DIN 52027-2003 Testing of carbonaceous materials - Distillation of refined coal tars《含碳物质的检测 提炼的煤焦油的蒸馏》.pdf

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1、 No part of this translation may be reproduced without the prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).Continued on pages 2 to 6.ICS 93.080.20Prfung von Kohlenstoffmater

2、ialien Siedeanalyse von rafnierten SteinkohlenteerenIn keeping with current practice in standards published by the International Organization for Standardization (ISO), a comma has been used throughout as the decimal marker.52027Distillation of rened coal tarTranslation by DIN-Sprachendienst.In case

3、 of doubt, the German-language original should be consulted as the authoritative text.DEUTSCHE NORM November 2003ForewordThis standard has been prepared by Technical Committee Prfverfahren fr Kohlenstoff und Graphit of the Normenausschuss Materialprfung (Materials Testing Standards Committee).Amendm

4、entsThis standard differs from the June 1989 edition as follows:a) the scope no longer covers bitumen;b) a different test method has been specied;c) the standard has been editorially revised and references have been updated.Previous editionsDIN 1995: 1929, 1934, 1941-11, 1960-02x; DIN DENOG 8: 1927-

5、07; DIN 12362: 1943-10, 1946-07; DIN DENOG 31: 1928-07; DIN 12575: 1943-09, 1953-05; DIN 52027: 1980-12, 1989-06.CAUTION. The use of this standard may involve hazardous materials, equipment and operations. Since this standard does not claim to deal with all the safety issues that may be associated w

6、ith applying the method, users of this standard should be familiar with standard laboratory practice. It is therefore the responsibility of the user to take appropriate safety precautions and to ensure that these comply with any relevant national regulations.Supersedes June 1989 edition.English pric

7、e group 7 www.din.de www.beuth.de04.05 9625738Page 2DIN 52027 : 2003-11All (approximate) dimensions are in millimetres.1 ScopeThe test method specied in this standard serves to fractionate rened coal tar by distillation.2 Normative referencesThis standard incorporates, by dated or undated reference,

8、 provisions from other publications. These norma-tive references are cited at the appropriate places in the text, and the titles of the publications are listed be-low. For dated references, subsequent amendments to or revisions of any of these publications apply to this standard only when incorporat

9、ed in it by amendment or revision. For undated references, the latest edition of the publication referred to applies.DIN 1333 Presentation of numerical dataDIN 12217 Borosilicate glass 3.3 tubing for laboratory useDIN 12245 Dimensions and tolerances of unground or coarsely ground glass 1:10 tapered

10、sockets for laboratory useDIN 12331 Beakers for laboratory useDIN 12779 Rapid-response distillation thermometers for laboratory useDIN 51777-1 Determination of water content of petroleum products and solvents by the Karl Fischer method (direct method)DIN 51920 Determining the Mettler softening point

11、 of carbonaceous binders and impregnating agentsDIN 51940 Sampling and sample preparation of solids, solid binders and impregnating agentsDIN EN ISO 4259 Petroleum products Determination and application of precision data in relation to meth-ods of test (ISO 4259 : 1992 + Corr 1 : 1993)DIN ISO 1773 L

12、aboratory glassware Narrow-necked boiling asks (ISO 1773 : 1997)DIN ISO 3585 Borosilicate glass 3.3 Properties (ISO 3585 : 1998)ISO 3733 : 1999 Petroleum products and bituminous materials Determination of water content Distilla-tion method3 PrincipleThe coal tar is fractionated under specied conditi

13、ons into the following substances by distillation at tempera-tures up to 350 C:a) water;b) light oil (up to 170 C);c) medium oil (170 C to 270 C);d) heavy oil (270 C to 300 C);e) anthracene oil (300 C to 350 C);f) residue (pitch).4 DesignationDesignation of the method of distilling rened coal tar in

14、 accordance with this standard (A):Test DIN 52027 A5 ApparatusThe following equipment shall be used.5.1 Distillation apparatus, as shown in gure 1, consisting of the following components:a) distillation ask, with beaded nish, as shown in gure 2, of nominal capacity 500 ml;b) two pierced cork stopper

15、s;c) DIN 12779 DST 0/360 thermometer or DIN 12779 DET 0/360 thermometer;d) DIN 12217 22 1,8 condenser tube, made of glass, 600 mm long;e) Liebig condenser (see gure 3), made of borosilicate glass 3.3 (as in ISO 3585); the connectors shall be joined to the smaller section of the evaporation tube so t

16、hat no liquid can build up if the condenser is inclined at an angle of 15 to the horizontal;f) draught screen, with wire gauze of mesh size 2 mm and a two-piece lid.Page 3DIN 52027 : 2003-115.2 Bunsen burner, with hose and hose clamp.5.3 Four receivers, each of nominal capacity 100 ml (e.g. conical

17、asks as in DIN ISO 1773 or beakers as in DIN 12331).5.4 Balance, with 0,01 g scale divisions.6 SamplesCollect and prepare the sample as specied in DIN 51940 and, if necessary, remove any water present using the procedure described in subclause 7.3.Key1 Slot for burner hose2 Two-piece lid3 Condenser

18、tube4 Two (opposite) openings, 45 mm in diameter5 Inserted wire gauze6 Opening for lighting the ame, 30 mm in diameter7 Air vents for burner, three on each side, opposing each otherFigure 1: Assembly of distillation apparatusPage 4DIN 52027 : 2003-11Key1 DIN 12245-A29/32 conical socketFigure 2: Dist

