1、Designation: D20 03 (Reapproved 2009)Standard Test Method forDistillation of Road Tars1This standard is issued under the fixed designation D20; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision.Anumber in pa
2、rentheses indicates the year of last reapproval.Asuperscriptepsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers the distillation of road tars.1.2 The values
3、 stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety problems, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safet
4、y and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E1 Specification for ASTM Liquid-in-Glass Thermometers3. Summary of Test Method3.1 A 100-g sample is distilled at a controlled rate from a300-mL flask into tared
5、receivers. The masses of distillatefractions at a series of specified temperatures and of residue atthe maximum specified temperature are determined. If desired,the residue and distillates may be used for further testing.4. Significance and Use4.1 The distillation test separates tar into fractions a
6、ccordingto a series of specified temperatures.5. Apparatus5.1 FlaskA side-arm distillation flask, as shown in Fig. 1,conforming to the following dimensions:Diameter of bulb, outside, mm 86.0 6 1.5Diameter of neck, inside, mm 22.0 6 1.0Diameter of side-arm, inside, mm 10.0 6 0.5Height of flask, outsi
7、de, mm 131.0 6 1.5Vertical distance, bottom of bulb, outside, to hori-zontaltangent at side-arm, inside, mm93.0 6 1.5Length of side-arm, mm 220 6 5Angle of side-arm, deg 75 6 2Thickness of side-arm wall, mm 1.0 to 1.55.2 Condenser Tube A tapered glass condenser, as shownin Fig. 2 and Fig. 3, having
8、the following dimensions:Outside diameter of small end, mm 12.5 6 1.5Outside diameter of large end, mm 28.5 6 3.0Length, mm 360 6 4Length of uniformly tapered part, mm 100 6 55.3 Source of Heat A heat source consisting of a bunsenor meker-type burner (Note 1) or an electric heater. The electricheate
9、r3shall have an output variable of 750 W and an upper1This method is under the jurisdiction of ASTM Committee D04 on Road andPaving Materials and is the direct responsibility of Subcommittee D04.43 onSpecifications and Test for Tar and Tar Products.Current edition approved Dec. 1, 2009. Published Ja
10、nuary 2010. Originallyapproved in 1911. Last previous edition approved in 2003 as D20 03. DOI:10.1520/D0020-03R09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to th
11、e standards Document Summary page onthe ASTM website.3The Precision Ful-Kontrol 750-W heater with built-in variable transformercontrol, available from Precision Scientific Co., Chicago, IL, has been foundsatisfactory. This heater is only available for 115 V. 50/60 Hz. If you are aware ofalternative
12、suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.FIG. 1 Distillation Flask1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Con
13、shohocken, PA 19428-2959, United States.refractory with dimensions as shown in Fig. 4. The temperatureof the heater shall be controlled by a variable transformer orrheostat suitable for the voltage used, and shall be fitted with aclamp for mounting on a vertical support rod.FIG. 2 Apparatus Assembly
14、 for Flame DistillationFIG. 3 Apparatus Assembly for Electric Heater DistillationFIG. 4 Upper Part of Electric HeaterD20 03 (2009)2NOTE 1An artificial gas model used with natural gas has been foundto give a uniform and easily controlled source of heat.5.4 Flask Shield and Cover for Flame Distillatio
15、nA steelshield (preferably stainless) lined with 3-mm Transite board,non-asbestos, with two-part cover made from 6-mm Transiteboard of the form and dimensions shown in Fig. 5.5.5 Flask Shield and Cover for Electric-HeaterDistillationA steel shield (preferably stainless) fitted withmica windows, and
16、a cover of the same construction anddimensions as those for flame distillation (5.4) except for theheight of the shield (see Fig. 6).5.6 Gauze for Flame DistillationTwo sheets of 1.0-mmopening wire gauze made of 0.56-mm diameter nickel-chromium wire measuring a minimum of 125 mm in diameteror (125 b
17、y 125-mm) square.5.7 Burner Chimney for Flame DistillationConstruct acylindrical metal shield approximately 100 mm high, 95 to 105mm in diameter, and having a peephole 25 mm in diametercentered about 32 mm below the ring support. The top of theshield shall be flanged to permit its being suspended fr
