1、Designation: D1461 17Standard Test Method forMoisture or Volatile Distillates in Asphalt Mixtures1This standard is issued under the fixed designation D1461; 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.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 This test method covers the determination, by
3、directmeasurement, of moisture or volatile fractions of the asphalt inasphalt mixtures.1.2 The values stated in SI units are to be regarded as thestandard. No other units of measurement are included in thisstandard.1.3 The text of this standard references notes and footnoteswhich provide explanatory
4、 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 theresponsibility of the user of this standard to establi
5、sh appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment
6、 of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D979/D979M Practice for Sampling Bituminous PavingMixturesD3666 Specification for Minimum Requirements for Agen-cies T
7、esting and Inspecting Road and Paving MaterialsD6997 Test Method for Distillation of Emulsified Asphalt3. Significance and Use3.1 This test method is used for determining either theamount of moisture or the amount of volatile petroleumdistillates in asphalt mixtures.3.2 Applicable standards are thos
8、e in which measurementsor calibrations are made, samples are procured, or products areselected.34. Apparatus4.1 Metal StillA vertical cylindrical still, similar to thatused in Test Method D6997, having a faced flange at the top towhich the head is tightly attached by means of a clamp. Thehead shall
9、be of metal, preferably of copper or brass, and shallhave a tube opening of 25.4 mm of inside diameter to facilitateattachment of the specified trap/condenser assembly.4.2 Condenser, of the water-cooled reflux glass-tube type,having a condenser jacket not less than 400 mm long with aninner tube 9.5
10、to 12.7 mm in outside diameter. The end of thecondenser inserted in the trap shall be ground off at an angle of30 from the vertical axis of the condenser. For mixtures withvery volatile solvents, it may be necessary to supplement thiswater-cooled condenser with a second water-cooled condenserof appr
11、oximately the same dimensions.4.3 Trap, of well-annealed glass, of one of the followingtypes depending upon the purpose of the test:4.3.1 For determination of water in asphalt mixtures, a glasstrap of 10- or 25-mL capacity shall be used. The trap shall begraduated in 0.1-mL divisions with 60.05-mL m
12、aximum errorbelow 1 mL, and in 0.2-mL divisions with a 60.1-mLmaximum error above 1 mL, as specified in Table 1 and Figs.1-4. Tapered ball traps require adaptors for connection to themetal still.1This test method is under the jurisdiction of ASTM Committee D04 on Roadand Paving Materials and is the
13、direct responsibility of Subcommittee D04.25 onAnalysis of Asphalt Mixtures.Current edition approved June 1, 2017. Published June 2017. Originallyapproved in 1956. Last previous edition approved in 2011 as D1461 11. DOI:10.1520/D1461-17.2For referenced ASTM standards, visit the ASTM website, www.ast
14、m.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.3The quality of the results produced by this standard are dependent on thecompetence of the personnel performing the procedu
15、re and the capacity, calibration,and maintenance of the equipment used. Agencies that meet the criteria ofSpecification D3666 are generally considered capable of competent and objectivetesting, sampling, inspection, etc. Users of this standard are cautioned thatcompliance with Specification D3666 al
16、one does not completely ensure reliableresults. Reliable results depend on many factors; following the suggestions ofSpecification D3666 or some similar acceptable guideline provides a means ofevaluating and controlling some of those factors.Copyright ASTM International, 100 Barr Harbor Drive, PO Bo
17、x C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by t
18、he World Trade Organization Technical Barriers to Trade (TBT) Committee.14.3.2 For determination of the volatile fractions of theasphalt, the trap shall conform to the dimensions shown in Fig.5.4.4 SolventFor general use, an aromatic solvent ispreferred, since it has high solvency and dispersing pow
19、er formost asphalt materials. Xylene, or a blend of 20 % toluene and80 % xylene, is recommended. For asphalts and similar petro-leum products, a petroleum distillate, 5 % boiling between 90and 100 C, and 90 % distilling below 210 C may be used. Forcoal tar, water-gas tar, and similar materials, the
20、aromaticsolvent must be used.4.5 Heating Device Any satisfactory source of heat thatwill be capable of maintaining a rate of distillation of 85 to95 drops min.TABLE 1 Dimensions and Sizes of TrapsStyleDescriptionFigureSize ofTrap,mLRange, mLSmall-estScaleDivision,mLScaleErrormax, mLTop ofGraduatedTu
21、beBottom ofGraduatedTubeBottom ofVaporTubeA$ joint conical $ joint 7100to 1.0over 1.0 to 10.00.10.20.050.1BCD joint$ jointplainconicalconicalconical jointplainplain8910 250to 1.0over 1.0 to 250.10.20.050.1E$ joint round $ joint 115100to 5.00to10.00.10.10.050.1NOTE 1All dimensions are in millimetres.
