1、 Reference number ISO 1017:2006(E) ISO 2006INTERNATIONAL STANDARD ISO 1017 Third edition 2006-12-01 Brown coals and lignites Determination of acetone-soluble material (“resinous substance”) in the benzene-soluble extract Charbons bruns et lignites Dtermination des matires solubles dans lactone de le
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7、 ISO 2006 All rights reserved iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body int
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11、ISO shall not be held responsible for identifying any or all such patent rights. ISO 1017 was prepared by Technical Committee ISO/TC 27, Solid mineral fuels, Subcommittee SC 5, Methods of analysis. This third edition cancels and replaces the second edition (ISO 1017:1985), which has been technically
12、 revised. INTERNATIONAL STANDARD ISO 1017:2006(E) ISO 2006 All rights reserved 1 Brown coals and lignites Determination of acetone-soluble material (“resinous substance”) in the benzene-soluble extract 1 Scope This International Standard specifies a method of determining the mass fraction of acetone
13、-soluble material (“resinous substance”) in the benzene-soluble extract from brown coals and lignites. NOTE The acetone extract will also contain a percentage of wax dissolved simultaneously with the “resinous substance“. 2 Normative references The following referenced documents are indispensable fo
14、r the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 975, Brown coals and lignites Determination of yield of benzene-soluble extract Semi-automatic metho
15、d 3 Principle The sample of benzene-soluble extract from brown coal or lignite obtained by the procedure described in ISO 975 is extracted with acetone at a temperature of 18 to 22 C. The soluble fraction is filtered or centrifuged off and, after evaporation of the solvent, dried to constant mass. T
16、he percentage of acetone-soluble material is calculated from the mass of residue after drying. 4 Reagent 4.1 Acetone, of analytical reagent grade. WARNING Acetone is flammable, and toxic by inhalation, ingestion or skin absorption 5 Apparatus 5.1 Centrifuge, capable of operating at 1 600 r/min. The
17、rotational frequency of the centrifuge shall be sufficient to ensure separation of the soluble fraction from the parent coal. 5.2 Glass centrifuge vessels, either cylindrical or conical, of capacity 15 ml and fitted with ground-glass stoppers, for use in the centrifuge. 5.3 Evaporating dish, of glas
18、s or silica, about 20 mm high and 50 mm in diameter. ISO 1017:2006(E) 2 ISO 2006 All rights reserved5.4 Vacuum drying oven, electrically heated, in which a temperature of 80 2 C and a pressure of about 50 kPa can be maintained. 5.5 Air oven, electrically heated, capable of maintaining a temperature
19、of 100 to 110 C. 5.6 Infrared drying lamp. 5.7 Wire-cloth test sieve, of nominal aperture size 100 m. 6 Preparation of sample The residue obtained from the benzene-soluble extract obtained by the method specified in ISO 975 shall be crushed to pass the sieve (5.7). If the residue is viscous liquid,
20、it shall be cooled in solid carbon dioxide to 80 C, and then crushed. 7 Procedure 7.1 Test condition The high selectivity of acetone requires a strict temperature control during the determination. The temperature of the solvent, the room temperature at the beginning of the determination and the room
21、 temperature at the end of the determination shall not differ from each other by more than 0,5 C and shall be within the range 18 to 22 C. 7.2 Determination Record the room temperature at the beginning of the extraction (t 2 ) and the temperature of the acetone (t 1 ). Weigh, to the nearest 1 mg, ab
22、out 0,5 g of the sample into a glass vessel (5.2). Add 7 ml of the acetone (Clause 4) and shake for exactly 2 min. Minimise warming of the solvent by holding the glass vessel at the upper end between the index and middle fingers, while the thumb secures the ground-glass stopper. Rubber finger-shield
23、s should be worn. Allow the acetone-soluble fraction to clear and decant it into a tared, dry evaporating dish (5.3). If the fraction does not clear, it may be centrifuged for 1 min and then decanted, or filtered if necessary using the smallest convenient size of filter paper, into the evaporating d
24、ish. Wash back any particles of benzene-soluble extract adhering to the upper end of the glass vessel, after shaking by cautiously tilting the vessel. Let any washed fraction settle or centrifuge it. Add a further 7 ml of the acetone to the glass vessel and repeat the above extraction (but not more
25、than 4 times) until the extract fraction is colourless. Record the room temperature at the end of the extraction (t 3 ) to the nearest 0,1 C. If a filter has been used, rinse it with a few millilitres of acetone and add the rinsings to the evaporating dish. Place the evaporating dish in the vacuum d
26、rying oven (5.4) and evaporate off the acetone at 80 2 C and about 50 kPa. Alternatively, the evaporation may be carried out using the infrared drying lamp (5.6). Transfer the dish to the air oven (5.5) and dry to constant mass at 105 3 C. ISO 1017:2006(E) ISO 2006 All rights reserved 3 8 Expression
27、 of results The mass fraction of acetone-soluble material, w Ac,20 , in the sample analysed, expressed as a percentage, is given by the equation , 2 Ac 20 1 Km w m = where m 1is the mass, in grams, of benzene-soluble extract taken; m 2is the mass, in grams, of acetone-soluble material recovered; K =
28、 100 + 2,5(20 t) in which 123 3 ttt t + = t 1being the temperature, in degrees Celsius, of the acetone used for the extraction; t 2being the room temperature, in degrees Celsius, at the beginning of the determination; t 3being the room temperature, in degrees Celsius, at the end of the determination
29、. The result (the mean of duplicate determinations, see 9.1) should be reported to the nearest 0,1 % (mass fraction). 9 Precision of the method Maximum acceptable difference between Mass fraction of acetone-soluble material results % repeatability reproducibility less than 20 0,3 % absolute 0,5 % ab
30、solute 20 to 30 0,4 % absolute 0,7 % absolute 30 to 50 0,5 % absolute 0,9 % absolute over 50 1,0 % of the mean result 1,8 % of the mean result 9.1 Repeatability The results of duplicate determinations, carried out in the same laboratory, by the same operator, using the same apparatus, on the same be
31、nzene-soluble extract, within short intervals of time, should not differ by more than the above value. 9.2 Reproducibility The means of the results of duplicate determinations, carried out in two different laboratories on representative test portions taken from the same benzene-soluble extract, shou
32、ld not differ by more than the above value. ISO 1017:2006(E) 4 ISO 2006 All rights reserved10 Test report The test report should include the following information: a) identification of the product tested; b) a reference to this International Standard; c) the results and the method of expression used. ISO 1017:2006(E) ICS 73.040 Price based on 4 pages ISO 2006 All rights reserved
