1、Designation: D 7553 09Standard Test Method forSolubility of Asphalt Materials in N-Propyl Bromide1This standard is issued under the fixed designation D 7553; 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
3、a replacement for method D 2042 specifying asolvent that, like trichloroethylene, is safe in that it has no flashpoint, and has similar solubilizing characteristics to trichloro-ethylene, but it is not considered to be an ozone depleterbanned by the Kyoto Protocol. Since a complete precisionstatemen
4、t for this test method has not yet been developed, thistest method should not be used for buying and selling purposesuntil the complete precision statement is available.NOTE 1This method is not applicable to tars and their distillationresidues or highly cracked petroleum products. For methods coveri
5、ng tars,pitches, and other highly cracked petroleum products, and the use of othersolvents, see Test Methods D4, D 2318, and D 2764.1.2 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 not
6、es and footnoteswhich provide explanatory material. These notes and footnotes(excluding those in tables and figures) shall not be consideredas requirements of the standard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibilit
7、y 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:2D4 Test Method for Bitumen ContentD 2042 Test
8、Method for Solubility of Asphalt Materials inTrichloroethyleneD 2318 Test Method for Quinoline-Insoluble (QI) Contentof Tar and PitchD 2764 Test Method for Dimethylformamide-Insoluble(DMF-I) Content of Tar and PitchD 3666 Specification for Minimum Requirements forAgen-cies Testing and Inspecting Roa
9、d and Paving MaterialsD 6368 Specification for Vapor-Degreasing Solvents Basedon normal-Propyl Bromide and Technical Grade normal-Propyl BromideE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision o
10、f 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 test method is a measure of the solubility of asphaltin n-propyl bromide. The portion tha
11、t 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 procedureand the capability, calibration, and maintenance of the equipment used.Agencies that meet th
12、e criteria of Specification D 3666 are generallyconsidered capable of competent and objective testing/sampling/inspection/etc. Users of this standard are cautioned that compliance withSpecification D 3666 alone does not completely assure reliable results.Reliable results depend on many factors; foll
13、owing the suggestions ofSpecification D 3666 or some similar acceptable guideline provides ameans of evaluating and controlling some of these factors.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 Bit
14、umen 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 a depth of 20-30 mm.5.1.2 Glass Microfiber Filter Pad, 3234 mm diameter, fineporosity, fast flo
15、w rate, 1.5 m particle retention.1This 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. Published June 2009.2For referenced ASTM standar
16、ds, visit the ASTM 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA
17、19428-2959, United States.5.1.3 Filter Flask, heavy-wall, with side tube, 250- or500-mL capacity.5.1.4 Filter Tube, 40 to 42 mm inside diameter.5.1.5 Rubber Tubing or Adapter, for holding the crucible onthe filter tube.NOTE 3Other suitable assemblies permitting vacuum filtration with acrucible may b
18、e 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, technical grade, conforming toSpecification D 6368. Warning: see Section 7.7. Hazards7.1 Warning: n-propyl bromide is toxic and should be usedonly under a hood or with an
19、 effective surface exhaust systemin a well-ventilated area.8. Preparation of Crucible8.1 Place the crucible plus one thickness of the filter 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.
20、Store in the desiccator untilready for use.9. Sample Preparation9.1 If the sample is not fluid, heat to any convenienttemperature, but in 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
21、 airtemperature. For referee tests, however, the flask and sample insolution shall be placed in a water bath maintained at 38.0 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 sui
22、table container. Smaller sample sizes may benecessary if more than 0.5 % insoluble material is expected.Allow the sample to cool to ambient 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 c
23、ontinuous agitation until all lumps disap-pear and no undissolved sample adheres to the container.Stopper the flask or otherwise cover the 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
24、a small portion ofn-propyl bromide and decant the solution through the filter padof the crucible with or without light suction as may benecessary. When the insoluble matter is appreciable, retain asmuch of it as possible in the container until the solution hasdrained through the mat. Wash the contai
25、ner with a smallamount of solvent and, using a stream of solvent from a washbottle, transfer all insoluble matter to the crucible. Use a“policeman” if necessary to remove any insoluble matteradhering to the container. Rinse the policeman and containerthoroughly. Wash the insoluble matter in the cruc
26、ible withsolvent until the filtrate is substantially colorless, and thenapply strong suction to remove the remaining solvent. Removethe crucible 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 bromi
27、de 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 adesiccator 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
28、as C.NOTE 4To obtain precise results, the cooling time in the desiccatormust be approximately 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 desiccator, the mass of the crucible containing theinsoluble matt
29、er should be determined after a 30 6 5-min cooling periodin the desiccator. Either 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 d
30、etermined.11. Calculation and Report11.1 Calculate either the total percentage of insoluble matteror the percentage of the sample soluble in the solvent used asfollows:% Insoluble 5SC ABD3 100 (1)% Soluble 5SB C A!BD3 100 (2)where:A = mass of crucible and filter,B = mass of sample, andC = mass of cr
31、ucible, filter and insoluble material.FIG. 1 Filtering Apparatus AssemblyD755309211.2 For percentages of insoluble less than 1.0, report to thenearest 0.01 %. For percentages of insoluble 1.0 or more,report to the nearest 0.1 %.12. Precision and Bias12.1 The precision of this test method is based on
32、 aninterlaboratory study of this test method, conducted in 2008. Asingle laboratory tested a total of four asphaltic materials.Every “test result” represents an individual determination. Thelaboratory reported triplicate test results for the analysis.Except for the limited number of laboratories, Pr
33、actice E 691was followed for the design and analysis of the data; the detailsare given in ASTM Research Report No. D04-1031.312.1.1 Repeatability limit (r)Two test results obtainedwithin one laboratory shall be judged not equivalent if theydiffer by more than the “r” value for that material; “r” is
34、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 Repeatability limits are listed in Table 1 below.12.1.2 Reproducibility limit “R”Two test results shall
35、 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 operators using different equipment indifferent laboratories.12.1.2.1 The reproducibility
36、of this test method is beingdetermined and will be available on or before January 1, 2012.12.1.3 The above terms (repeatability limit and reproduc-ibility limit) are used as specified in Practice E 177.12.1.4 Any judgment in accordance with statements 12.1.1and 12.1.2 would normally have an approxim
37、ate 95 % prob-ability of being correct, however the precision statistics ob-tained in the ILS must not be treated as exact mathematicalquantities which are applicable to all circumstances and uses.The limited number of laboratories reporting replicate resultsguarantees that there will be times when
38、differences greaterthan predicted by the ILS results will arise, sometimes withconsiderably greater or smaller frequency than the 95 %probability limit would imply. The repeatability limit should beconsidered as a general guide, and the associated probability of95 % as only a rough indicator of what
39、 can be expected.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 of 12 results, from a single l
40、aboratory, onthe four materials described below:Unmodified AsphaltPolymer Modified AsphaltTire Rubber Modified AsphaltAsphalt Emulsion Residue13. Keywords13.1 asphalt; n-propyl bromide; solubilityASTM International takes no position respecting the validity of any patent rights asserted in connection
41、 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 t
42、echnical 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 International Headquarters. Your comments will receive careful conside
43、ration 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
44、 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
45、(www.astm.org).3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D041031.TABLE 1 Solubility (Mass %)Material AverageARepeatabilityStandardDeviationRepeatabilityLimitXSrrUnmodified Asphalt 99.973 0.021 0.058Polymer Modified Asphalt 99.867 0.025 0.070Tire Rubber Modified Asphalt 99.397 0.090 0.253Asphalt Emulsion Residue 98.867 0.270 0.757AThe average of the laboratories calculated averages.D7553093
