1、Designation: D 402 0227/74 (88)American Association StateHighway and Transportation Officials StandardAASHTO No.: T78Standard Test Method forDistillation of Cut-Back Asphaltic (Bituminous) Products1This standard is issued under the fixed designation D 402; the number immediately following the design
2、ation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by
3、agencies of the Department of Defense. This method was adopted as a joint ASTM-IPstandard in 1961.1. Scope1.1 This test method covers a distillation test for cut-backasphaltic (bituminous) products.1.2 The values given in SI units are to be regarded as thestandard. The inch-pound units given in pare
4、ntheses are forinformation only.1.3 This standard does not purport to address all of thesafety concerns, 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 limitati
5、ons prior to use.2. Referenced Documents2.1 ASTM Standards:D 86 Test Method for Distillation of Petroleum Products atAtmospheric Pressure2D 370 Test Method for Dehydration of Oil-Type Preserva-tives3E 1 Specification for ASTM Thermometers4E 133 Specification for Distillation Equipment5E 220 Test Met
6、hod for Calibration of Thermocouples byComparison Techniques42.2 IP Standards:IP 123/ASTM D 86, Distillation of Petroleum ProductsThermometers as specified in IP StandardsCrow Receiver as specified in British Standards 658:1989C.O.3Standard Methods for Testing Tar and its Products(Published by the U
7、.K. Standardization of Tar ProductsTests Committee)3. Summary of Method3.1 Two hundred millilitres of the sample are distilled in a500-mL flask, at a controlled rate, to a temperature in the liquidof 360C (680F), and the volumes of distillate obtained atspecified temperatures are measured. The resid
8、ue from thedistillation, and also the distillate, may be tested as required.4. Significance and Use4.1 This procedure measures the amount of the more vola-tile constituents in cut-back asphaltic products. The propertiesof the residue after distillation are not necessarily characteristicof the bitume
9、n used in the original mixture, nor of the residuewhich may be left at any particular time after field applicationof the cut-back asphaltic product. The presence of silicone inthe cut-back may affect the distillation residue by retarding theloss of volatile material after the residue has been poured
10、 intothe residue container.5. Apparatus5.1 Distillation Flask, 500-mL side-arm, having the dimen-sions shown in Fig. 1.5.2 Condenser, standard glass-jacketed, of nominal jacketlength from 200 to 300 mm and overall tube length of 450 610 mm (see Fig. 3).5.3 Adapter, heavy-wall (1-mm) glass, with rein
11、forced top,having an angle of approximately 105. The inside diameter atthe large end shall be approximately 18 mm, and at the smallend, not less than 5 mm. The lower surface of the adapter shallbe on a smooth descending curve from the larger end to thesmaller. The inside line of the outlet end shall
12、 be vertical, andthe outlet shall be cut or ground (not fire-polished) at an angleof 45 6 5 to the inside line.5.4 Shield, steel, lined with 3-mm fire proof insulation andfitted with transparent mica windows, of the form and dimen-sions shown in Fig. 2, used to protect the flask from air currentsand
13、 to reduce radiation. The cover (top) shall be made in twoparts of 6.4-mm fire proof insulation.5.5 Shield and Flask SupportTwo 15-cm2sheets of 16-mesh Chromel wire gauze on a tripod or ring.1This test method is under the jurisdiction of ASTM Committee D04 on Roadand Paving Materials and is the dire
14、ct responsibility of Subcommittee D04.46 onDurability and Distillation Tests.Current edition approved Dec. 10, 2002. Published February 2003. Originallyapproved in 1934. Last previous edition approved in 1997 as D 402 97.In the IP, this method is under the jurisdiction of the Standardization Committ
15、ee.2Annual Book of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 04.09.4Annual Book of ASTM Standards, Vol 14.03.5Annual Book of ASTM Standards, Vol 14.02.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.6 Heat Sourc
16、e5.6.1 Adjustable Tirrill-type gas burner or equivalent.5.6.2 An electric heater equipped with a transformer ca-pable of controlling from 0 to 750 W. The shield and supportshall be a refractory with an opening of 79 mm, with the uppersurface beveled to 86 mm to accommodate the specified500-mL flask.
