1、Designation: D5404/D5404M 12 (Reapproved 2017)Standard Practice forRecovery of Asphalt from Solution Using the RotaryEvaporator1This standard is issued under the fixed designation D5404/D5404M; the number immediately following the designation indicates theyear of original adoption or, in the case of
2、 revision, the year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice is intended to recover asphalt from asolvent using the rotary evaporator to ensur
3、e that changes inthe asphalt properties during the recovery process are mini-mized.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
4、 the other. Combiningvalues from the two systems may result in nonconformancewith the standard.1.2.1 Residual pressure measurements are shown in both theSI unit of kPa and the commonly used non-standard equivalentunit of “mm of Hg.”1.2.2 Measurements of volume and mass are only given inSI units beca
5、use they are the only units typically used inpractice when performing this standard practice.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, health, and en
6、vironmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Stan
7、dards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D92 Test Method for Flash and Fire Points by ClevelandOpen Cup TesterD1856 Test Method for Recovery of Asphalt From Solutionby Abson MethodD
8、2939 Test Methods for Emulsified Bitumens Used asProtective Coatings (Withdrawn 2012)3D3666 Specification for Minimum Requirements for Agen-cies Testing and Inspecting Road and Paving MaterialsD6368 Specification for Vapor-Degreasing Solvents Basedon normal-Propyl Bromide and Technical Grade normal-
9、Propyl Bromide3. Summary of Practice3.1 The solution of solvent and asphalt from a prior extrac-tion is distilled by partially immersing the rotating distillationflask of the rotary evaporator in a heated oil bath while thesolution is subjected to a partial vacuum and a flow of nitrogengas or carbon
10、 dioxide gas. The recovered asphalt can then besubjected to testing as required.4. Significance and Use4.1 In order to determine the characteristics of the asphalt inan asphalt paving mixture, it is necessary to extract the asphaltfrom the aggregate by means of a suitable solvent and then torecover
11、the asphalt from the solvent without significantlychanging the asphalts properties. The asphalt recovered fromthe solvent by this practice can be tested using the samemethods as for the original asphalt cement, and comparisonsbetween the properties of the original and recovered asphaltcan be made.NO
12、TE 1The quality of the results produced by this standard aredependent on the competence of the personnel performing the procedureand the capability, calibration, and maintenance of the equipment used.Agencies that meet the criteria of Specification D3666 are generallyconsidered capable of competent
13、and objective testing, sampling,inspection, etc. Users of this standard are cautioned that compliance withSpecification D3666 alone does not completely ensure reliable results.Reliable results depend on many factors; following the suggestions ofSpecification D3666 or some similar acceptable guidelin
14、e provides ameans of evaluating and controlling some of those factors.5. Apparatus5.1 Rotary Evaporator (see Fig. 1), equipped with a distil-lation flask, a variable speed motor capable of rotating the1This practice is under the jurisdiction of ASTM Committee D04 on Road andPaving Materials and is t
15、he direct responsibility of Subcommittee D04.25 onAnalysis of Asphalt Mixtures.Current edition approved Oct. 1, 2017. Published October 2017. Originallyapproved in 1993. Last previous edition approved in 2012 as D5404/D5404M 12.DOI: 10.1520/D5404_D5404M-12R17.2For referenced ASTM standards, visit th
16、e ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM In
17、ternational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standard
18、s, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1distillation flask at a rate of at least 50 rpm, condenser, solventrecovery flask, and heated oil bath. The angle of the distillationflask from the horizontal to the bath is set at appro
19、ximately 15.The distillation flask (Note 2), when fully immersed, should beat a depth of approximately 40 mm 1.5 in.NOTE 2A flask having a 2000-mL capacity is recommended.5.1.1 Thermometric DeviceA built-in temperature mea-surement device capable of displaying the oil temperatures tothe nearest 1 C
20、2 F.5.2 Manometer or Vacuum Gage, suitable for measuring thespecified vacuum.5.3 Gas Flowmeter, capable of indicating a gas flow of up to1000 mL/min.5.4 Sample Container, having adequate volume to hold thesample and added solvent.5.5 Vacuum System, capable of maintaining a vacuum towithin 60.7 kPa 6
21、5 mm of Hg of the desired level up to andincluding 80 kPa 600 mm of Hg.5.6 Oven, capable of maintain a temperature of 165 6 5C329 6 10 F.6. Reagents and Materials6.1 Nitrogen Gas or Carbon Dioxide GasA pressurizedtank with pressure-reducing valve, or other convenient source.NOTE 3Different flow rate
22、s may be required depending on whethernitrogen gas or carbon dioxide gas is used.6.2 OilThe oil for the heated oil bath should be USPWhite Oil or Silicone Fluid SWS-101 with flash point above215 C 420 F or an equivalent. The flash point is determinedin accordance with Test Method D92.6.3 Solvents:6.
23、3.1 Trichloroethylene and Methylene ChlorideThe sol-vent for extracting the asphalt from mixtures should bereagent-grade trichloroethylene or methylene chloride. A tech-nical grade of trichloroethylene may be used, but it is recom-mended that for each new supply of solvent, a blank should berun on a
24、n asphalt with known properties.6.3.2 Normal Propyl Bromides (nPB)The solvent forextracting the asphalt from the mixtures should conform toSpecification D6368. Because there may be some interactionsdue to differences in nPB products, it is recommended that fora new supply of solvent, a blank should
25、be run on an asphaltwith known properties.7. Precautions7.1 CautionThe solvents listed in 6.3 should be used onlyunder a hood or with an effective surface exhaust system in awell-ventilated area, since they are toxic to various degrees.Consult the current Threshold Limit Concentration Committeeof th
26、e American Conference of Governmental Industrial Hy-gienists4for the current threshold limit values.7.2 These solvents in the presence of heat and moisture maybe hydrolyzed to form acids that are extremely corrosive tocertain metals, particularly when subject to contact overlengthy periods of time.
