1、BRITISH STANDARD CONFIRMED APRIL 1979 BS 1016-14: 1963 Methods for The analysis and testing of coal and coke Part 14: Analysis of coal ash and coke ash UDC 662.62.01:543.822BS1016-14:1963 This British Standard, having been approved by the Solid FuelIndustry Standards Committee and endorsed by theCha
2、irman of the Engineering Divisional Council, was publishedunder the authority ofthe General Council on 23December1963 BSI 11-1999 First published March 1942 First revision December 1963 The following BSI references relate to the work on this standard: Committee references SFE/45 andSFE/45/8 Draft fo
3、r comment D 62/5808 ISBN 0 580 35600 0 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: The Government
4、 department and 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: Association of Boiler Setters, Chimney and Federation of British Industr
5、ies* Furnace Constructors Gas Council* Association of British Chemical Heating and Ventilating Contractors Manufacturers* Association Association of Consulting Engineers Imperial Chemical Industries Limited* Incorporated Institute of British Foundrymen* British Cast Iron Research Association Institu
6、te of Fuel* British Chemical Plant Manufacturers Institution of Chemical Engineers Association Institution of Gas Engineers* British Coal Utilisation Research Association* Institution of Heating and Ventilating British Coke Research Association* Engineers British Coking Industry Association* Institu
7、tion of Mechanical Engineers* British Electrical and Allied Manufacturers Iron and Steel Institute Association Low Temperature Coal Distillers Association British Iron and Steel Federation* of Great Britain, Ltd. British Ironfounders Association Ministry of Housing and Local Government British Mecha
8、nical Engineering Federation Ministry of Power Chamber of Coal Traders Ministry of Public Building and Works Coal Utilisation Council National Coal Board* Coke Oven Managers Association* Society of British Gas Industries Combustion Engineering Association* Water-tube Boilermakers Association Council
9、 of Ironfoundry Associations Womens Advisory Council on Solid Fuel Electricity Council, the Generating Board and Area Boards in England and Wales* British Ceramic Research Association London Coal Exporters Association British Coal Exporters Federation London Transport Board Cement Makers Federation
10、Society of Chemical Industry D.S.I.R. Warren Spring Laboratory Solid Smokeless Fuels Federation Institution of Electrical Engineers South Wales Institute of Engineers Amendments issued since publication Amd. No. Date CommentsBS1016-14:1963 BSI 11-1999 i Contents Page Co-operating organizations Insid
11、e front cover Foreword ii 14.1 Definitions 1 14.2 Introduction 1 14.3 Principle 1 14.4 Special apparatus 2 14.5 Coal or coke sample 2 14.6 Preparation of ash 2 14.7 Loss on ignition 2 14.8 Preparation of solutions 3 14.8.1 Solution A 3 14.8.2 Solution B 3 14.9 Silica 4 14.10 Alumina 4 14.11 Sodium o
12、xide and potassium oxide 5 14.12 Iron oxide 6 14.13 Titanium oxide 7 14.14 Manganese oxide 7 14.15 Phosphorus pentoxide 9 14.16 Calcium oxide and magnesium oxide 9 14.17 Sulphur trioxide 11 14.18 Tolerances 11 14.19 Reporting of results 11 Appendix Spectrochemical analysis 12 Figure 1 Scheme of anal
13、ysis of coal ash and coke ash 8 Table 1 Characteristic composition of British coal and coke ashes 1 Table A.1 Suitable line pairs 14 Table A.2 Pure materials and preparation of the primary solutions 15 Table A.3 Data for preparation of standard ash solutions 16 Table A.4 Relative intensities of suit
14、able iron lines 17BS1016-14:1963 ii BSI 11-1999 Foreword This standard makes reference to the following British Standards: BS410, Test sieves. BS1016, Methods for the analysis and testing of coal and coke Part3:Proximate analysis of coal Part 4: Proximate analysis of coke. BS1017, The sampling of co
15、al and coke. BS1041, Code for temperature measurement. In1942, when BS1016, “Methods for the analysis and testing of coal and coke”, was published it superseded a number of other standards, each dealing with special methods, bringing them up to date and embodying them in one standard. BS1016:1942 al
16、so dealt with the receipt of samples and their preparation in the laboratory for analysis and was linked directly with a companion standard on methods of collection of samples, BS1017, “The sampling of coal and coke”. Continued work by the Committee concerned and international discussion under the a
17、egis of the International Organization for Standardization have led to the revision of these collected methods and a new edition of BS1016 has become necessary. A similar revision of BS1017 has been undertaken and the link between the two standards is maintained. The division between them, however,
