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1、INTERNATIONAL STANDARD ANSI Internat I?ex a=400net; p o=isocs; s=central Printed in Switzerland ii Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Defense Supply Ctr/9960866100 Not for Resale, 04/24/2007 09:48:18 MDTNo reproduction or networki
2、ng permitted without license from IHS -,-,- INTERNATIONAL STANDARD 0 IS0 IS0 587: 1997(E) Solid mineral fuels - Determination of chlorine using Eschka mixture 1 Scope This International Standard specifies a method of determining the chlorine content of hard coal, brown coals and lignite, and coke us
3、ing Eschka mixture. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agre
4、ements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 331 :I 983, Coal - Determination of moisture in t
5、he analysis sample - Direct gravimetric method. IS0 667:1974, Coke - Determination of moisture in the analysis sample. IS0 1015:1992, Brown coals and /ignites - Determination of moisture content - Direct volumetric method. IS0 1170: 1977, Coal and coke - Calculation of analyses to different bases. I
6、S0 1968:1975, l-lard coal - Sampling. IS0 2309:1980, Coke - Sampling. IS0 5066:1963, Brown coals and /ignites - Determination of moisture content - Indirect gravimetric method. IS0 5069-2:1983, Brown coals and /ignites - Principles of sampling - Part 2: Sample preparation for determination of moistu
7、re content and for genera/ analysis. IS0 941 l-l :I 994, Solid mineral fuels - Mechanical sampling from moving streams - Part 1: Coal. IS0 9411-2:1993, Solid mineral fuels - Mechanical sampling from moving streams - Part 2: Coke. 3 Principle A known mass of sample is ignited in intimate contact with
8、 Eschka mixture in an oxidizing atmosphere to remove combustible matter and to convert the chlorine to alkaline chlorides. These are extracted with nitric acid or water and determined by either the Volhard or the Mohr method, or by potentiometric titration using an Ion Selective Electrode (ISE). 1 C
9、opyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Defense Supply Ctr/9960866100 Not for Resale, 04/24/2007 09:48:18 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 587: 1997(E) IS0 4 Reagents WARNING - Care should be
10、 exercised when handling reagents, many of which are toxic and corrosive. During analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water, or water of equivalent purity. 4.1 For all methods 4.1 .I Eschka mixture Mix two parts by mass of light, calc
11、ined magnesium oxide with one part of anhydrous sodium or potassium carbonate. The mixture shall entirely pass a test sieve of 0,212 mm nominal aperture. 4.1.2 Nitric acid, concentrated, chlorine-free, approximately 70 % (m/m). 4.2 For the Volhard and ISE methods 4.2.1 Silver nitrate, standard volum
12、etric solution, c(AgNOs) = 0,025 mol/l. Heat crushed, crystalline silver nitrate at 125 “C for two to three hours. Dissolve 4,247 g in water and dilute to 1 I. Store in an amber glass bottle. 4.3 For the Volhard method only 4.3.1 3,5,5-trimethylhexan-l-01. 4.3.2 n-Hexan-l-01. 4.3.3 Potassium thiocya
13、nate, standard volumetric solution, c(KSCN) = 0,025 mol/l. Dissolve 2,4 g of potassium thiocyanate in water and dilute to 1 I. Titrate against the silver nitrate solution (4.2.1) and calculate the exact equivalence. 4.3.4 Iron(lll) alum (ammonium iron(lll) sulfate) indicator, saturated solution. Sat
14、urate 100 ml of water with approximately 125 g or iron(lll) alum (NH V, is the volume, in millilitres, of the potassium thiocyanate solution (4.3.3) used in the determination (7.2.1); V, is the volume, in millilitres, of the potassium thiocyanate solution (4.3.3) used in the blank test (7.3); m is t
15、he mass, in grams, of the test portion. 8.2 Mohr titration The chlorine content (WC,) of the sample, as analyzed, expressed as a percentage by mass, is given by the formula WC, = 3,545c*(V,-vq) m where c2 is the concentration, in moles per litre, of the silver nitrate solution (4.4.1); V, is the vol
16、ume, in millilitres, of the silver nitrate solution (4.4.1) used in the determination (7.2.2); V, is the volume, in millilitres, of the silver nitrate solution (4.4.1) used in the blank test (7.3); m is the mass, in grams, of the test portion. 8.3 ISE method The chlorine content (WC,) of the sample,
17、 as analyzed, expressed as a percentage by mass, is given by the formula WI = 3,545 c3(V5 -V,) m where c3 is the concentration, in moles per litre, of the silver nitrate solution (4.2.1); V, is the volume, in millilitres, of the silver nitrate solution (4.2.1) used in the determination (7.2.3); V, i
