ASTM D402-2008 Standard Test Method for Distillation of Cutback Asphaltic (Bituminous) Products《稀释沥青产品蒸馏的标准试验方法》.pdf

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1、Designation: D 402 0827/74 (88)American Association StateHighway and Transportation Officials StandardAASHTO No.: T78Standard Test Method forDistillation of Cutback Asphaltic (Bituminous) Products1This standard is issued under the fixed designation D 402; the number immediately following the designa

2、tion 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 () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by ag

3、encies 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 cutbackasphaltic (bituminous) products.1.2 The values given in SI units are to be regarded as thestandard. The inch-pound units given in parenth

4、eses 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 limitations

5、 prior to use.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD 370 Practice for Dehydration of Oil-Type PreservativesE1 Specification for ASTM Liquid-in-Glass ThermometersE 133 Specification for Distillation EquipmentE 220 Test

6、 Method for Calibration of Thermocouples ByComparison Techniques2.2 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 th

7、e U.K. Standardization of Tar ProductsTests Committee)3. Summary of Method3.1 Two hundred millilitres of the sample are distilled in a500-mLflask, at a controlled rate, to a temperature in the liquidof 360C (680F), and the volumes of distillate obtained atspecified temperatures are measured. The res

8、idue 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 cutback asphaltic products. The propertiesof the residue after distillation are not necessarily characteristicof the bitum

9、en used in the original mixture, nor of the residuewhich may be left at any particular time after field applicationof the cutback asphaltic product.The presence of silicone in thecutback may affect the distillation residue by retarding the lossof volatile material after the residue has been poured i

10、nto theresidue 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 reinfo

11、rced 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 b

12、e vertical, andthe outlet shall be cut or ground (not fire-polished) at an angleof 45 6 5 to the inside line.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.Curre

13、nt edition approved July 15, 2008. Published August 2008. Originallyapproved in 1934. Last previous edition approved in 2002 as D 402 02.In the IP, this method is under the jurisdiction of the Standardization Committee.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact A

14、STM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.4 Shield, steel, lined wi

15、th 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 and Flask SupportTwo 15-cm2shee

16、ts of 16-mesh Chromel wire gauze on a tripod or ring.5.6 Heat Source5.6.1 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 uppe

17、rsurface 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 between thebottom of the flask and the heating elements.FIG. 1 Distillation FlaskFIG. 2 ShieldD4020825.7 ReceiverA standard 100-mL graduated

18、 cylinder con-forming to dimensions of Specification E 133, or a 100-mLCrow receiver as shown in Fig. 4 of this 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.5.8 Residue ContainerA s

19、eamless metal container withslip on cover of 75 6 5 mm in diameter, and 55 6 5mminheight.5.9 Thermometric Device ASTM High Distillation Ther-mometers having a range from 6 to 400C (20 to 760F) andconforming to the requirements for Thermometers 8C (8F) asprescribed in Specification E1, or IP Thermome

20、ter 6C con-forming to IP Specifications for Standard Thermometers, or anequivalent thermometric device that has been calibrated inaccordance with Test Method E 220. ASTM 8C Thermometersshall be used for referee testing.6. Hazards6.1 WarningMercury has been designated by the UnitedStates Environmenta

21、l ProtectionAgency (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 handling mercury and mercury containingproducts. See the app

22、licable 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 prohibitedby state law.7. Sampling7.1 Stir the sample thor

23、oughly, 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 large to preventfoaming over into the side arm. When fo

24、aming 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 removal for analysis.An alternativeprocedure is descri

25、bed in Test Method D 370.8. 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 two sheets ofgauze on a tripod or ring. Connect th

26、e 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 dimensions are in millimetresFIG. 4 Crow Receivers of Capa

27、city 25, 50, and 100 mLD402083the 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 flask so that the bulb of the thermo-metric device rests on the

28、 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 burner by a suitable shield or chimney. Placethe receiver s

29、o 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 tube, adapter, and receiver shall beclean and dry before star

30、ting 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. Procedure9.1 Correct the temperatures to be observed in th

31、e 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 pressure in millimetres ofmercury is known, correct the temperatur

32、e 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 specificationsother than ASTM/IP specifications.9.2 Apply heat

33、 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 (500F)20 to 70 drops per minute between 260 and 316C

34、(500 and 600F)Not over 10 min to complete distillation from 316 to 360C (600 to 680F)9.2.1 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 receivers graduated in0.1-mL divisions and immersed in

35、 a transparent bath main-tained at 15.6 6 3C.NOTE 3Some cutback asphaltic products yield either no distillate orvery little distillate over portions of the temperature range to 316C(600F). In this case it becomes impractical to maintain the abovedistillation rates. For such cases the intent of the m

36、ethod 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, remove the thermometric device and immedia

37、telypour 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 residue.NOTE 4The formation of skin on the

38、 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 359300 189 223 258 314 358450 188 223 257

39、 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 180 215 249 304 3472250 180 214 248 303 3462400 17

40、9 214 248 303 346TABLE 2 Corrected Distillation Temperatures for VariousAltitudes, FElevation abovesea level, m (ft)Distillation 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 371 434 497 597 676450 370 433 495 595 6

41、75600 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 6572250 356 418 479 577 6552400 355 416

42、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) 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.

43、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 beadded in case barometric pressure is above 760 mm Hg.D402084cooling entraps vapors which will condense and cause higher penetra

44、tionresults 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 receiv

45、er and record the totalvolume of distillate collected as total distillate to 360C(680F).9.5 When the residue has cooled until fuming 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,

46、 or softening point. Proceed asrequired by the appropriateASTM or IP method from the pointthat follows 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 IP 123, or, when thedi

47、stillate is of coal-tar origin, Method C.O.3.10. Calculation and Report10.1 Asphaltic ResidueCalculate the percent residue tothe nearest 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.10.1.1 Report as the

48、residue from distillation to 360(680F), percent volume by difference.10.2 Total Distillate Calculate the percent total distillateto the nearest 0.1 as follows:TD % 5 TD/200! 3 100 (2)10.2.1 Report as the total distillate to 360C (680F),volume percent.10.3 Distillate Fractions:10.3.1 Determine the pe

49、rcentages 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 316C (600F)10.3.2 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 360