22、FIG. 1 Traps (Style A)NOTE 1All dimensions are in millimetres.FIG. 2 Traps (Style B)D1461 1725. Sampling5.1 Sampling shall be carried out in accordance with theprocedures set forth in Test Method D979/D979M.5.2 The sample shall be representative of the material andshall be of such size as practical
23、to fill the container in whichit is transported to the laboratory. For duplicate tests, a 1.9-Lfriction-top tin pail full of the material would be satisfactory.6. Test Specimen and Sample6.1 Thoroughly mix the sample and weigh out an amountestimated to show a percentage of moisture or diluent within
24、the capacity of the trap calibration. Keep the remainder of thesample in its tightly covered container. The weighed sampleshould be preferably not less than 500 g for normal mixtures.Thoroughly break up this sample to avoid larger lumps, andplace it in the still.7. Procedure for Determination of Moi
25、sture7.1 After the sample has been placed in the still, add 200 mLof the solvent and quickly stir it into the sample.7.2 Assemble the components of the apparatus as illustratedin Fig. 6, choosing the trap in accordance with the expectedwater content of the sample and making all connections vaporand
26、liquid tight. Insert a gasket of heavy paper, moistened withwater between the still body and cover. The condenser tube andtrap must be chemically clean to ensure free drainage of waterinto the bottom of the trap. Insert a loose cotton plug in the tipof the condenser to prevent condensation of atmosp
27、hericmoisture inside it. Circulate cold water through the jacket ofthe condenser.7.3 Apply heat at such a rate that refluxing will start within5 to 10 min after the heat has been applied and the condensersolvent will drip into the trap at a rate of 85 to 95 drops/min.NOTE 1All dimensions are in mill
28、imetres.FIG. 3 Traps (Style C)NOTE 1All dimensions are in millimetres.FIG. 4 Traps (Style D)D1461 173Continue the distillation until three successive readings of thetrap at 15-min intervals show no increase in the amount ofwater being condensed, except that in no case shall distillationcontinue for
29、more than 112 h.7.4 Allow the contents of the trap to reach room temperatureand read the volume of water in the trap to the nearest scaledivision. Record the volume of water and calculate in weightpercent as described in 9.1.8. Procedure for Determination of Volatile Distillates8.1 After the sample
30、has been placed in the still, add 350 mLof water and approximately3gofsodium carbonate (Na2CO3)and quickly stir into the sample. Firmly attach the still coverand assemble the trap and condenser in the manner prescribedin 7.2, except that the gasket is moistened with solvent and thetrap used shall be
31、 the dilution trap specified in 4.3.2.8.2 Apply heat at such a rate that the water and solvent willbegin to reflux in 5 to 10 min after the heat has been appliedand will drip from the condenser at the rate of 85 to95 drops min. In case the sample contains a large amount ofvery volatile solvent, it m
32、ay be necessary to add a secondwater-cooled condenser above the first one or to reduce the rateof distillation somewhat to prevent escape of the solvent.8.3 Continue distillation until three successive readings ofthe upper and lower levels of the diluent at 15-min intervalsshow no increase in the qu
33、antity being collected. Then removethe source of heat and allow the trap and contents to reachroom temperature. Allow the trap to stand a minimum of12 hto permit the solvent to separate.8.4 Record the volume of diluent in the trap to the nearestscale division and calculate in weight percent as descr
34、ibed in9.2. Use the specific gravity of the diluent at 25 C.9. Calculation9.1 Calculate the moisture content as follows:Water, % 5volume of water in trapweight of sample3100 (1)9.2 Calculate the volatile distillate as follows:Diluent, % 5volume diluent in trap!sp gr diluent at 25 C!weight of sample3
35、100(2)10. Report10.1 Report the moisture content as the weight percentwater content in accordance with 9.1.10.2 Report the volatile distillates as the weight percentdiluent content in accordance with 9.2.NOTE 1Assume specific gravity of diluent based on knowledge ofdiluent type or values in the rang
36、e of 0.85 to 0.90. This only definesFIG. 5 Apparatus for Determining Volatile Fractions of the AsphaltD1461 174volatiles that are obtained at the maximum test temperature.11. Precision11.1 Precision for Determination of MoistureThe follow-ing criteria should be used for judging the acceptability ofr
37、esults (95 % probability) when using the 10-mL or 25-mLtraps.11.1.1 RepeatabilityDuplicate determination of water bythe same operator should be considered suspect if they differ bymore than the following amounts:Water Collected, mL0to1.0 0.1mL1.1 to 25 0.1 mL or 2 % of the mean,whichever is greater1
38、1.1.2 ReproducibilityThe results submitted by each oftwo laboratories should be considered suspect if they differ bymore than the following amounts:Water Collected, mL0to1.0 0.2mL1.1 to 25 0.2 mL or 10 % of the mean,whichever is greater11.2 Precision for Determination of Volatile DistillatesThe prec
39、ision of this method as obtained by statistical exami-nation of interlaboratory test results is as follows:11.2.1 RepeatibilityDuplicate determinations of volatiledistillates by the same operator should be considered suspect ifthey differ by more than 0.6 volume %.11.2.2 ReproducibilityThe results s
40、ubmitted by each oftwo laboratories should be considered suspect if they differ bymore than 1.4 volume %.NOTE 1Trap shall be 15 to 16 mm in inside diameter.FIG. 6 Typical Assemblies with Metal StillD1461 175ASTM International takes no position respecting the validity of any patent rights asserted in
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