19、illation askFigure 3: Liebig condenser7 Procedure7.1 Standard procedureWeigh, to an accuracy of 0,1 g, 250 g to 300 g of sample into a distillation ask which has previously been weighed. Weigh the empty receiver to the same accuracy. Put the draught screen around the Bunsen burner, place the distill

20、ation ask on the wire gauze in the draught screen and t it with a pierced cork stopper. Push the thermometer through the stopper until the upper end of its bulb is level with the lower rim of the side tube of the ask. Using a pierced cork stopper, make a tight connection between the side tube and th

21、e condenser tube. Place the receiver under the end of the condenser tube so that it can readily be replaced without delay. Cover the draught screen with the two-piece lid.Light the Bunsen burner through the opening provided for that purpose. First heat carefully with a luminous ame so that boiling s

22、tarts after 10 minutes to 15 minutes. Then continue heating the ask, setting the burner so that two drops are collected in the receiver every second. Replace the receiver at 170 C, 270 C and 300 C without interrupting the heating.Page 5DIN 52027 : 2003-11If the sample contains so much water that the

23、 distillation rate cannot be maintained, remove the water as de-scribed in subclause 7.3.For the subsequent evaluation, it is essential to stop the distillation at (350 t 1) C by shutting off the burner shortly before reaching that temperature and removing the lid of the draught screen. On completin

24、g the distil-lation, gently heat to transfer any oil remaining in the condenser tube to the receiver. Allow the receivers to cool to ambient temperature and determine the individual fractions to an accuracy of 0,1 g by reweighing the receivers. To determine the residue, weigh the distillation ask co

25、ntaining the residue to an accuracy of 0,1 g immediately after distillation.Determine the softening point of the residue by the Mettler method specied in DIN 51920. To do this, swirl the still hot and low-viscosity residue in the distillation ask so that the residue also absorbs any oil in the upper

26、 section of the ask. Prior to pouring the residue into the test nipple, discard the rst portions to remove the oil residue in the ask neck.If the light oil fraction contains water, determine the water content of a further portion of the sample as speci-ed in DIN 51777-11).7.2 Additional instructions

27、 for samples with low ambient temperature viscosityTo distil the light oil, use a Liebig condenser with adapter instead of the condenser tube, and cool the receiver with ice. After this fraction has been collected, interrupt the distillation briey and weigh the receiver immedi-ately. Then replace th

28、e Liebig condenser with the condenser tube and continue the distillation as specied in subclause 7.1.7.3 Removal of water from samplesDistill about 1 kg of sample material in a sufciently large ask having a Liebig condenser until no more water passes over. Separate the distillate into water and ligh

29、t oil, if necessary after moderate heating. Add the light oil to the water-free sample cooled to about 80 C and mix thoroughly until the sample is homogeneous. Then perform the distillation as described in subclause 7.1.8 Evaluation8.1 Base the results on the water-free substance.8.2 If the sum of t

30、he masses of all the fractions, including the distillation residue, is less than 99 % of the initial sample mass, repeat the analysis.8.3 The distillation residue based on the water-free substance yields a pitch content, PR, expressed as a percentage. Convert this amount to pitch having a Mettler so

31、ftening point (as in DIN 51920) of 85 C, P85, us-ing equation (1):.P85= (tSPM+ 65 C) (1)wherePRis the pitch content found by distillation, as a percentage;tSPMis the Mettler softening point of the pitch (as in DIN 51920) obtained by distillation.For every 1,5 C that the experimental softening point

32、of the distillation residue is above or below 85 C, in-crease or decrease the experimental pitch content by 1 % ( m/m) and correct the anthracene oil content ac-cordingly.8.4 The anthracene oil (above 300 C) may be separated into anthracene oil no. 1 (300 C to 350 C) and anthracene oil no. 2 (above

33、350 C). The sample will contain anthracene oil no. 2 if the softening point of the residue is below 85 C with distillation up to 350 C. Anthracene oil no. 1 is obtained directly during distillation as the last fraction. The content of anthracene oil no. 2, as a percentage, is given by the difference

34、 PR P85.9 Expression of resultRefer to this standard and report the result as a percentage (absolute) to an accuracy of 0,1 % ( m/m), using the following (specimen) table.1) The procedure described in ISO 3733 may be used as an alternative.Page 6DIN 52027 : 2003-11Parameter Percentage by massWater c

35、ontent as in ISO 3733Water-free substance contentLight oil (up to 170 C)Medium oil (170 C to 270 C)Heavy oil (270 C to 300 C)Anthracene oil above 300 C after correctionPitch converted to a Mettler softening point of 85 CLossMettler softening point of distillation residue, in CMass ratio of anthracen

36、e oil no. 2 to no. 1DIN 1333 is to be taken into account when rounding to the last signicant place.10 Precision(cf. DIN EN ISO 4259)10.1 GeneralThe following details are for a single fraction. To assess the reliability of the results, use the characteristics specied in subclauses 10.2 and 10.3.10.2

37、Repeatability limit(same operator, same equipment)If two results are obtained under repeatability conditions, both results shall be considered acceptable and in conformity with this standard if they differ by no more than 1 % (absolute).10.3 Reproducibility limit(different operators, different equip

38、ment)If two separate laboratories each obtain a result under reproducibility conditions, both results shall be consid-ered acceptable and in conformity with this standard if they differ by no more than 1,5 % (absolute).11 Test reportThe test report shall refer to this standard and include the following details:a) number of samples;b) expression of results (see clause 9);c) any deviation from this standard;d) date of testing.