1、Designation: D 20 03Standard Test Method forDistillation of Road Tars1This standard is issued under the fixed designation D 20; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision. A number in parentheses indi
2、cates the year of last reapproval. A superscriptepsilon (e) 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 This standard does no
3、t 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 safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standard
4、s:E 1 Specification for ASTM Thermometers23. Summary of Test Method3.1 A 100-g sample is distilled at a controlled rate from a300-mL flask into tared receivers. The masses of distillatefractions at a series of specified temperatures and of residue atthe maximum specified temperature are determined.
5、If desired,the residue and distillates may be used for further testing.4. Significance and Use4.1 The distillation test separates tar into fractions accordingto a series of specified temperatures.5. Apparatus5.1 FlaskA side-arm distillation flask, as shown in Fig. 1,conforming to the following dimen
6、sions: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, outside, 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 5Ang
7、le 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 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
8、 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 electricheater3shall have an output variable of 750 W and an upperrefractory with dimensions as shown in Fig. 4. The temperatureof the heater shall be controlled b
9、y a variable transformer orrheostat suitable for the voltage used, and shall be fitted with aclamp for mounting on a vertical support rod.NOTE 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 Dist
10、illationA 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 window
11、s, and a cover of the same construction and1This method is under the jurisdiction of ASTM Committee D04 on Road andPaving Materials and is the direct responsibility of Subcommittee D04.43 onSpecifications and Tests for Tar and Tar Products.Current edition approved July 10, 2003. Published September
12、2003. Originallyapproved in 1911. Last previous edition approved in 1999 as D 20 99.2Annual Book of ASTM Standards, Vol 14.03.3The Precision Ful-Kontrol 750-W heater with built-in variable transformercontrol, available from Precision Scientific Co., Chicago, IL, has been foundsatisfactory. This heat
13、er is only available for 115 V. 50/60 Hz.FIG. 1 Distillation Flask1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.dimensions as those for flame distillation (5.4) except for theheight of the shield (see Fig. 6).5.6 Gauze for Flame Di
14、stillationTwo 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 by 125-mm) square.5.7 Burner Chimney for Flame DistillationConstruct acylindrical metal shield approximately 100 mm high, 95 to 105FIG. 2 Apparatus Assembly
15、 for Flame DistillationFIG. 3 Apparatus Assembly for Electric Heater DistillationFIG. 4 Upper Part of Electric HeaterD20032mm 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 from ther
16、ing 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 ThermometerAn ASTM High Distillation Thermom-eter having a range from 2 to + 400C and conforming to therequirements for Thermom
17、eter 8C as prescribed in Specifica-tion E 1.6. 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 mater
18、ial.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 the
19、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 through a n
20、ew 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 adjust t
21、he thermometer in the cork sothat the top of the bulb is level with the lowest point of thejuncture between the side-arm and the neck of the flask. Alignthe stem of the thermometer on the axis of the bulb through theneck of the flask.7.1.3 When using the flame distillation apparatus, place theflask
22、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, place the flask in the flask shield and support the flask sothat its bottom is between 4 and 7 mm above th
23、e 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 flask to theoutlet end of the condenser tube shall be between 500 and 600mm. Support the condenser tube in
24、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.FIG. 5 Shield and Cover for Flame DistillationFIG. 6 Shield for Use with Electric HeaterD200338. Procedure8.1 Weigh the flas
25、k (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, adjust the ra
26、te 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, chang-ing receive
27、rs 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, or 300 to 35
28、5C 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 temperaturein accordanc
29、e 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 150 mm. Allow
30、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 inplace) and res
31、idue 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 Transfer the
32、 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 weighing, addtol
33、uene 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 exceeding 150C
34、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 surfaces of the
35、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 receptacle.9. Calcula
36、tion9.1 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 andW = millilitres of water, expressed as grams, in the frac-tion d
37、istilling to 170C.10. Report10.1 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 max
38、ima specified for thefractions.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
39、” value listed in Table 2.TABLE 1 Adjustment of Distillation Test Temperatures 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
40、 765 170 200 235 270 300 355746 to 755 169 199 234 269 299 354736 to 745 169 199 234 269 299 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 685 166 195 230 265 295 349
41、666 to 675 165 195 230 264 294 348656 to 665 165 194 229 264 293 348646 to 655 164 194 228 263 292 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 343D2003411.1.2 Reproducibility
42、 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 tarASTM International t
43、akes 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, are entirely their own
44、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 standardsand should be addr
45、essed 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 Committee on Standards, at
46、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 or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).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 4.2D20035