18、has been changed and this standard deals only with the analysis and testing of coal and coke; all the preparation of samples for analysis is included in the revised BS1017. The new standard is published in separate parts, each covering a particular group of analyses, e.g.proximate analysis, ultimate
19、 analysis. This method of presentation permits the revision of any part with the minimum of delay without the necessity of issuing a new comprehensive standard. Where the methods for a particular group of analyses for coke differ widely from those for coal they are published as a separate part but w
20、here the modifications for coke are slight they are given as separate sections of the same part. In the interests of international discussion it is important that there should be uniformity in definition and in method of reporting of results. Each part of the new standard begins, therefore, with a l
21、ist of definitions relevant to the methods described in it and ends with a section dealing with reporting of the results. Part14 Analysis of coal ash and coke ash deals with the determination of the major constituents common to all ashes. In March,1960, BSI Document PD3714 gave a brief review of the
22、 considerable progress which has been made in the development of more rapid techniques. The committee responsible for this revision of BS1016 has now recommended the adoption of the B.C.U.R.A. rapid method 1)which, as well as being accurate, enables several ashes to be analysed in the time taken for
23、 one by the classical method. The saving of time has been made by eliminating lengthy chemical separations and substituting selective complexometric and physico-chemical methods which utilize the relatively inexpensive spectrophotometers and flame photometers now available commercially. A growing ne
24、ed for even more rapid methods of ash analysis has led to the development of a spectrochemical method, based on the use of the Hilger large quartz spectrograph, for the determination of some of the major constituents. Its precision is lower than that of the B.C.U.R.A. rapid method and so far, becaus
25、e of the high initial cost of the equipment, its use has been limited to a few laboratories. However, the possibility of future developments requiring large numbers of ash analyses warrants a description of the method in an Appendix. 1) K. Archer, D. Flint and J. Jordan, Fuel, Lond.,1958,37,421.BS10
26、16-14:1963 BSI 11-1999 iii 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 legal obligations. Summary of pag
27、es This document comprises a front cover, an inside front cover, pages i to iv, pages1to18, 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.iv
28、blankBS1016-14:1963 BSI 11-1999 1 14.1 Definitions For the purposes of this British Standard, the following definitions apply: 14.1.1 ash (coal 2)and coke 3) ) the inorganic matter remaining after the coal or coke has been incinerated to constant weight under standard conditions 14.1.2 within-labora
29、tory tolerance the maximum acceptable difference between determinations made in the same laboratory on the same preparation of ash by the same operator using the same apparatus 14.1.3 between-laboratory tolerance the maximum acceptable difference between the means of two determinations carried out b
30、y two different laboratories on representative samples taken from the same preparation of ash 14.1.4 temperature measurement where the temperature is specified as a definite figure, it is to be understood that this figure should be attained as closely as possible and that it should be subject only t
31、o the errors inherent in accurate temperature measurement, as defined in BS1041 4) where a range of temperature is given, the temperature may be anywhere in the range without detriment to the result. However, the mean of the range should be aimed at in order that errors of measurement do not cause a
32、 temperature outside the specified range to be used inadvertently Table 1 Characteristic composition of British coal and coke ashes 14.2 Introduction One of the important factors governing the industrial usage of coal and coke is the behaviour of the mineral matter associated with it. The plant may
33、be designed for this to be removed as particulate ash, fly ash, clinker or liquid slag and operational difficulties may be encountered if any other than the intended form of residue is produced. The analysis of ash prepared under standard condition 5) 6)is often used as a guide to the selection of s
34、uitable solid, fuel. Ash consists mainly of the oxides of silicon, aluminium, iron, calcium, magnesium, titanium, manganese and the alkali metals, partly combined as silicates, sulphates and phosphates; its composition reflects the constitution of the original mineral matter. These constituents norm