27、Proper precautions should be taken tonot allow these solvents to remain in small quantities in theeffluent tanks of aluminum vacuum extractors.7.3 Exposure of these solvents or their vapors to hightemperatures such as contact with flames, hot glowing surfaces,or electric arcs can produce decompositi
28、on products such ashydrogen chloride. Steel drums containing these solventsshould be stored in a cool, dry location, kept tightly sealed, andopened as infrequently as possible. The hydrogen chloride indecomposed solvent may harden an asphalt during the extrac-tion and recovery test.4Available from A
29、merican Conference of Governmental Industrial Hygienists,1330 Kemper Meadow Drive, Cincinnati, OH 45240, (513) 7422020, (www.acgi-h.org).NOTE 1It is important that the needle valve is located as shown instead of being placed ahead of the flowmeter.FIG. 1 Rotary Evaporator and Recovery SystemD5404/D5
30、404M 12 (2017)28. Sample Preparation8.1 The sample shall be obtained and handled in accordancewith Test Method D1856. This includes the procedure forcentrifuging the solution from a previous extraction.9. Procedure9.1 Heat the oil bath to a temperature of 140 6 3 C 285 65 F. Circulate cold water thr
31、ough the condenser.9.2 Apply a vacuum of 5.3 6 0.7 kPa 40 6 5mmofHgbelow atmospheric pressure and draw approximately 600 mLof asphalt solution from the sample container into the distilla-tion flask by way of the sample line. Begin a nitrogen or carbondioxide flow of approximately 500 mL/min through
32、the system(Note 4). Begin rotating the distillation flask (at approximately40 rpm) and lower the flask into the oil bath. Initially theimmersion depth of the flask will be determined by the need toachieve a controlled solvent evaporation rate. The correct rateof evaporation can be observed as a stea
33、dy controlled stream ofcondensed solvent being collected in the recovery flask.NOTE 4The vacuum and nitrogen or carbon dioxide flow values mayneed to be adjusted depending on the location. Also, low flow values arerecommended at the beginning of the rotary process when the samplevolume is large beca
34、use of the possibility of backflow into the vacuumsystem. The possibility of backflow can also be minimized by regulatingthe depth of immersion of the flask.9.3 When the amount of asphalt solution within the distil-lation flask appears low enough so that more solution may beadded, discontinue the ni
35、trogen or carbon dioxide flow. Drawthe remaining asphalt solution from the sample container intothe distillation flask and readjust the nitrogen or carbon dioxideflow (Note 5).NOTE 5The equipment may be modified to allow a continuous flow ofsolution from the sample container into the distillation fl
36、ask such that thevolume in the distillation flask is maintained at approximately 600 mL.The nitrogen or carbon dioxide flow is not started until all the solution hasentered the distillation flask.9.4 When the bulk of the solvent has been distilled from theasphalt and no obvious condensation is occur
37、ring on thecondenser, immerse the flask to the recommended maximumimmersion depth of approximately 40 mm 1.5 in. Slowlyapply a vacuum of 80.0 6 0.7 kPa 600 6 5 mm of Hg belowatmospheric pressure. Increase nitrogen or carbon dioxide flowto approximately 600 mL/min and the spin rate of the distilla-ti
38、on flask to about 45 rpm (Note 6). Hold or reduce vacuum iffoaming or a bubbly formation occurs. When foamingsubsides, apply maximum vacuum. Maintain this condition for10 6 1 min.NOTE 6It is recommended that the flask be immersed for up to 2 minbefore slowly applying the vacuum.NOTE 7A faster flask
39、spin rate exposes more surface area of theasphalt and, hence, dislodges more traces of solvent from the asphalt. Therotation speed of the flask may also be varied or the flask rotation may bestopped to enhance the removal of solvent.NOTE 8Due to the cooling effect of the increased nitrogen or carbon
40、dioxide flow, an increase in the temperature of the oil bath is generallyneeded to maintain a constant sample temperature. Experience has shownthat a typical oil bath temperature range of 150 to 155 C 300 to 310 Fis satisfactory for this purpose.9.5 At the end of the 10-min period, remove the distil
41、lationflask from the apparatus and wipe the flask clean of oil. Pourthe asphalt into a proper size container. If needed, the flask maybe inverted and placed into an oven at 165 6 5 C 329 610 F for 10 to 15 min to cause the asphalt to flow into thecontainer. The asphalt should not be allowed to be di
42、stributedover the interior of the flask.9.6 Portions of the recovered asphalt, while still in a liquidstate, can be taken for penetration, softening point, ductility,and kinematic and absolute viscosity determinations as re-quired. If ash content determinations are to be conducted, theyshall be dete
43、rmined in accordance with Test Methods D2939and reported with other test data on the recovered asphalt.NOTE 9Ash contents of recovered asphalts greater than 1 % mayaffect the accuracy of the penetration, ductility, softening point, orviscosity tests.NOTE 10Results reported by the AASHTO Materials Re
44、ferenceLaboratory for proficiency samples from 1992 to 1996 indicate that thebetween-laboratory precision (1S%) ranges from 16 to 30 % for penetra-tion of recovered asphalt, 10 to 22 % for kinematic viscosity (135 C275 F), and 16 to 45 % for viscosity at 60 C 140 F. These ranges aresignificantly lar
45、ger than reported for testing original asphalts.10. Keywords10.1 bituminous paving mixtures; recovery; rotary evapora-torASTM 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 expres
46、sly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are 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,
47、 either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may at
48、tend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee 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.
49、 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 12 (2017)3
