1、Designation: D402/D402M 14 American Association StateHighway and Transportation Officials StandardAASHTO No.: T7827/74 (88)Standard Test Method forDistillation of Cutback Asphalt1This standard is issued under the fixed designation D402/D402M; the number immediately following the designation indicate
2、s the yearof original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.A superscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a distillation test fo
3、r cutbackasphalts.1.2 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard. The values stated ineach system may not be exact equivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems may result in no
4、n-conformancewith the standard.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 limitatio
5、ns prior to use.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD370 Practice for Dehydration of Oil-Type PreservativesE1 Specification for ASTM Liquid-in-Glass ThermometersE77 Test Method for Inspection and Verification of Ther
6、-mometersE133 Specification for Distillation EquipmentE220 Test Method for Calibration of Thermocouples ByComparison TechniquesE644 Test Methods for Testing Industrial Resistance Ther-mometersE1137 Specification for Industrial Platinum Resistance Ther-mometers3. Summary of Method3.1 Two hundred mill
7、ilitres 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 residue from thedistillation, and also the distillate, may be tested as required.4. Significance a
8、nd Use4.1 This procedure measures the amount of the more vola-tile constituents in cutback asphalt. The properties of theresidue after distillation are not necessarily characteristic of thebitumen used in the original mixture, nor of the residue whichmay be left at any particular time after field ap
9、plication of thecutback asphalt. The presence of silicone in the cutback asphaltmay affect the distillation residue by retarding the loss ofvolatile material after the residue has been poured into theresidue container.5. Apparatus5.1 Distillation Flask, 500-mL side-arm, having the dimen-sions shown
10、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 reinforced top,having an angle of approximately 105. The inside diameter atthe large end shall be approximately 1
11、8 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 be vertical, andthe outlet shall be cut or ground (not fire-polished) at an angleof 45 6 5 to the inside lin
12、e.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 to reduce radiation. The cover (top) shall be made in twoparts of 6.4-mm fire proof insulation.5.5 Shield an
13、d 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 direct responsibility of Subcommittee D04.46 onDurability and Distillation Tests.Current edition approved June 1,
14、 2014. Published August 2014. Originallyapproved in 1934. Last previous edition approved in 2008 as D402 08. DOI:10.1520/D0402_D0402M-14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume i
15、nformation, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.6 Heat Source:5.6.1 Adjustable Tirrill-type gas burner or equivalent.5.6.2 An electric heater equipped with
16、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. When the flask is placed on the refractory, thereshould be a distance of approximately 3 mm be
17、tween thebottom of the flask and the heating elements.5.7 ReceiverA standard 100-mL graduated cylinder con-forming to dimensions of Specification E133, or a 100-mLCrow receiver as shown in Fig. 4 of this test method.NOTE 1Receivers of smaller capacity having 0.1-mLdivisions may beused when low volum
18、es of total distillate are expected and the addedaccuracy required.5.8 Residue ContainerA seamless metal container withslip on cover of 75 6 5 mm in diameter, and 55 6 5mminheight.FIG. 1 Distillation FlaskFIG. 2 ShieldD402/D402M 1425.9 ThermometerThe thermometer shall be one of thefollowing:5.9.1 An
19、 8C (8F) thermometer which conforms to therequirements of Specification E1. Calibrate the thermometer inaccordance with one of the methods in Test Method E77.5.9.2 Aplatinum resistance thermometer (PRT) with a probewhich conforms to the requirements of Specification E1137.The PRT shall have a 3- or
20、4-wire connection configuration andthe overall sheath length shall be at least 50 mm 2 in. greaterthan the immersion depth. Calibrate the PRT system (probe andreadout) in accordance with Test Methods E644. Correctionsshall be applied to ensure accurate measurements within 1C2F.5.9.3 A metal-sheathed
21、 Type T thermocouple with a sensorsubstantially-similar in construction to the PRT probe de-scribed in 5.9.2. Calibrate the thermocouple system (sensor andreadout) in accordance with Test Method E220. Correctionsshall be applied to ensure accurate measurements within 1C2F.6. Hazards6.1 WarningMercur
22、y has been designated by the UnitedStates Environmental Protection Agency (EPA) and many stateagencies as a hazardous material that can cause central nervoussystem, kidney and liver damage. Mercury, or its vapor, may behazardous to health and corrosive to materials. Caution shouldbe taken when handl
23、ing mercury and mercury containingproducts. See the applicable product Material Safety DataSheet (MSDS) for details and EPAs websitehttp:/www.epa.gov/mercury/faq.htmfor additional information.Users should be aware that selling mercury, mercury-containing products, or both, into your state may be pro
24、hibitedby state law.7. Sampling7.1 Stir the sample thoroughly, warming if necessary, toensure homogeneity before removal of a portion for analysis.7.2 If sufficient water is present to cause foaming orbumping, dehydrate a sample of not less than 250 mL byheating in a distillation flask sufficiently
25、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 the contents have cooled justsufficiently to prevent loss of volatile oil. Mix the contents ofthe flask thoroughly before
26、 removal for analysis.An alternativeprocedure is described in Practice D370.8. Preparation of Apparatus8.1 Calculate the weight of 200 mL of the sample from thespecific gravity of the material at 15.6/15.6C. Weigh thisamount 60.5 g into the 500-mL flask.8.2 Place the flask in the shield supported by
27、 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 the flask through thecenter of its neck is vertical. Adjust the adapter over the end ofFIG. 3 Distillation ApparatusAll dimens
28、ions are in millimetresFIG. 4 Crow Receivers of Capacity 25, 50, and 100 mLD402/D402M 143the 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).8.3 Insert the thermometric device through a tightly fittingcork in the neck of the flas
29、k so that the bulb of the thermo-metric device rests on the bottom of the flask. Raise thethermometric device approximately 6 mm from the bottom ofthe flask using the scale divisions or a reference mark on thethermometric device to estimate the 6 mm distance above thetop of the cork.8.4 Protect the
30、burner by a suitable shield or chimney. Placethe receiver so that the 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.8.5 The flask, condenser tu
31、be, adapter, and receiver shall beclean and dry before starting the distillation. Place the seamlessresidue container on its cover in an area free from drafts.8.6 Pass cold water through the condenser jacket. Use warmwater if necessary to prevent formation of solid condensate inthe condenser tube.9.
