ISO-609-1996.pdf
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1、INTERNATIONAL STANDARD IS0 609 Second edition 1996-02-I 5 AN251 IBPntemat Dot se!c Solid mineral fuels - Determination of carbon and hydrogen - High temperature combustion method Combustibles minkaux solides - Dosage du carbone et de I hydrogene - MBthode par combustion B haute tempkrature - - 1 gff
2、i 1 k 75.160.10 Ref. No. IS0 609:1996/Cor.l:1996(E) Descriptors: solid fuels, fossil fuels, coal, lignite, coke, chemical analysis, determination of content, carbon, hydrogen, combustion analysis, gravimetric analysis. 0 IS0 1996 Printed in Switzerland Copyright International Organization for Standa
3、rdization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/20/2007 07:14:05 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 609:1996/Cor.l:1996(E) Page 8, subclause 8.3 Change “(see note 8)” to “(see note 9)“at the
4、 end of the first paragraph. Change “(see note 8)” to “(see note 9)” and “(see note 9)” to “(see note IO)“, in the second paragraph. Page 9, subclause 10.4 Change “formula” to “equation”at the end of the first paragraph (introducing the equation) Page 1 I, clauses A.2 and A.3 Change “formula” to “eq
5、uation” at the end of the first paragraph (introducing the equation). 2 IS0 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/20/2007 07:14:05 MDTNo reproduction or networking permitted wi
6、thout license from IHS -,-,- INTERNATIONAL STANDARD 0 IS0 IS0 609:1996(E) Solid mineral fuels - Determination of carbon and hydrogen - High temperature combustion method 1 Scope This International Standard specifies a method of de- termining the total carbon and the total hydrogen in hard coal, brow
7、n coal and lignite, and coke, by a high temperature combustion method. The results include the carbon in the carbonates and the hydrogen combined in the moisture and in the water of constitution of silicates. A determination of moisture is carried out at the same time, and an ap- propriate correctio
8、n is applied to the hydrogen value obtained by combustion. A determination of carbon dioxide may also be made and the total carbon value corrected for the presence of mineral carbonates. 2 Normative references The following standards contain provisions which, through reference in this text, constitu
9、te provisions of this International Standard. At the time of publi- cation, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most re- cent editions of
10、 the standards indicated below. Members of IEC and IS0 maintain registers of cur- rently valid International Standards. IS0 331:1983, Coal - Determination of moisture in the analysis sample - Direct gravimetric method. IS0 687:1974, Coke - Determination of moisture in the analysis sample. IS0 925: 1
11、980, Solid mineral fuels - Determination of carbon dioxide content - Gravimetric method. IS0 1015:1992, Brown coals and /ignites - Determi- nation of moisture content - Direct volumetric method. IS0 1170:1977, Coal and coke - Calculation of analyses to different bases. IS0 1988: 1975, Hard coal - Sa
12、mpling. IS0 2309:1980, Coke - Sampling. IS0 5068:1983, Brown coals and /ignites - Determi- nation of moisture content - Indirect gravimetric method. IS0 5069-2:1983, Brown coals and /ignites - Prin- ciples of sampling - Part 2: Sample preparation for determination of moisture content and for general
13、 analysis. 3 Principle A known mass of coal or coke is burnt in a stream of oxygen, at a temperature of 1 350 “C, in a tube impervious to gases. All the hydrogen is converted to water and all the carbon to carbon dioxide. These products are absorbed by suitable reagents and de- termined gravimetrica
14、lly. The chlorine and oxides of sulfur which are formed are retained by a silver gauze roll at the outlet end of the tube. 4 Reagents and materials WARNING - Care should be exercised when handling reagents, many of which are toxic and corrosive. During the analysis, unless otherwise stated, use only
15、 reagents of recognized analytical grade and only dis- tilled water or water of equivalent purity. 1 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/20/2007 07:14:05 MDTNo reproduction o
16、r networking permitted without license from IHS -,-,- IS0 609:1996(E) 4.1 Magnesium perchlorate, anhydrous, less than I,2 mm in size and preferably within the size range I,2 mm to 0,7 mm. WARNING - Due regard must be taken of local regulations when disposing of exhausted mag- nesium perchlorate. Reg
17、eneration of magnesium perchlorate must not be attempted, owing to the risk of explosion. 4.2 Sodium hydroxide on an inert base, preferably of a coarse grading, for example 3,0 mm to I,5 mm, but not finer than the grading I,2 mm to 0,7 mm, and preferably of the self-indicating type. 4.3 Aluminium ox
18、ide (alumina), finely divided, ap- proximately 0,l mm in size. 4.4 Sodium tetraborate, standard volumetric sol- ution, c(NazB,O,) = 0,025 mol/l. Dissolve 9,534 2 g of sodium tetraborate decahydrate in water and dilute to 1 litre. Mix thoroughly. 4.5 Hydrogen peroxide, approximately 30 % (m/m). 4.6 P
19、ure silver gauze, of mesh approximately 1 mm, made of wire approximately 0,3 mm in diam- eter. 4.7 Oxygen, hydrogen-free, preferably prepared from liquid air and not by electrolysis. Electrolytically prepared oxygen shall be passed over red-hot copper oxide before use to remove any trace of hydrogen
20、. 4.8 Mixed indicator solution 4.8.1 Solution A Dissolve 0,125 g of 2-(4-dimethylaminophenyl- azo)benzoic acid, sodium salt (methyl red) in 100 ml of water. 4.8.2 Solution B Dissolve 0,083 g of 3,7-bis(dimethylamino)pheno- thiazine-5-ylium chloride (methylene blue) in 100 ml of water. Store in a dar
21、k bottle. 4.8.3 Mixed solution Mix equal volumes of solution A and solution B. Store in a dark bottle. Discard the mixed solution after 1 week. 4.9 Air, compressed. 4.10 Glass wool. 5 Apparatus 5.1 Analytical balance, capable of weighing to the nearest 0,l mg. 5.2 Graduated glassware, conforming to
22、the re- quirements for class A in the International Standards prepared by ISO/TC 48, Laboratory glassware and re- lated apparatus. 5.3 Two purification trains, one for absorbing water vapour and carbon dioxide from the oxygen used for the combustion and the other for similarly treating the air used
23、for sweeping out the absorption train before and after a determination. Assemble each train using a series of U-tubes or Midvale tubes con- taining the following reagents in the order stated, in the direction of flow: a) b) cl magnesium perchlorate (4.1) for absorbing water; sodium hydroxide on an i
24、nert base (4.2) for ab- sorbing dioxide; magnesium perchlorate for absorbing the water evolved in the reaction between carbon dioxide and sodium hydroxide. The purification trains shall be large enough to render frequent recharging unnecessary, even with continu- ous use. NOTE 1 Midvale tubes that h
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