35、ally account for at least99 per cent of the ash. The usual limits within which they are encountered are shown in Table 1, although the compositions of some ashes can be considerably outside these limits. On exposure to air, some ashes rapidly absorb water and carbon dioxide. It is, therefore, necess
36、ary either to re-ignite each portion of ash immediately before weighing or to determine the loss on ignition using a separate portion. The results are reported on the “Ignited at800 C” basis. Although the procedure is written for a single analysis of one ash, full advantage of the saving of time aff
37、orded by the method can best be taken by conducting several analyses simultaneously. The use of calibration graphs for these colorimetric methods leads to results which are less reproducible than those obtained by the specified procedure and is therefore not recommended. 14.3 Principle The scheme of
38、 analysis is shown diagrammatically in Figure 1. Two solutions are prepared from the ash. Solution A is prepared by fusing the ash with sodium hydroxide, leaching the melt with water and acidifying with hydrochloric acid. It is used for the colorimetric determination of silica and alumina. 2) BS1016
39、-3, “Proximate analysis of coal”. 3) BS1016-4, “Proximate analysis of coke”. 4) BS1041, “Code for temperature measurement”. Constituent Expressed as Range per cent Silica Alumina Ferric oxide SiO 2 Al 2 O 3 Fe 2 O 3 1555 1040 140 Calcium oxide Magnesium oxide Sodium oxide CaO MgO Na 2 O 125 0.55 08
40、Potassium oxide Titanium oxide Manganese oxide K 2 O TiO 2 Mn 3 O 4 05 03 01 Sulphate Phosphate SO 3 P 2 O 5 012 03 5) BS1016-3, “Proximate analysis of coal”. 6) BS1016-4, “Proximate analysis of coke”.BS1016-14:1963 2 BSI 11-1999 Solution B is prepared by decomposition of the ash with hydrofluoric,
41、nitric and sulphuric acids. After removal of the silica by evaporation, the residue is dissolved in water. This solution is used for the flame photometric determination of sodium and potassium, the colorimetric determination of iron, titanium, manganese and phosphorus, and the determination of calci
42、um and magnesium by titration with EDTA. Separate portions of the sample are used for the gravimetric determination of sulphate and the determination of loss on ignition at800 C. The spectrophotometer or flame photometer is calibrated for every determination using standard solutions prepared from sa
43、lts of adequate purity or, in the case of silica and alumina, from either N.B.S. standard feldspar No.99 or B.C.S. firebrick No.269. Unless otherwise stated, the coloured solutions prepared for optical density measurements are stable for several hours. Should an abnormally low total be obtained, the
44、 oxides of other elements, e.g.arsenic, boron, barium, germanium and tin, may be present and, if desired, may be identified and determined by appropriate chemical or spectrographic methods. Substantial percentages of such oxides may influence the results of other analytical determinations. 14.4 Spec
45、ial apparatus Muffle furnace. A muffle furnace 7)capable of giving a zone within the range490510 C in30 minutes from cold, of being raised to790810 C in a further60 to90 minutes and of maintaining this latter temperature at the end of the run-up period. The ventilation shall be such as to give at le
46、ast four air changes per minute at800 C 8) . Silica trays,15cm 8cm 1cm. Silica plate, a silica plate6mm thick, which is an easy sliding fit into the muffle furnace. Platinum crucibles, each of capacity30ml, with lid. Cooling block, of aluminium. Nickel crucibles, each of capacity40ml, with lid. Spec
47、trophotometer, of adequate sensitivity and selectivity 9) . Flame photometer, of adequate sensitivity and selectivity 10) . 14.5 Coal or coke sample The coal or coke used for the preparation of the sample of ash shall be prepared in a similar manner to the“ lb analysis sample of coal or the2oz analy
48、sis sample of coke, taken according to BS1017 11) , ground to pass a72mesh BS test sieve 12)and thoroughly mixed, preferably by mechanical means. The weight of coal or coke necessary will vary with its ash content, but sufficient is required to provide at least5g of ash. 14.6 Preparation of ash Usin
49、g the silica trays, prepare5g of ash in the manner described for the determination of ash in coal (Part3 13) ) or coke (Part4 14) ). The loading of the trays shall not exceed0.14g/cm 2for coal or0.07g/cm 2for coke. Grind the ash in an agate mortar so that it all passes a240 mesh BStest sieve. Re-ignite the ash at800 C for one hour in the muffle furnace. Allow to cool, store in an airtight glass bottle of1oz capacity and mix thoroughly. 14.7 Loss on ignition PRINCIPLE One of two procedures may be adopted to minimize errors due
