1、Designation: D 2042 01Standard Test Method forSolubility of Asphalt Materials in Trichloroethylene1This standard is issued under the fixed designation D 2042; 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 (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers the determination of the
3、 degreeof solubility in trichloroethylene of asphalt materials havinglittle or no mineral matter.NOTE 1Use of carbon disulfide, carbon tetrachloride, and benzene hasbeen discontinued in this method because of the safety hazards involved.This method is not applicable to tars and their distillation re
4、sidues orhighly cracked petroleum products. For methods covering tars, pitches,and other highly cracked petroleum products, and the use of othersolvents, see Test Methods D 4, D 2318, and D 2764.1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use.
5、 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. Specific precautionstatements are given in Section 7.2. Referenced Documents2.1 ASTM Standards:D 4 Test Method for Bitu
6、men Content2D 2318 Test Method for Quinoline-Insoluble (QI) Contentof Tar and Pitch3D 2764 Test Method for Dimethylformamide-Insoluble(DMF-I) Content of Tar and Pitch4E 177 Practice for the Use of the Terms Precision and Biasin ASTM Test Methods52.2 AASHTO Standard:T44 Solubility of Bituminous Mater
7、ials in Organic Sol-vents63. Summary of Method3.1 The sample is dissolved in trichloroethylene and filteredthrough a glass fiber pad. The insoluble material is washed,dried, and weighed.4. Significance and Use4.1 This test method is a measure of the solubility of asphaltin trichloroethylene. The por
8、tion that is soluble in trichloroet-hylene represents the active cementing constituents.5. Apparatus and Materials5.1 The assembly of the filtering apparatus is illustrated inFig. 1. Details of the component parts are as follows:5.1.1 Gooch Crucible, glazed inside and outside with theexception of ou
9、tside bottom surface. The approximate dimen-sions shall be a diameter of 44 mm at the top, tapering to 36mm at the bottom, and a depth of 24-28 mm.5.1.2 Glass Fiber Pad, 3.2-cm.75.1.3 Filter Flask, heavy-wall, with side tube, 250- or500-mL capacity.5.1.4 Filter Tube, 40- to 42-mm inside diameter.5.1
10、.5 Rubber Tubing or Adapter, for holding the Goochcrucible on the filter tube.NOTE 2Other suitable assemblies permitting vacuum filtration with aGooch crucible may be used.5.1.6 Erlenmeyer Flask, 125 mL.5.1.7 Oven, capable of maintaining a temperature of 110 65C.6. Reagent6.1 Trichloroethylene, tech
11、nical grade.7. Safety Precautions7.1 Trichloroethylene is toxic, and good ventilation shouldbe provided. It is more flammable than carbon tetrachloride.1This test method is under the jurisdiction of ASTM Committee D04 on Roadand Paving Materials and is the direct responsibility of Subcommittee D04.4
12、7 onMiscellaneous Asphalt Tests.Current edition approved Dec. 10, 2001. Published March 2002. Originallypublished as D 2042 66. Last previous edition D 2042 97.2Annual Book of ASTM Standards, Vol 04.04.3Annual Book of ASTM Standards, Vol 05.01.4Annual Book of ASTM Standards, Vol 05.02.5Annual Book o
13、f ASTM Standards, Vol 14.02.6Available from AASHTO, 444 N. Capitol St., NW, Suite 249, Washington, DC20001.7Whatman Grade 934 AH glass microfiber filter pad, available from ReevesAngel and Co., Clifton, NJ, has been found suitable.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, We
14、st Conshohocken, PA 19428-2959, United States.8. Preparation of Gooch Crucible8.1 Place the Gooch crucible plus one thickness of the glassfiber pad in an oven at 110 6 5C for 15 min, allow to cool ina desiccator, and then determine the mass to the nearest 0.1 mg.Designate this mass as A. Store in th
15、e desiccator until ready foruse.9. Sample Preparation9.1 If the sample is not fluid, heat to any convenienttemperature, but in any case not more than 111C above thesoftening point. Normally the temperature at which this test isrun is not critical, and it may be performed at the laboratory airtempera
16、ture. For referee tests, however, the flask and sample insolution shall be placed in a water bath maintained at 37.8 60.3C for 1 h before filtering.10. Procedure10.1 Note safety precautions in Section 7. Transfer approxi-mately2gofthesample into a tared 125-mL Erlenmeyer flaskor other suitable conta
17、iner. Allow the sample to cool to ambienttemperature and then determine the mass to the nearest 1 mg.Designate this mass as B. Add 100 mL of the trichloroethyleneto the container in small portions with continuous agitationuntil all lumps disappear and no undissolved sample adheres tothe container. S
18、topper the flask or otherwise cover the con-tainer and set aside for at least 15 min (see Section 7).10.2 Place the previously prepared and weighed Goochcrucible in the filtering tube. Wet the glass fiber pad with asmall portion of trichloroethylene and decant the solutionthrough the glass fiber pad