18、om thering support.5.8 ReceiversErlenmeyer flasks or beakers having anominal capacity of 50 to 125 mL, and tared to the nearest 0.1g.5.9 Balance and Masses, accurate to 0.1 g.5.10 ThermometerAnASTM High Distillation Thermom-eter having a range from 2 to + 400C and conforming to therequirements for T
19、hermometer 8C as prescribed in Specifica-tion E1.6. Preparation of Sample6.1 Thoroughly stir or otherwise mix the sample immedi-ately before removing the portion for testing, to ensure thatsuch portion will be representative of the sample. If warming isnecessary, take care to avoid loss of volatile
20、material.7. Preparation of Apparatus7.1 Assemble the apparatus as follows (see Fig. 2 and Fig.3):7.1.1 Suspend the burner chimney by its flange from thesupport ring, place the specified two sheets of flat wire gauzeon the burner chimney, and place the flask shield on the uppersheet of gauze. In case
21、 the electric heater is used, attach theheater to a vertical support so that at the end of the distillationit can be lowered at least 150 mm. Place the upper refractoryon the heater with the larger opening facing upwards. Set theflask shield on the upper refractory.7.1.2 Inset the thermometer throug
22、h a new and rolled selectquality regular-length cork of suitable size. Position the ther-mometer and cork in the neck of the flask so that the cork fitstightly and the bottom of the cork is from 23 to 28 mm abovethe lowest point of the junction between the side-arm and theneck of the flask. Then adj
23、ust the thermometer in the cork sothat the top of the bulb is level with the lowest point of theFIG. 5 Shield and Cover for Flame DistillationFIG. 6 Shield for Use with Electric HeaterD20 03 (2009)3juncture between the side-arm and the neck of the flask. Alignthe stem of the thermometer on the axis
24、of the bulb through theneck of the flask.7.1.3 When using the flame distillation apparatus, place theflask in the flask shield with its bulb resting on the gauze.Position the burner so that it is directly beneath the point wherethe bulb of the flask contacts the gauze. If the electric heater isused,
25、 place the flask in the flask shield and support the flask sothat its bottom is between 4 and 7 mm above the heating coils.7.1.4 Connect the condenser tube to the side-arm of the flaskwith a tight cork joint, having the side-arm project 30 to 50 mmthrough the cork. The distance from the neck of the
26、flask to theoutlet end of the condenser tube shall be between 500 and 600mm. Support the condenser tube in a position such that it is inalignment with the side-arm of the flask, and the thermometeris vertical. Place the shield cover over the flask shield aroundthe neck of the flask.8. Procedure8.1 W
27、eigh the flask (along with the thermometer and cork)to the nearest 0.1 g and then weigh 100.0 6 0.1 g of the sampleinto the flask.8.2 Apply heat to the flask so that the first drop of distillate(oil or water) falls from the end of the condenser tube in 5 to15 min. Within 2 min after the first drop,
28、adjust the rate ofdistillation, and subsequently maintain the rate, so that from 50to 70 drops per min fall from the end of the condenser. Warmthe condenser tube whenever necessary to prevent accumula-tion of solid distillates in the tube.8.3 Collect the distillate fractions in tared receivers, chan
29、g-ing receivers as the thermometer indicates the maximumtemperature, corrected as described in 8.4, for each specifiedfraction. The following fractions are usually specified.Up to 170C170 to 235C235 to 270C270 to 300CResidue at 300CFractions at other temperatures, such as 170 to 200C and200 to 235C,
30、 or 300 to 355C and residue at 355C, aresometimes required.8.4 Do not change the position of the thermometer duringthe distillation. Make no correction for the emergent stem ofthe thermometer, but if the barometric pressure is outside therange of 756 to 765, adjust (but do not report) the temperatur
31、ein accordance with Table 1.8.5 When the maximum temperature specified for the test isindicated by the thermometer, immediately remove the flameand the flask-shield cover; or when the electric heater is usedas a source of heat, immediately remove the flask shield coverand lower the heater at least 1
