ASTM D5546 - 09 Standard Test Method for Solubility of Asphalt Binders in Toluene by Centrifuge (Withdrawn 2017).pdf

1、Designation: D5546 09Standard Test Method forSolubility of Asphalt Binders in Toluene by Centrifuge1This standard is issued under the fixed designation D5546; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio

2、n. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers determination of the degree ofsolubility of asphalt binders in toluene using centrifugalseparation. The me

3、thod is an alternative to Test Method D2042,and may be preferable to Test Method D2042 when testingmodified asphalt binders.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 The text of this standard references notes and f

4、ootnoteswhich provide explanatory material. These notes and footnotes(excluding those in tables and figures) shall not be consideredas requirements of the standard.1.4 A complete precision statement for this standard has notbeen developed at this time. Therefore, this standard should notbe used for

5、acceptance or rejection of a material for purchasingpurposes.1.5 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-

6、bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D36 Test Method for Softening Point of Bitumen (Ring-and-Ball Apparatus)D2042 Test Method for Solubility of Asphalt Materials inTrichloroethyleneD3666 Specification for Minimum Requirements for Agen-cies Testing

7、 and Inspecting Road and Paving MaterialsD4007 Test Method for Water and Sediment in Crude Oil bythe Centrifuge Method (Laboratory Procedure)3. Summary of Test Method3.1 The sample is dissolved in toluene and centrifuged toseparate the insoluble material. The insoluble material is driedand weighed.4

8、. Significance and Use4.1 This test method is a measure of the solubility ofpolymer-modified asphalt in toluene. The portion that issoluble in toluene represents the active cementing constituents.Additional tests to characterize the insoluble residue may beconducted. Such tests might include infrare

9、d spectroscopy,microscopy, ash content, and so forth.NOTE 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 Specificat

10、ion D3666 are generallyconsidered capable of competent and objective testing/sampling/inspection/etc. Users of this standard are cautioned that compliance withSpecification D3666 alone does not completely assure reliable results.Reliable results depend on many factors; following the suggestions ofSp

11、ecification D3666 or some similar acceptable guideline provides ameans of evaluating and controlling some of these factors.5. Apparatus and Materials5.1 Centrifuge:5.1.1 A centrifuge with a swinging bucket rotor capable ofspinning two or more filled centrifuge tubes shall be used. Thecentrifuge shal

12、l be capable of delivering a minimum relativecentrifugal force (RCF) of 700 at the tip of the tubes, andmaintaining this RCF for a minimum of 10 min.5.1.2 The revolving head, trunnion rings, and trunnion cups,including the cushions, shall be constructed soundly to with-stand the maximum centrifugal

13、force capable of being deliv-ered by the power source. The trunnion cups and cushions shallsupport the tubes firmly when the centrifuge is in motion. Thecentrifuge shall be enclosed by a metal chamber strong enoughto eliminate danger if any breakage occurs. The centrifugechamber shall be isolated fr

14、om potential ignition sources.5.2 Centrifuge TubesFor referee testing, each centrifugetube shall be a 100-mL cone-shaped tube conforming to thedimensions given in Fig. 1. For routine quality assurancetesting, alternate centrifuge tubes may be used. Alternatecentrifuge tubes shall have a cone shaped

15、bottom, a lengthbetween 150-210 mm, and a nominal capacity of 100 mL. All1This test method is under the jurisdiction of ASTM Committee D04 on Roadand Paving Materials and is the direct responsibility of Subcommittee D04.47 onMiscellaneous Asphalt Tests.Current edition approved June 1, 2009. Publishe

16、d June 2009. Originallyapproved in 1994. Last previous edition approved in 2001 as D5546 01. DOI:10.1520/D5546-09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to th

17、e standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesNOTICE: This standard has either been superseded and replaced by a new version or withdrawn.Contact ASTM International (www.astm.org)

18、for the latest information1centrifuge tubes shall be made of thoroughly annealed glassand shall be marked at the 100-mL level.NOTE 2Centrifuge tubes meeting the requirements of Test MethodsD4007 are widely available, and are suitable for use in this test. The203-mm centrifuge tubes described in D400

19、7 are suitable for refereetesting.5.3 Erlenmeyer FlaskA 125-mL Erlenmeyer flask shall beused.5.4 OvenAn explosion-proof, ventilated oven capable ofmaintaining a temperature of 130 6 5C shall be used to drythe insoluble material.5.5 BalanceA balance or scale with a capacity of 100 g orhigher, sensiti