19、 of the crucible with or without lightsuction as may be necessary. When the insoluble matter isappreciable, retain as much of it as possible in the containeruntil the solution has drained through the mat. Wash thecontainer with a small amount of solvent and, using a stream ofsolvent from a wash bott
20、le, transfer all insoluble matter to thecrucible. Use a “policeman” if necessary to remove anyinsoluble matter adhering to the container. Rinse the policemanand container thoroughly. Wash the insoluble matter in thecrucible with solvent until the filtrate is substantially colorless,then apply strong
21、 suction to remove the remaining solvent.Remove the crucible from the tube, wash the bottom free ofany dissolved matter, and place the crucible on top of an ovenor on a steam bath until all odor of the trichloroethylene isremoved (see safety precautions in Section 6). Place thecrucible in an oven at
22、 110 6 5C for at least 20 min. Cool thecrucible in a desiccator for 30 6 5 min and determine its massto the nearest 0.1 mg. Repeat the drying and weighing untilconstant mass (6 0.3 mg) is obtained. Designate this mass asC.NOTE 3To obtain precise results, the cooling time in the desiccatormust be app
23、roximately the same (within 65 min) after all heatings. Forexample, if the mass of the empty crucible is determined after a 30-mincooling period in the dessicator, the mass of the crucible containing theinsoluble matter should be determined after a 30 6 5-min cooling periodin the desiccator. Either
24、empty crucibles or crucibles containing insolublematter that have remained in a desiccator overnight should be reheated inan oven for at least 30 min, then allowed to cool for the prescribed periodbefore the mass is determined.11. Calculation and Report11.1 Calculate either the total percentage of i
25、nsoluble matteror the percentage of the sample soluble in the solvent used asfollows:% Insoluble 5SC 2 ABD3 100 (1)% Soluble 5SB 2 C 2 A!BD3 100 (2)where:A = mass of crucible and filter,B = mass of sample, andC = mass of crucible, filter and insoluble material.11.2 For percentages of insoluble less
26、than 1.0, report to thenearest 0.01 %. For percentages of insoluble 1.0 or more,report to the nearest 0.1 %.12. Precision12.1 The following precision statement was formulatedwhen it was permissible to use carbon disulfide, carbontetrachloride, and benzene, as well as trichloroethylene andbefore the
27、substitution of the glass fiber pad for asbestos. It isincluded in the test method as a guide only.12.2 Estimates of standard deviations (sr8) for this proce-dure and the criteria for judging the acceptability of results(95 % confidence level) are as follows:FIG. 1 Filtering Apparatus AssemblyD20420
28、12Within-LaboratoryVariabilityABetween-LaboratoryVariabilityAStandardDeviationBRepeat-abilityCStandardDeviationBReproduc-ibilityDAsphalts, solubilitymorethan 99 % (appli-cablewhen either carbondisulfide,carbon tetrachloride,trichloroethylene, orbenzene are used)0.035 0.10 0.090 0.26AFor definitions
29、of terms and recommended use of precision indexes, seePractice E 177.BThe standard deviations shown (sr8) represent the estimated standarddeviation of the measurement process for the stated conditions. They arecalculated by multiplying the standard deviations of the applicable data by thefactor 1 +
30、14 (N 1) where N is the number of tests in the set of data.CTwo results obtained by an operator of the same sample should be consideredsuspect if they differ by more than the stated amount. As defined in Practice E 177,this is the “difference two-sigma” limits for single-laboratory-operator-machine-
31、multiday precision.DTwo results obtained by operators in different laboratories should be consid-ered suspect if they differ by more than the stated amount. As defined in PracticeE 177, this is the“ difference two-sigma” limits for multilaboratory-operator-machine-day precision.12.3 The estimates of
32、 standard deviation are based on thefollowing:Materials 4Replications 3Solvents 4Laboratories 26Degrees of freedom:Within-laboratory variability 159Between-laboratory variability 81Standard deviation (s) of data:Within-laboratory variation 0.035Between-laboratory variation 0.09012.4 AASHTO Materials
33、 Reference Laboratory (AMRL)data for Test Method D 2042 (and its AASHTO equivalentstandard, T44) were analyzed in 2001. These data representapproximately 13 200 repetitions of the test, conducted on 132samples having solubility values between 99.5 % and 100.0 %.For samples within this range, the ana
34、lysis suggests thefollowing precision values are appropriate:Multilab Standard Deviation (1S) = 0.01 + (0.753 % Insoluble)Single-Operator Standard Deviation (1S) = 0.01 + (0.25 3 % Insoluble)13. Keywords13.1 asphalt; Gooch crucible; solubility; trichloroethyleneASTM International takes no position r
35、especting 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 rights, are entirely their own responsibility.Thi
36、s 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 standardsand should be addressed to ASTM Inte
37、rnational 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 Committee on Standards, at the address shown
38、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).D2042013
