1、Designation: D7553 15Standard Test Method forSolubility of Asphalt Materials in N-Propyl Bromide1This standard is issued under the fixed designation D7553; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision.
2、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 the determination of the degreeof solubility in n-propyl bromide of asphalt materials. It isintended to be a
3、replacement for Test Method D2042 specify-ing a solvent that, like trichloroethylene, is safe in that it has noflash point, and has similar solubilizing characteristics totrichloroethylene, but it is not considered to be an ozonedepleter banned by the Kyoto Protocol.NOTE 1This method is not applicab
4、le to tars and their distillationresidues or highly cracked petroleum products. For methods covering tars,pitches, and other highly cracked petroleum products, and the use of othersolvents, see Test Methods D4, D2318, and D2764.1.2 The text of this standard references notes and footnoteswhich provid
5、e explanatory material. These notes and footnotes(excluding those in tables and figures) shall not be consideredas requirements of the standard.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purpo
6、rt 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-bility of regulatory limitations prior to use. Specific precautionstatements are given in Sec
7、tion 7.2. Referenced Documents2.1 ASTM Standards:2D4 Test Method for Bitumen ContentD2042 Test Method for Solubility of Asphalt Materials inTrichloroethyleneD2318 Test Method for Quinoline-Insoluble (QI) Content ofTar and PitchD2764 Test Method for Dimethylformamide-Insoluble(DMF-I) Content of Tar a
8、nd PitchD3666 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-Propyl BromideE177 Practice for Use of the Terms Precision and Bias inASTM Tes
9、t MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Summary of Test Method3.1 The sample is dissolved in n-propyl bromide and filteredthrough a glass fiber pad. The insoluble material is washed,dried, and weighed.4. Significance and Use4.1 This
10、 test method is a measure of the solubility of asphaltin n-propyl bromide. The portion that is soluble in n-propylbromide represents the active cementing constituents.NOTE 2The quality of the results produced by this standard aredependent on the competence of the personnel performing the procedurean
11、d the capability, calibration, and maintenance of the equipment used.Agencies that meet the criteria of Specification D3666 are generallyconsidered capable of competent and objective testing/sampling/inspection/etc. Users of this standard are cautioned that compliance withSpecification D3666 alone d
12、oes not completely assure reliable results.Reliable results depend on many factors; following the suggestions ofSpecification D3666 or some similar acceptable guideline provides ameans of evaluating and controlling some of these factors.5. Apparatus and Materials5.1 The assembly of a typical filteri
13、ng apparatus is illus-trated in Fig. 1. Details of the component parts are as follows:5.1.1 Bitumen Crucible or Gooch Crucible, glazed insideand outside with the exception of outside bottom surface. Theapproximate dimensions shall be a diameter of 44 mm at thetop tapering to 36 mm at the bottom and
14、a depth of 20 to 30mm.5.1.2 Glass Microfiber Filter Pad, 3234 mm diameter, fineporosity, fast flow rate, 1.5 m particle retention.5.1.3 Filter Flask, heavy-wall, with side tube, 250, 500, or1000 mL capacity.5.1.4 Filter Tube, 40 to 42 mm inside diameter.1This test method is under the jurisdiction of
15、 ASTM Committee D04 on Roadand Paving Materials and is the direct responsibility of Subcommittee D04.47 onMiscellaneous Asphalt Tests.Current edition approved June 1, 2015. Published July 2015. Originallypublished 2010 as D7553 10. DOI: 10.1520/D7553-15.2For referenced ASTM standards, visit the ASTM
16、 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United
17、States15.1.5 Rubber Tubing or Adapter, for holding the crucible onthe filter tube.NOTE 3Other suitable assemblies permitting vacuum filtration with acrucible 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 n-Propyl Bromide, technic
18、al grade, conforming toSpecification D6368. Warning: see Section 7.7. Hazards7.1 Warning: n-propyl bromide is toxic and should be usedonly under a hood or with an effective surface exhaust systemin a well-ventilated area.8. Preparation of Crucible8.1 Place the crucible plus one thickness of the filt
19、er pad inan oven at 110 6 5C for 15 min, allow to cool in a desiccatorfor 30 6 5 min, and then determine the mass to the nearest 0.1mg. Designate this mass as A. Store in the desiccator untilready for use.9. Sample Preparation9.1 If the sample is not fluid, heat to any convenienttemperature, but in
20、any case not more than 100C above thesoftening point. Normally the temperature at which this test isrun is not critical, and it may be performed at the laboratory airtemperature. For referee tests, however, the flask and sample insolution shall be placed in a water bath maintained at 38.0 60.3C for
21、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 container. Smaller sample sizes may benecessary if more than 0.5 % insoluble material is expected.Allow the sample to cool to ambien
22、t temperature and thendetermine the mass to the nearest 1 mg. Designate this mass asB. Add 100 mL of the n-propyl bromide to the container insmall portions with continuous agitation until all lumps disap-pear and no undissolved sample adheres to the container.Stopper the flask or otherwise cover the