20、ve to 0.1 mg and accurate within 0.1 % of theload.NOTE 3Static electricity may cause unstable mass measurements, duein part to the characteristics of the glass centrifuge tubes. This problem canbe minimized by mounting a passive ion source inside the balance draftshield. Passive ion sources are avai

21、lable from electronic balancemanufacturers, distributors and service companies.6. Reagent6.1 Toluene, reagent grade.7. Preparation of Centrifuge Tubes7.1 Place two clean centrifuge tubes in an oven at130 6 5C for 20 min, allow to cool in a desiccator for aminimum of 30 min, and then weigh to the nea

22、rest 1 mg. Storein the desiccator until ready for use.8. Sample Preparation8.1 If the sample is not fluid, heat to any convenienttemperature, but in any case not more than 100C above thesoftening point (Test Method D36). The test may be performedat the laboratory air temperature. For referee tests,

23、however, theflask and sample in solution shall be placed in a water bathmaintained at 25 6 1C for about 1 h before centrifuging.9. Procedure9.1 Transfer approximately2gofthesample into a tared125-mL Erlenmeyer flask. Weigh accurately to the nearest 1mg. Add 100 mL of the toluene to the container in

24、smallportions, with continuous agitation, until all lumps disappearand no undissolved sample adheres to the container. Stopperthe flask or otherwise cover the container, and set aside for atleast 15 min (see Section 8).9.2 Transfer the solution to two clean pre-weighed centri-fuge tubes. Use additio

25、nal solvent to ensure that all insolublematter is transferred to the centrifuge tubes, and fill both tubesto the 100-mL mark. Stopper the tubes tightly and shake well.Carefully remove the stoppers to relieve any pressure in thetubes, and replace the stoppers. Place the tubes in the centri-fuge on op

26、posite sides to provide proper balance, and spin for10 min at a rate sufficient to produce a minimum relativecentrifugal force of 700, as calculated in 9.2.1.9.2.1 Calculate the minimum required speed of the rotatinghead in revolutions per minute (r/min) as follows:r/min 5 1335 =rcf/d (1)where:rcf =

27、 relative centrifugal force (700), andd = diameter of swing (mm) measured between tips ofopposite tubes when in rotating position.9.3 After centrifuging the samples, inspect each tube andnote the presence of any film or particulate matter floating onthe surface.NOTE 4Any floating material represents

28、 insoluble matter with adensity less than toluene (0.87 g/cc at 25C). The only known insolublematerials that will float under these conditions are particles which containan entrained gas. Any such floating material cannot be reliably quantifiedby this method, due to potential loss during decanting.9

29、.4 Decant the liquid from the centrifuge tubes withoutdisturbing the insoluble material. Refill the tubes with toluene,and shake well to wash the insoluble material. Repeat thecentrifuging and decanting steps after carefully relieving anybuilt-up pressure in the tubes.9.5 Place the tubes containing

30、the washed insoluble materialin the oven at 130 6 5C for at least 20 min. Cool in adesiccator for a minimum of 30 min and weigh. Repeat thedrying and weighing until constant weight is obtained.FIG. 1 100-mL Centrifuge TubeD5546 0929.6 Alternate methods of drying the tubes, such as vacuumdesiccation,

31、 are also acceptable. However, the method de-scribed in 9.5 shall be the referee method.10. Calculation and Report10.1 Calculate the percentage of the sample soluble intoluene as follows:percent soluble 5 100 2 A/B! 3100# (2)where:A = total weight of insoluble material, andB = weight of sample.10.2

32、Report the results to the nearest 0.01 %.10.3 If both tubes contained floating insoluble material, asdescribed in 9.3, append the words “or less” to the numericresult, and report that “This sample contained an undeterminedquantity of low-density insoluble matter.”11. Precision and Bias11.1 Available

33、 precision information for this test is summa-rized in the following table:Numberof Labs Binder Type Repetitions Mean Std Dev1 PMA 4 99.71 % 0.20 %1 Neat + TLA 4 99.19 % 0.23 %4 Neat 8 99.97 % 0.03 %Additional precision information is being developed and willbe included in future revisions of this s

34、tandard.11.2 A complete precision statement is not available at thistime. Therefore, this standard should not be used for accep-tance or rejection of material for purchasing purposes.11.3 Since there is no accepted reference material suitablefor determining the bias in this test method, no statement

35、 onbias is made.12. Keywords12.1 asphalt binder; centrifuge; solubility; tolueneASTM 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 val

36、idity 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, either reapproved or withdrawn. Your com

37、ments 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 attend. If you feel that your comments have

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