32、 Procedure9.1 Correct the temperatures to be observed in the distilla-tion if the elevation of the laboratory at which the distillationis made deviates 150 m or more from sea level. Correctedtemperatures for the effect of altitude are shown in Table 1 andTable 2. If the prevailing barometric pressur
33、e 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 (if used).NOTE 2Table 3 covers a wide range of temperatures from 160 to360C 320 to 680F and is to be preferred for world-wide speci
34、ficationsother than ASTM specifications.9.2 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 of the adapter:50 to 70 drops per minute to 260C
35、 500F20 to 70 drops per minute between 260 and 316C 500 and 600FNot over 10 min to complete distillation from 316 to 360C 600 to 680F9.2.1 Record the volumes of distillate to the nearest 0.5 mLin the receiver at the corrected temperatures. If the volume ofdistillate recovered is critical, use receiv
36、ers graduated in0.1-mL divisions and immersed in a transparent bath main-tained at 15.6 6 3C.NOTE 3Some cutback asphalt products yield either no distillate orvery little distillate over portions of the temperature range to 316C600F. In this case it becomes impractical to maintain the abovedistillati
37、on rates. For such cases the intent of the method shall be met if therate of rise of temperature exceeds 5C 9F/min.9.3 When the temperature reaches the corrected temperatureof 360C 680F, turn off the heat and remove the flaskcontaining the thermometric device. With the flask in a pouringposition, re
38、move the thermometric device and immediatelypour the contents into the residue container. The total timefrom turning off the heat to starting the pour shall not exceed60 s. When pouring, the side-arm should be substantiallyhorizontal to prevent condensate in the side-arm from beingreturned to the re
39、sidue.NOTE 4The formation of skin on the surface of a residue duringTABLE 1 Corrected Distillation Temperatures for VariousAltitudes, CElevation aboveSea Level, mDistillation Temperatures for Various Altitudes, C300 192 227 262 318 362150 191 226 261 317 3610 190 225 260 316 360150 189 224 259 315 3
40、59300 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 3511650 182 217 251 306 3501800 182 216 250 306 3491950 181 216 250 305 3482100 180 215 24
41、9 304 3472250 180 214 248 303 3462400 179 214 248 303 346TABLE 2 Corrected Distillation Temperatures for VariousAltitudes, FElevation abovesea level, m ftDistillation Temperatures for Various Altitudes, F300 377 440 503 604 684150 375 438 502 602 6820 374 437 500 600 680150 373 436 499 598 678300 37
42、1 434 497 597 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 360 422 484 583 6611800 359 421 483 581 6601950 358 420 482 580 6582100 357 419 481 579 65
43、72250 356 418 479 577 6552400 355 416 478 576 654TABLE 3 Factors for Calculating Temperature CorrectionsNominal Temperatures,C FCorrectionAper 10 mm HgDifference in Pressure,C F160 320 0.514 0.925175 347 0.531 0.957190 374 0.549 0.989225 437 0.591 1.063250 482 0.620 1.116260 500 0.632 1.138275 527 0
44、.650 1.170300 572 0.680 1.223315.6 600 0.698 1.257325 617 0.709 1.277360 680 0.751 1.351ATo be subtracted in case the barometric pressure is below 760 mm Hg; to beadded in case barometric pressure is above 760 mm Hg.D402/D402M 144cooling entraps vapors which will condense and cause higher penetratio
45、nresults when they are stirred back into the sample. If skin begins to formduring cooling, it should be gently pushed aside. This can be done with aspatula with a minimum of disturbance to the sample.9.4 Allow the condenser and any distillates trapped in thecondenser neck to drain into the receiver
46、and record the totalvolume of distillate collected as total distillate to 360C680F.9.5 When the residue has cooled until fuming just ceases,stir thoroughly and then, when the material reaches 135 6 5C275 6 9F, pour into the receptacles for testing for propertiessuch as penetration, viscosity, or sof
47、tening point. Proceed asrequired by the appropriate ASTM method from the point thatfollows the pouring stage.9.6 If desired, the distillate, or the combined distillates fromseveral tests, may be submitted to a further distillation, inaccordance with Test Method D86.10. Calculation and Report10.1 Asp
48、halt ResidueCalculate the percent residue to thenearest 0.1 as follows:R 5 200 2 TD!/200# 3100 (1)where:R = residue content, in volume percent, andTD = total distillate recovered to 360C 680F, mL.10.1.1 Report as the residue from distillation to 360680F, percent volume by difference.10.2 Total Disti
49、llate Calculate the percent total distillateto the nearest 0.1 as follows:TD% 5 TD/200! 3100 (2)10.2.1 Report as the total distillate to 360C 680F,volume percent.10.3 Distillate Fractions:10.3.1 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 374FUp to 225C 437FUp to 260C 500FUp to