23、 container and set asidefor at least 15 min (see Section 9).10.2 Place the previously prepared and weighed crucible inthe filtering tube. Wet the filter pad with a small portion ofn-propyl bromide and decant the solution through the filter padof the crucible with or without light suction as may bene
24、cessary. When the insoluble matter is appreciable, retain asmuch of it as possible in the container until the solution hasdrained through the mat. Wash the container with a smallamount of solvent and, using a stream of solvent from a washbottle, transfer all insoluble matter to the crucible. Use a“p
25、oliceman” if necessary to remove any insoluble matteradhering to the container. Rinse the policeman and containerthoroughly. Wash the insoluble matter in the crucible withsolvent until the filtrate is substantially colorless, and thenapply strong suction to remove the remaining solvent. Removethe cr
26、ucible from the tube, wash the bottom free of anydissolved matter, and place the crucible on top of an oven or ona steam bath until all odor of the n-propyl bromide is removed(see safety precautions in Section 7). Place the crucible in anoven at 110 6 5C for at least 20 min. Cool the crucible in ade
27、siccator for 30 6 5 min and determine its mass to the nearest0.1 mg. Repeat the drying and weighing until constant mass(60.3 mg) is obtained. Designate this mass as C.NOTE 4To obtain precise results, the cooling time in the desiccatormust be approximately the same (within 65 min) after all heatings.
28、 Forexample, if the mass of the empty crucible is determined after a 30-mincooling period in the desiccator, the mass of the crucible containing theinsoluble matter should be determined after a 30 6 5-min cooling periodin the desiccator. Either empty crucibles or crucibles containing insolublematter
29、 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 insoluble matteror the percentage of the sample soluble
30、in the solvent used asfollows:% Insoluble 5SC 2 ABD3100 (1)% Soluble 5SB 2 C 2 A!BD3100 (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 than 1.0, report to thenearest 0.01 %. For percentages of
31、 insoluble 1.0 or more,report to the nearest 0.1 %.FIG. 1 Filtering Apparatus AssemblyD7553 15212. Precision and Bias312.1 The precision of this test method is based on aninterlaboratory study of Test Method D7553 conducted in2010. Fifteen laboratories participated in this study. Each of thelabs was
32、 asked to report three replicate test results for tendifferent sample materials, nine which were an assortment ofdifferent sources of modified and unmodified paving asphalts,roofing asphalts, and emulsified asphalt residues, and a singlespecimen type representing natural asphalts or high mineralfill
33、er asphalts. Every “test result” reported represents a singledetermination or measurement. Practice E691 was followed forthe design and analysis of the data; the details are given inASTM Research Report No. D04-1034.12.1.1 Repeatability limit (r)Two test results obtainedwithin one laboratory shall b
34、e judged not equivalent if theydiffer by more than the “r” value for that material; “r” is theinterval representing the critical difference between two testresults for the same material, obtained by the same operatorusing the same equipment on the same day in the samelaboratory.12.1.1.1 Repeatabilit
35、y limits are listed in Table 1.12.1.2 Reproducibility limit “R”Two test results shall bejudged not equivalent if they differ by more than the “R” valuefor that material; “R” is the interval representing the criticaldifference between two test results for the same material,obtained by different opera
36、tors using different equipment indifferent laboratories.12.1.2.1 Reproducibility limits are listed in Table 1.12.1.3 The above terms (repeatability limit and reproduc-ibility limit) are used as specified in Practice E177.12.1.4 Any judgment in accordance with statements 12.1.1and 12.1.2 would have a
37、n approximate 95 % probability ofbeing correct.12.2 BiasAt the time of the study, there was no acceptedreference material suitable for determining the bias for this testmethod. Therefore, no statement on bias is being made.12.3 The precision statement was determined through sta-tistical examination
38、of 435 results, from fifteen laboratories, ona total of ten different sample materials from various sourcesthroughout the Western Hemisphere.13. Keywords13.1 asphalt; n-propyl bromide; solubilityASTM International takes no position respecting the validity of any patent rights asserted in connection
39、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.This standard is subject to revision at any time by the responsible te
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41、ation 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 below.This standard is copyrighted by ASTM International, 100 Barr
42、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(
43、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:/ data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D04-1034.T
44、ABLE 1 Solubility (Mass %)Sample AverageARepeatabilityStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitXHSrSRrRModified and Unmodified PavingAsphalts, Roofing Asphalts, andEmulsified Asphalt ResiduesB99.7677 0.0576 0.0921 0.1612 0.2580Natural Asphalts or High MineralFiller Asphalts66.9931 10.1178 16.9740 28.3300 47.5272AThe average of the laboratories calculated averages.BThe results from nine different specimen types were averaged to produce these statisticsD7553 153
