulative errors of all the determinations made, and it should therefore be reported as “oxygen (plus errors)”. A more satisfactory value for ox
34、ygen is obtained when the ultimate analysis is expressed on the dry, mineral matter free basis (see Part16of this standard). The value for oxygen (d.m.m.f.) so calculated, can be checked by comparing the determined calorific value of the coal (corrected to the d.m.m.f. basis) with the calorific valu
35、e calculated from the formula: Q 80.3 C + 339 H 36.6O + 0.172 O 2 where If the calculated and determined values of the calorific value agree within125J/g, then it can be considered that the determined values of C, H and N and therefore the calculated value of the oxygen content lie within the range
36、of experimental error. 5 Sample The coal used for the ultimate analysis shall be the analysis sample having a top size not greater than0.2mm (ground to pass a2124m test sieve complying with the requirements of BS 410), taken and prepared according to BS 1017-1. C represents the determined value of c
37、arbon H represents the determined value of hydrogen O represents the value of oxygen calculated from the following formula: O = 100 (C + H + N) d.m.m.f. basisBS1016-6:1977 2 BSI 11-1999 The sample received in the laboratory shall be brought into approximate equilibrium with the laboratory atmosphere
38、 by exposing it in a thin layer on a tray. The exposure time shall be kept to the minimum necessary for this purpose, particularly with coals liable to oxidation. The sample shall be thoroughly mixed, preferably by mechanical means, immediately before the determination. Duplicate determinations shal
39、l not be made at the same time in the same apparatus. 6 Carbon and hydrogen 6.1 Principle. A known mass of coal is burned at a temperature of1350 C in a rapid current of oxygen, so that all the carbon is converted to carbon dioxide and all the hydrogen to water. Chlorine and oxides of sulphur are re
40、tained in the apparatus by silver gauze. The water formed is absorbed by magnesium perchlorate and the carbon dioxide by sodium hydroxide on an insert base. A determination of moisture is carried out at the same time and the value for hydrogen is corrected for that present as moisture in the sample.
41、 6.2 Special reagents. All reagents, unless otherwise specified, shall be of analytical reagent quality. Distilled or deionized water complying with the requirements of BS3978shall be used throughout. 6.2.1 Magnesium perchlorate 1) , 1.2 mm to 0.7 mm. 6.2.2 Sodium hydroxide on an insert base, prefer
42、ably of coarse grading, for example3.0mm to1.5mm, but not finer than1.2mm to0.7mm, and preferably of the self-indicating type. WARNING. Reagents containing asbestos as the base material should not be used. 6.2.3 Aluminium oxide, finely divided, approximately0.1mm. 6.2.4 Sodium borate solution, 0.05N
43、. 6.2.5 Hydrogen peroxide solution containing3parts of100volume H 2 O 2and97parts of water, neutralized with the sodium borate solution (see6.2.4) to the screened indicator (see 6.2.6). 6.2.6 Screened indicator. Proceed as follows. A) Dissolve 0.125 g of methyl red in 100 ml of ethanol (95 v/v). B)
44、Dissolve0.083g of methylene blue in100mm of ethanol (95 % v/v); store in a dark glass bottle. Mix equal volumes of A) and B) immediately before use. 6.2.7 Pure silver gauze, one mesh permillimetre,0.3mm diameter wire. 6.2.8 Oxygen, hydrogen-free. 6.3 Special apparatus. The following special apparatu
45、s is required. 6.3.1 Purification trains. Two purification trains, one for removing water and carbon dioxide from the oxygen used for the combustion and the other for similarly purifying the air (see note) used for sweeping out the absorption train before and after a determination. The trains shall
46、be assembled using the following reagents in the order stated. a) Magnesium perchlorate (see 6.2.1) for removing water. b) Sodium hydroxide on an insert base (see 6.2.2) for removing carbon dioxide. c) Magnesium perchlorate (see 6.2.1) for removing water produced in the reaction between carbon dioxi
47、de and sodium hydroxide. The trains should be large enough to avoid the necessity for frequent recharging. NOTEThe air used should not be taken from a compressed air system, as this is liable to contain organic matter, but should be drawn through the trains from the atmosphere by means of a pump or
48、aspirator. 6.3.2 Heating unit. An electrically heated furnace designed to carry a tube of28.5mm outside diameter and to heat it over a length of about125mm to give a temperature of1350 C at the centre of the hot zone and a temperature-distribution curve similar to that shown in Figure 1. NOTEFurnace
49、s of the type normally used for the determination of carbon or sulphur in steel are not suitable, because of the absence of the auxiliary section to maintain the silver gauze roll at the correct temperature. 6.3.3 Combustion tube. A tube,22mm internal diameter and28.5mm outside diameter by0.65m long, made of refractory aluminous porcelain that is not permeable to gases at1400 C 2) . 6.3.4 Combustion boat. A combustion boat of iron-free unglazed porcelain,70mm long by12.5mm wide by10mm deep, that does not bl
