1、Designation: D5404/D5404M 11D5404/D5404M 12Standard 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 re
2、vision, 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 a solvent using the rotary evaporator to ensure
3、that changes in the asphaltproperties during the recovery process are minimized.1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in eachsystem may not be exact equivalents; therefore, each system shall be used independently of
4、the other. Combining values from thetwo systems may result in non-conformance with the standard.1.2.1 Residual pressure measurements are shown in both the SI 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 in SI units b
5、ecause they are the only units typically used in practicewhen performing this standard practice.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health p
6、ractices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D92 Test Method for Flash and Fire Points by Cleveland Open Cup TesterD1856 Test Method for Recovery of Asphalt From Solution by Abson MethodD2939 Test Methods for Emulsified Bit
7、umens Used as Protective Coatings (Withdrawn 2012)3D3666 Specification for Minimum Requirements for Agencies Testing and Inspecting Road and Paving MaterialsD6368 Specification for Vapor-Degreasing Solvents Based on normal-Propyl Bromide and Technical Grade normal-PropylBromide3. Summary of Practice
8、3.1 The solution of solvent and asphalt from a prior extraction is distilled by partially immersing the rotating distillation flaskof the rotary evaporator in a heated oil bath while the solution is subjected to a partial vacuum and a flow of nitrogen gas or carbondioxide gas. The recovered asphalt
9、can then be subjected to testing as required.4. Significance and Use4.1 In order to determine the characteristics of the asphalt in an asphalt paving mixture, it is necessary to extract the asphaltfrom the aggregate by means of a suitable solvent and then to recover the asphalt from the solvent with
10、out significantly changingthe asphalts properties. The asphalt recovered from the solvent by this practice can be tested using the same methods as for theoriginal asphalt cement, and comparisons between the properties of the original and recovered asphalt can be made.NOTE 1The quality of the results
11、 produced by this standard are dependent on the competence of the personnel performing the procedure and thecapability, calibration, and maintenance of the equipment used. Agencies that meet the criteria of Standard Practice D3666 are generally considered1 This practice is under the jurisdiction of
12、ASTM Committee D04 on Road and Paving Materials and is the direct responsibility of Subcommittee D04.25 on Analysis ofBituminous Mixtures.Current edition approved Jan. 1, 2011June 1, 2012. Published March 2011May 2013. Originally approved in 1997. Last previous edition approved in 20032011 asD5404D5
13、404/D5404M 03.11. DOI: 10.1520/D5404_D5404M-11.10.1520/D5404_D5404M-12.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the AST
14、M website.3 The last approved version of this historical standard is referenced on www.astm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically po
15、ssible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700,
16、West Conshohocken, PA 19428-2959. United States1capable of competent and objective testing/sampling/inspection/etc. Users of this standard are cautioned that compliance with Practice D3666 alone doesnot completely assure reliable results. Reliable results depend on many factors; following the sugges
17、tions of Practice D3666 or some similar acceptableguideline provides a means of evaluating and controlling some of those factors.5. Apparatus5.1 Rotary Evaporator (see Fig. 1), equipped with a distillation flask, a variable speed motor capable of rotating the distillationflask at a rate of at least
18、50 rpm, condenser, solvent recovery flask, and heated oil bath. The angle of the distillation flask from thehorizontal to the bath is set at approximately 15. The distillation flask (Note 2), when fully immersed, should be at a depth ofapproximately 40 mm 1.5 in.NOTE 2A flask having a 2000 mL capaci
19、ty is recommended.5.1.1 Thermometric DeviceA built-in temperature measurement device capable of displaying the oil temperatures to thenearest 1C 2F.5.2 Manometer or Vacuum Gage, suitable for measuring the specified vacuum.5.3 Gas Flowmeter, capable of indicating a gas flow of up to 1000 mL/min.5.4 S
20、ample Container, having adequate volume to hold the sample and added solvent.5.5 Vacuum System, capable of maintaining a vacuum to within 60.7 kPa 65 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 5C 329 6 10F.6. Reagents and
21、 Materials6.1 Nitrogen Gas or Carbon Dioxide GasA pressurized tank with pressure-reducing valve, or other convenient source.NOTE 3Different flow rates may be required depending on whether nitrogen gas or carbon dioxide gas is used.6.2 OilThe oil for the heated oil bath should be USP White Oil or Sil
22、icone Fluid SWS-101 with flash point above 215C420F or an equivalent. The flash point is determined in accordance with Test Method D92.6.3 Solvents:6.3.1 Trichloroethylene and Methylene ChlorideThe solvent for extracting the asphalt from mixtures should be reagent gradetrichloroethylene or methylene
23、 chloride. A technical grade of trichloroethylene may be used, but it is recommended that for eachnew supply of solvent, a blank should be run on an asphalt with known properties.6.3.2 Normal Propyl Bromides (nPB)The solvent for extracting the asphalt from the mixtures should conform to Specificatio
24、nD6368. Because there may be some interactions due to differences in nPB products, it is recommended that for a new supply ofsolvent, a blank should be run on an asphalt with known properties.NOTE 1It is important that the needle valve is located as shown instead of being placed ahead of the flowmet
25、er.FIG. 1 Rotary Evaporator and Recovery SystemD5404/D5404M 1227. Precautions7.1 CautionThe solvents listed in 6.3 should be used only under a hood or with an effective surface exhaust system in a wellventilated area, since they are toxic to various degrees. Consult the current Threshold Limit Conce