32、50 mm. Allow the apparatus tocool, for at least 5 min, or until no vapors are visible. Drain anyoil remaining in the condenser tube into the receiver containingthe last fraction.8.6 Weigh the receivers containing the distillate fractions tothe nearest 0.1 g. Weigh the flask (with the thermometer inp
33、lace) and residue to the nearest 0.1 g.8.7 Should the fraction to 170C contain water, determinethe water volume and calculate the new mass of oil distillate,assuming that 1 mL of water weighs 1 g. The amount of watercontained in this fraction may be determined by either of thefollowing methods.8.7.1
34、 Transfer the fraction after weighing, to a tube orcylinder graduated in 0.1 mL. Rinse the receiver several timeswith toluene, adding the rinsings to the tube or cylindercontaining the fraction or,8.7.2 The fraction of 170C may be collected in a taredgraduated cylinder having a flared top. After wei
35、ghing, addtoluene which will result in a clear separation of the water andoil distillate.8.8 If the residue from distillation is required for furthertesting, lower the thermometer until its bulb is in the liquidresidue. If the residue is not completely fluid, heat it carefullyto a temperature not ex
36、ceeding 150C by holding the bulb ofthe flask over a wire gauze heated by a gas burner or byimmersion in a suitable bath whose temperature does notexceed 150C. Incline the flask and rotate it so that the fluidresidue will flow around the sides, and collect any oils thathave condensed on the upper sur
37、faces of the flask. Mix thecontents of the flask until they are homogeneous. Allow theresidue to cool to a temperature at which it can be readilypoured from the flask without loss of volatile material and thenpour it into the desired testing equipment or into a suitablereceptacle. Cover the receptac
38、le.9. Calculation9.1 Convert the distillation results to a water-free basis, D,in %, as follows:D 5 F 2 W! 3 100/100 2 W!# (1)Second and Subsequent Fractions Including Residue:D 5 F 3 100/100 2 W!# (2)where:F = mass of the fraction or residue, g andTABLE 1 Adjustment of Distillation Test Temperature
39、s forBarometric PressureBarometricPressure,mm HgFractionation Temperatures for VariousBarometric Pressure Ranges, C786 to 795 172 202 237 272 302 357776 to 785 171 201 236 271 301 356766 to 775 171 201 236 271 301 356756 to 765 170 200 235 270 300 355746 to 755 169 199 234 269 299 354736 to 745 169
40、199 234 269 299 354726 to 735 168 198 233 268 298 353716 to 725 168 198 233 267 297 352706 to 715 167 197 232 267 297 351696 to 705 167 197 231 266 296 351686 to 695 166 196 231 265 295 350676 to 685 166 195 230 265 295 349666 to 675 165 195 230 264 294 348656 to 665 165 194 229 264 293 348646 to 65
41、5 164 194 228 263 292 347636 to 645 164 193 228 262 292 346626 to 635 163 193 227 262 291 345616 to 625 163 192 226 261 290 345606 to 615 162 191 226 260 290 344596 to 605 162 191 225 260 289 343D20 03 (2009)4W = millilitres of water, expressed as grams, in the frac-tion distilling to 170C.10. Repor
42、t10.1 Report the following information:10.1.1 The results of the distillation test as percentages tothe nearest 0.1 %, based on the mass of water-free material. Forroad tars, it is customary to report the total distillate to a seriesof temperatures corresponding to the maxima specified for thefracti
43、ons.11. Precision11.1 The following criteria should be used for judging theacceptability of results at the 95 % probability level:11.1.1 Repeatability Duplicate results by the same opera-tor should be considered suspect if the reported percentagediffers by more than the “r” value listed in Table 2.1
44、1.1.2 Reproducibility Results submitted by two labora-tories should be considered suspect if the reported percentagediffers by more than the “R” value listed in Table 2.NOTE 2The precision limits given only apply to fractions havinggreater than 2.0 % distillate.12. Keywords12.1 distillation; road ta
45、rASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, ar
46、e entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standa
47、rdsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Commit
48、tee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress
49、 or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 2 Repeatability (r) and Reproducibility (R) for distillationfractionsFraction r Rup to 170C 0.6 1.8170 to 235C 1.8 5.2235 to 275C 2.4 5.0270 to 300C 1.9 4.2D20 03 (2009)5
