1、Designation: D 5546 01Standard Test Method forSolubility of Asphalt Binders in Toluene by Centrifuge1This standard is issued under the fixed designation D 5546; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、 method is an alternative to Test MethodD 2042, and may be preferable to Test Method D 2042 whentesting modified asphalt binders.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address
4、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 prior to use.2. Referenced Documents2.1 ASTM Standards:D36 Test Method for
5、 Softening Point of Bitumen (Ring-and-Ball Apparatus)2D96 Test Methods for Water and Sediment in Crude Oil byCentrifuge Method (Field Procedure)3D 2042 Test Method for Solubility of Asphalt Materials inTrichloroethylene43. Summary of Test Method3.1 The sample is dissolved in toluene and centrifuged
6、toseparate the insoluble material. The insoluble material is driedand weighed.4. 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 chara
7、cterize the insoluble residue may beconducted. Such tests might include infrared spectroscopy,microscopy, ash content, and so forth.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. Thecentri
8、fuge shall 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 cen
9、trifugal 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 is
10、olated from potential ignition sources.5.2 Centrifuge TubesFor referee testing, each centrifugetube shall be a 203-mm 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 con
11、e shaped bottom, a lengthbetween 150-210 mm, and a nominal capacity of 100 ml. Allcentrifuge tubes shall be made of thoroughly annealed glassand shall be marked at the 100-ml level.NOTE 1Centrifuge tubes meeting the requirements of Test MethodsD96 are widely available, and are suitable for use in th
12、is test. The203-mm centrifuge tubes described in D96are suitable for referee testing.The 167-mm centrifuge tubes described in D96are suitable for routinequality-assurance testing.5.3 Erlenmeyer FlaskA125-mL Erlenmeyer flask shall beused.5.4 OvenAn explosion-proof, ventilated oven capable ofmaintaini
13、ng 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, sensitive to 0.1 mg and accurate within 0.1 % of theload.NOTE 2Static electricity may cause unstable mass measurements, duein part to the characteristics of the gl
14、ass centrifuge tubes. This problem canbe minimized by mounting a passive ion source inside the balance draftshield. Passive ion sources are available from electronic balance manu-facturers, distributors and service companies.6. Reagent6.1 Toluene, reagent grade.1This test method is under the jurisdi
15、ction of ASTM Committee D04 on Roadand Paving Materials and is the direct responsibility of Subcommittee D04.47 onMiscellaneous Asphalt Tests.Current edition approved Dec. 10, 2001. Published February 2002. Originallypublished as D 5546 94. Last previous edition D 5546 94a.2Annual Book of ASTM Stand
16、ards, Vol 04.04.3Discontinued. See 2000 Annual Book of ASTM Standards, Vol 05.01.4Annual Book of ASTM Standards, Vol 04.03.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. Preparation of Centrifuge Tubes7.1 Place two clean centrifu
17、ge 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 nearest 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 a
18、bove thesoftening point (Test Method D36). The test may be performedat the laboratory air temperature. For referee tests, 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 approximately2gofthesampl
19、e into a tared125-mL Erlenmeyer flask. Weigh accurately to the nearest 1mg. Add 100 mL of the toluene to the container in smallportions, with continuous agitation, until all lumps disappearand no undissolved sample adheres to the container. Stopperthe flask or otherwise cover the container, and set
20、aside for atleast 15 min (see Section 8).9.2 Transfer the solution to two clean pre-weighed centri-fuge tubes. Use additional 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 r
21、emove the stoppers to relieve any pressure in thetubes, and replace the stoppers. Place the tubes in the centri-fuge on opposite 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
22、minimum required speed of the rotatinghead in revolutions per minute (r/min) as follows:r/min 5 1335 =rcf/d (1)where:rcf = 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
23、 tube andnote the presence of any film or particulate matter floating onthe surface.NOTE 3Any floating material represents 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 entra
24、ined gas. Any such floating material cannot be reliably quantifiedby this method, due to potential loss during decanting .9.4 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 thec
25、entrifuging and decanting steps after carefully relieving anybuilt-up pressure in the tubes.9.5 Place the tubes containing 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 wei
26、ght is obtained.9.6 Alternate methods of drying the tubes, such as vacuumdesiccation, 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!
27、 3 100 (2)where:A = total weight of insoluble material, andB = weight of sample.10.2 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 undet
28、erminedquantity of low-density insoluble matter.”11. Precision and Bias11.1 Available 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 %FIG. 1 203-mm (8
29、-in.) Centrifuge TubeD5546012Additional precision information is being developed and willbe included in future revisions of this standard.11.2 Bias has not been determined since there is no acceptedreference material suitable for determining the bias for theprocedure in this test method.12. Keywords
30、12.1 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 validity of any such patent rig
31、hts, 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 comments are invited either for
32、 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 not received a fair hearing
33、 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. 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).D5546013