17、 When the flask is placed on the refractory, thereshould be a distance of approximately 3 mm between thebottom of the flask and the heating elements.5.7 ReceiverA standard 100-mL graduated cylinder con-forming to dimensions of Specification E 133, or a 100-mLCrow receiver as shown in Fig. 4 of this
18、test method.NOTE 1Receivers of smaller capacity having 0.1-mL divisions maybe used when low volumes of total distillate are expected and the addedaccuracy required.FIG. 1 Distillation FlaskFIG. 2 ShieldD4020225.8 Residue ContainerA seamless metal container withslip on cover of 75 6 5 mm in diameter,
19、 and 55 6 5mminheight.5.9 Thermometer ASTM High Distillation Thermometershaving a range from 6 to 400C (20 to 760F) and conformingto the requirements for Thermometers 8C (8F) as prescribed inSpecification E 1, or IP Thermometer 6C conforming to IPSpecifications for Standard Thermometers, or an equiv
20、alentthermometric device that has been calibrated in accordancewith Test Method E 220. ASTM 8C Thermometers shall beused for referee testing.6. Sampling6.1 Stir the sample thoroughly, warming if necessary, toensure homogeneity before removal of a portion for analysis.6.2 If sufficient water is prese
21、nt to cause foaming orbumping, dehydrate a sample of not less than 250 mL byheating in a distillation flask sufficiently large to preventfoaming over into the side arm. When foaming has ceased, stopthe distillation. If any light oil has distilled over, separate andpour this back into the flask when
22、the contents have cooled justsufficiently to prevent loss of volatile oil. Mix the contents ofthe flask thoroughly before removal for analysis. An alternativeprocedure is described in Test Method D 370.7. Preparation of Apparatus7.1 Calculate the weight of 200 mL of the sample from thespecific gravi
23、ty of the material at 15.6/15.6C. Weigh thisamount 6 0.5 g into the 500-mL flask.7.2 Place the flask in the shield supported by two sheets ofgauze on a tripod or ring. Connect the condenser tube to thetubulature of the flask with a tight cork joint. Clamp thecondenser so that the axis of the bulb of
24、 the flask through thecenter of its neck is vertical. Adjust the adapter over the end ofthe condenser tube so that the distance from the neck of theflask to the outlet of the adapter is 650 6 50 mm (see Fig. 3).7.3 Insert the thermometer through a tightly fitting cork inthe neck of the flask so that
25、 the bulb of the thermometer restson the bottom of the flask. Raise the thermometer 6 mm fromthe bottom of the flask using the scale divisions on thethermometer to estimate the 6 mm distance above the top of thecork.7.4 Protect the burner by a suitable shield or chimney. Placethe receiver so that th
26、e adapter extends at least 25 mm but notbelow the 100-mL mark. Cover the graduate closely with apiece of blotting paper, or similar material, suitably weighted,which has been cut to fit the adapter snugly.7.5 The flask, condenser tube, adapter, and receiver shall beclean and dry before starting the
27、distillation. Place the seamlessresidue container on its cover in an area free from drafts.7.6 Pass cold water through the condenser jacket. Use warmwater if necessary to prevent formation of solid condensate inthe condenser tube.8. Procedure8.1 Correct the temperatures to be observed in the distill
28、a-tion if the elevation of the laboratory at which the distillationis made deviates 150 m or more from sea level. CorrectedFIG. 3 Distillation ApparatusAll dimensions are in millimetresFIG. 4 Crow Receivers of Capacity 25, 50, and 100 mLD402023temperatures for the effect of altitude are shown in Tab
29、le 1 andTable 2. If the prevailing barometric pressure in millimetres ofmercury is known, correct the temperature to be observed withthe corrections shown in Table 3. Do not correct for theemergent stem of the thermometer.NOTE 2Table 3 covers a wide range of temperatures from 160 to360C (320 to 680F
30、) and is to be preferred for world-wide specificationsother than ASTM/IP specifications.8.2 Apply heat so that the first drop of distillate falls fromthe end of the flask side-arm in 5 to 15 min. Conduct thedistillation so as to maintain the following drop rates, the dropcount to be made at the tip
31、of the adapter:50 to 70 drops per minute to 260C (500F)20 to 70 drops per minute between 260 and 316C (500 and 600F)Not over 10 min to complete distillation from 316 to 360C (600 to 680F)8.2.1 Record the volumes of distillate to the nearest 0.5 mLin the receiver at the corrected temperatures. If the
32、 volume ofdistillate recovered is critical, use receivers graduated in0.1-mL divisions and immersed in a transparent bath main-tained at 15.6 6 3C.NOTE 3Some cut-back asphaltic products yield either no distillate orvery little distillate over portions of the temperature range to 316C(600F). In this
33、case it becomes impractical to maintain the abovedistillation rates. For such cases the intent of the method shall be met if therate of rise of temperature exceeds 5C (9F)/min.8.3 When the temperature reaches the corrected temperatureof 360C (680F), cut off the heat and remove the flask andthermomet
34、er. With the flask in a pouring position, remove thethermometer and immediately pour the contents into theresidue container. The total time from cutting off the heat tostarting the pour shall not exceed 30 s. When pouring, theside-arm should be substantially horizontal to prevent conden-sate in the
35、side-arm from being returned to the residue.NOTE 4The formation of skin on the surface of a residue duringcooling entraps vapors which will condense and cause higher penetrationresults when they are stirred back into the sample. If skin begins to formduring cooling, it should be gently pushed aside.