18、s the volume, in millilitres, of the silver nitrate solution (4.2.1) used in the blank test (7.3); m is the mass, in grams, of the test portion. 8.4 All methods Report the results as the mean of duplicate determinations, to the nearest 0,Ol %. The results of the determination described in this Inter
19、national Standard are reported on the “air-dried” basis. Calculation of results to other bases in dealt with in IS0 1170. 5 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Defense Supply Ctr/9960866100 Not for Resale, 04/24/2007 09:48:18 MDTNo
20、 reproduction or networking permitted without license from IHS -,-,- IS0 587:1997(E) 9 Precision 9.1 Repeatability limit IS0 The results of duplicate determinations, carried out at different times within a short interval, in the same laboratory, by the same operator, with the same apparatus, on repr
21、esentative portions taken from the same analysis sample, should not differ by more than 0,03 % absolute. 9.2 Reproducibility critical difference The means of the results of duplicate determinations, carried out in each of two laboratories, on representative portions taken from the same sample after
22、the last stage of sample separation, should not differ by more than 0,06 % absolute. 10 Test report The test report shall include the following information: 4 reference to this International Standard; W an identification of the sample tested; c) the results and the method of expression used; 4 any u
23、nusual features noted during the determination; 4 any operation not included in this International Standard, or regarded as optional; f) the date of the test. 6 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Defense Supply Ctr/9960866100 Not
24、for Resale, 04/24/2007 09:48:18 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 IS0 587: 1997(E) Annex A (informative) Derivation of factors used in calculations in this International Standard A.1 General In this annex, relative atomic masses and relative molecular mass
25、es are represented by the chemical formulae in square brackets. The following equivalences occur in the determinations in this International Standard AgNO, = Cl AgNOs = KSCN A.2 Volhard method The percentage by mass, WC, of chlorine in the sample is given by the formula WC, = (CV- c,vj) - (CV - c,V2
26、) x 3545 100 x- 1 000 m 3,545 c, (V, - v,) m where V is the volume, in millilitres, of the silver nitrate solution (4.2.1) used in the determination (7.2.1) and the blank test (7.3); v, is the volume, in millilitres, of the potassium thiocyanate solution (4.3.3) used in the determination (7.2.1); v2
27、 is the volume, in millilitres, of the potassium thiocyanate solution (4.3.3) used in the blank test (7.3); C is the concentration, in moles per litre, of the silver nitrate solution (4.2.1); Cl is the concentration, in moles per litre, of the potassium thiocyanate solution (4.3.3); m is the mass, i
28、n grams, of the test portion; 35,45 is the relative atomic mass of chlorine, Cl. A.3 Mohr method The percentage by mass, WC, of chlorine in the sample is given by the formula WC, = c2 (V, - V,) x 35,45 xE! 1000 m 3,545 c2 (V, - V,) m where c2 is the concentration, in moles per litre, of the silver n
29、itrate solution (4.4.1); v3 is the volume, in millilitres, of the silver nitrate solution (4.4.1) used in the determination (7.2.2); v4 is the volume, in millilitres, of the silver nitrate solution (4.4.1) used in the blank test (7.3); m is the mass, in grams, of the test portion; 35,45 is the relat
30、ive atomic mass of chlorine, Cl. 7 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Defense Supply Ctr/9960866100 Not for Resale, 04/24/2007 09:48:18 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 587: 1997(E) A.4
31、 ISE method IS0 The percentage by mass, Wc, of chlorine in the sample is given by the formula WC, = c3 (VI - V,) x 3545 x 100 1000 m 3,545 c3 (V, - V,) m where c3 is the concentration, in moles per litre, of the silver nitrate solution (4.2.1); v5 is the volume, in millilitres, of the silver nitrate
32、 solution (4.2.1) used in the determination (7.2.3); v6 is the volume, in millilitres, of the silver nitrate solution (4.2.1) used in the blank test (7.3); m is the mass, in grams, of the test portion; 35,45 is the relative atomic mass of chlorine, Cl. Copyright International Organization for Standa
33、rdization Provided by IHS under license with ISO Licensee=Defense Supply Ctr/9960866100 Not for Resale, 04/24/2007 09:48:18 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO587:1997(E) ICS 75160.10 Descriptors: fossil fuels, solid fuels, coal, lignite, coke, chemical anal
34、ysis, determination of content, chlorine, extraction methods. Price based on 8 pages Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Defense Supply Ctr/9960866100 Not for Resale, 04/24/2007 09:48:18 MDTNo reproduction or networking permitted without license from IHS -,-,-