26、ntration Committee of theAmerican Conference of Governmental Industrial Hygienists4 for the current threshold limit values.7.2 These solvents in the presence of heat and moisture may be hydrolyzed to form acids that are extremely corrosive to certainmetals, particularly when subject to contact over
27、lengthy periods of time. Proper precautions should be taken to not allow thesesolvents to remain in small quantities in the effluent tanks of aluminum vacuum extractors.7.3 Exposure of these solvents or their vapors to high temperatures such as contact with flames, hot glowing surfaces, or electrica
28、rcs can produce decomposition products such as hydrogen chloride. Steel drums containing these solvents should be stored in acool, dry location, kept tightly sealed, and opened as infrequently as possible. The hydrogen chloride in decomposed solvent mayharden an asphalt during the extraction and rec
29、overy test.8. Sample Preparation8.1 The sample shall be obtained and handled in accordance with 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 3C 285 6 5F. Circulate cold water through
30、 the condenser.9.2 Apply a vacuum of 5.3 6 0.7 kPa 40 6 5 mm of Hg below atmospheric pressure and draw approximately 600 mL ofasphalt solution from the sample container into the distillation flask by way of the sample line. Begin a nitrogen or carbon dioxideflow of approximately 500 mL/min through t
31、he system (Note 4). Begin rotating the distillation flask (at approximately 40 rpm)and lower the flask into the oil bath. Initially the immersion depth of the flask will be determined by the need to achieve a controlledsolvent evaporation rate. The correct rate of evaporation can be observed as a st
32、eady controlled stream of condensed solvent beingcollected in the recovery flask.NOTE 4The vacuum and nitrogen or carbon dioxide flow values may need to be adjusted depending on the location. Also, low flow values arerecommended at the beginning of the rotary process when the sample volume is large
33、because of the possibility of back flow into the vacuum system.The possibility of back flow can also be minimized by regulating the depth of immersion of the flask.9.3 When the amount of asphalt solution within the distillation flask appears low enough so that more solution may be added,discontinue
34、the nitrogen or carbon dioxide flow. Draw the remaining asphalt solution from the sample container into the distillationflask and readjust the nitrogen or carbon dioxide flow (Note 5).NOTE 5The equipment may be modified to allow a continuous flow of solution from the sample container into the distil
35、lation flask 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 has enteredthe distillation flask.9.4 When the bulk of the solvent has been distilled from the asphalt and no obvious condensati
36、on is occurring on the condenser,immerse the flask to the recommended maximum immersion depth of approximately 40 mm 1.5 in. Slowly apply a vacuum of80.0 6 0.7 kPa 600 65 mm of Hg below atmospheric pressure. Increase nitrogen or carbon dioxide flow to approximately 600mL/min and the spin rate of the
37、 distillation flask to about 45 rpm (Note 6). Hold or reduce vacuum if foaming or a bubbly formationoccurs. When foaming subsides apply maximum vacuum. Maintain this condition for 1510 6 1 min.NOTE 6It is recommended that the flask be immersed for up to 2 min before slowly applying the vacuum.NOTE 7
38、A faster flask spin rate exposes more surface area of the asphalt and, hence, dislodges more traces of solvent from the asphalt. The rotationspeed of the flask may also be varied or the flask rotation may be stopped to enhance the removal of solvent.NOTE 8Due to the cooling effect of the increased n
39、itrogen or carbon dioxide flow, an increase in the temperature of the oil bath is generally neededto maintain a constant sample temperature. Experience has shown that a typical oil bath temperature range of 150 to 155C300 to 310F is satisfactoryfor this purpose.9.5 At the end of the 1510 min period,
40、 remove the distillation flask from the apparatus and wipe the flask clean of oil. Pour theasphalt into a proper size container. If needed, the flask may be inverted and placed into an oven at 165 6 1C5C 329 62F10F for 10 to 15 min to cause the asphalt to flow into the container. The asphalt should
41、not be allowed to be distributed overthe interior of the flask.9.6 Portions of the recovered asphalt, while still in a liquid state, can be taken for penetration, softening point, ductility, andkinematic and absolute viscosity determinations as required. If ash content determinations are to be condu
42、cted, they shall bedetermined in accordance with Methods D2939 and reported with other test data on the recovered asphalt.NOTE 9Ash contents of recovered asphalts greater than 1 % may affect the accuracy of the penetration, ductility, softening point, or viscosity tests.NOTE 10Results reported by th
43、e AASHTO Materials Reference Laboratory for proficiency samples from 1992 to 1996 indicate that thebetween-laboratory precision (1S%) ranges from 16 to 30 % for penetration of recovered asphalt, 10 to 22 % for kinematic viscosity (135C 275F),4 Available from American Conference of Governmental Indus
44、trial Hygienists, 1330 Kemper Meadow Drive, Cincinnati, OH 45240, (513) 7422020, (www.acgih.org).D5404/D5404M 123and 16 to 45 % for viscosity at 60C 140F. These ranges are significantly larger than reported for testing original asphalts.10. Keywords10.1 bituminous paving mixtures; recovery; rotary e
45、vaporatorASTM 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 expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such ri
46、ghts, 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, either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional
47、 standardsand should be addressed 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
48、 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. 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 ASTM website (www.astm.org/COPYRIGHT/).D5404/D5404M 124