36、 This can be done with aspatula with a minimum of disturbance to the sample.8.4 Allow the condenser and any distillates trapped in thecondenser neck to drain into the receiver and record the totalvolume of distillate collected as total distillate to 360C(680F).8.5 When the residue has cooled until f
37、uming just ceases,stir thoroughly and then, when the material reaches 135 6 5C(275 6 9F), pour into the receptacles for testing for propertiessuch as penetration, viscosity, or softening point. Proceed asrequired by the appropriate ASTM or IP method from the pointthat follows the pouring stage.8.6 I
38、f desired, the distillate, or the combined distillates fromseveral tests, may be submitted to a further distillation, inaccordance with Test Method D 86 IP 123, or, when thedistillate is of coal-tar origin, Method C.O.3.9. Calculation and Report9.1 Asphaltic ResidueCalculate the percent residue to t
39、henearest 0.1 as follows:R 5 200 2 TD!/200# 3 100 (1)where:R = residue content, in volume percent, andTD = total distillate recovered to 360C (680F), mL.TABLE 1 Corrected Distillation Temperatures for VariousAltitudes, CElevation aboveSea Level, mDistillation Temperatures for Various Altitudes, C300
40、 192 227 262 318 362150 191 226 261 317 3610 190 225 260 316 360150 189 224 259 315 359300 189 223 258 314 358450 188 223 257 313 357600 187 222 257 312 356750 186 221 256 311 355900 186 220 255 311 3541050 185 220 254 310 3531200 184 219 254 309 3521350 184 218 253 308 3511500 183 218 252 307 35116
41、50 182 217 251 306 3501800 182 216 250 306 3491950 181 216 250 305 3482100 180 215 249 304 3472250 180 214 248 303 3462400 179 214 248 303 346TABLE 2 Corrected Distillation Temperatures for VariousAltitudes, FElevation abovesea level, m (ft)Distillation Temperatures for Various Altitudes, F300 377 4
42、40 503 604 684150 375 438 502 602 6820 374 437 500 600 680150 373 436 499 598 678300 371 434 497 597 676450 370 433 495 595 675600 369 431 494 593 673750 368 430 493 592 671900 366 429 491 590 6691050 365 427 490 589 6681200 364 426 488 587 6661350 363 425 487 586 6651500 362 424 486 584 6631650 360
43、 422 484 583 6611800 359 421 483 581 6601950 358 420 482 580 6582100 357 419 481 579 6572250 356 418 479 577 6552400 355 416 478 576 654TABLE 3 Factors for Calculating Temperature CorrectionsNominal Temperatures,C (F)CorrectionAper 10 mm HgDifference in Pressure,C (F)160 (320) 0.514 (0.925)175 (347)
44、 0.531 (0.957)190 (374) 0.549 (0.989)225 (437) 0.591 (1.063)250 (482) 0.620 (1.116)260 (500) 0.632 (1.138)275 (527) 0.650 (1.170)300 (572) 0.680 (1.223)315.6 (600) 0.698 (1.257)325 (617) 0.709 (1.277)360 (680) 0.751 (1.351)ATo be subtracted in case the barometric pressure is below 760 mm Hg; to bead
45、ded in case barometric pressure is above 760 mm Hg.D4020249.1.1 Report as the residue from distillation to 360 (680F),percent volume by difference.9.2 Total Distillate Calculate the percent total distillate tothe nearest 0.1 as follows:TD % 5 TD/200! 3 100 (2)9.2.1 Report as the total distillate to
46、360C (680F), volumepercent.9.3 Distillate Fractions:9.3.1 Determine the percentages by volume of the originalsample by dividing the observed volume (in millilitres) of thefraction by 2. Report to the nearest 0.1 as volume percent asfollows:Up to 190C (374F)Up to 225C (437F)Up to 260C (500F)Up to 316
47、C (600F)9.3.2 Determine the percentages by volume of total distil-late by dividing the observed volume in millilitres of thefraction by the millilitres recovered to 360C (680F) andmultiplying by 100. Report to the nearest 0.1 as the distillate,volume percent of total distillate to 360C (680F) as fol
48、lows:Up to 190C (374F)Up to 225C (437F)Up to 260C (500F)Up to 316C (600F)9.4 Where penetration, viscosity, or other tests have beencarried out, report with reference to this test method as well asto any other method used. ExamplePenetration (ASTM D5or IP 49) of residue from ASTM D402/IP 27.10. Preci
49、sion and Bias10.1 The following criteria shall be used for judging theacceptability of results (95 % probability):10.1.1 Repeatability Duplicate values by the same opera-tor shall not be considered suspect unless the determinedpercentages differ by more than 1.0 volume % of the originalsample.10.1.2 Reproducibility The values reported by each oftwo laboratories, shall not be considered suspect unless thereported percentages differ by more than the following:Distillation Fractions, volume percent of the
