1、Designation: D1461 11Standard Test Method forMoisture or Volatile Distillates in Bituminous PavingMixtures1This 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
2、revision. 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 Department of Defense.1. Scope1.1 This test method covers the determination,
3、 by directmeasurement, of moisture or volatile fractions of the bitumenin bituminous paving mixtures.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 all of thesafety concerns, i
4、f 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:2D979 Practice for Sampling Bituminous Paving M
5、ixturesD6997 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 bituminous paving mixtures.4. Apparatus4.1 Metal Still A vertical cylindrical still, simil
6、ar to thatused in Test Methods D6997, having a faced flange at the topto which the head is tightly attached by means of a clamp. Thehead shall be of metal, preferably of copper or brass, and shallhave tube opening of 25.4 mm (1 in) of inside diameter tofacilitate attachment of the specified trap/con
7、denser assembly.4.2 Condenser, of the water-cooled reflux glass-tube type,having a condenser jacket not less than 400 mm (1534 in.) longwith an inner tube 9.5 to 12.7 mm (38 to12 in.) in outsidediameter. The end of the condenser inserted in the trap shall beground off at an angle of 30 from the vert
8、ical axis of thecondenser. For mixtures with very volatile solvents, it may benecessary to supplement this water-cooled condenser with asecond water-cooled condenser of approximately the samedimensions.4.3 Trap, of well-annealed glass, of one of the followingtypes depending upon the purpose of the t
9、est:4.3.1 For determination of water in bituminous pavingmixtures, a glass trap of 10 or 25-mL capacity shall be used.The trap shall be graduated in 0.1-mL divisions with60.05-mL maximum error below 1 mL, and in 0.2-mLdivisions with a 60.1-mL maximum error above 1 mL, asspecified in Table 1 and Fig.
10、 1, Fig. 2, Fig. 3, and Fig. 4.Tapered Ball traps require adaptors for connection to the metalstill.4.3.2 For determination of the volatile fractions of thebitumen, the trap shall conform to the dimensions shown inFig. 5.4.4 SolventFor general use, an aromatic solvent is pre-ferred, since it has hig
11、h solvency and dispersing power formost bituminous materials. Xylene, or a blend of 20 % tolueneand 80 % xylene, is recommended. For asphalts and similarpetroleum products, a petroleum distillate, 5 % boiling be-tween 90 and 100C, and 90 % distilling below 210C may beused. For coal-tar, water-gas ta
12、r, and similar materials, thearomatic solvent must be used.4.5 Heating Device Any satisfactory source of heat thatwill be capable of maintaining a rate of distillation of 85 to 95drops/min.1This test method is under the jurisdiction of ASTM Committee D04 on Roadand Paving Materials and is the direct
13、 responsibility of Subcommittee D04.25 onAnalysis of Bituminous Mixtures.Current edition approved Dec. 15, 2011. Published December 2011. Originallyapproved in 1956. Last previous edition approved in 2006 as D1461 85 (2006).DOI: 10.1520/D1461-11.2For referenced ASTM standards, visit the ASTM website
14、, 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 19428-2959, United States.
15、5. Sampling5.1 Sampling shall be carried out in accordance with theprocedures set forth in Test Methods D979.TABLE 1 Dimensions and Sizes of TrapsStyleDescriptionFigureSize ofTrap,mLRange, mLSmall-estScaleDivision,mLScaleErrormax, mLTop ofGraduatedTubeBottom ofGraduatedTubeBottom ofVaporTubeA $ join
16、t conical $ joint 7 100to 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.FIG. 1 Traps (Style A)NOTE 1All dimensions are
17、in millimetres.FIG. 2 Traps (Style B)D1461 1125.2 The sample shall be representative of the material andshall be of such size as practical to fill the container in whichit is transported to the laboratory. For duplicate tests a 1.9-L(12-gal) friction-top tin pail full of the material would besatisfa
18、ctory.6. Test Specimen and Sample6.1 Thoroughly mix the sample and weigh out an amountestimated to show a percentage of moisture or diluent withinthe capacity of the trap calibration. Keep the remainder of thesample in its tightly covered container. The weighed sampleshould be preferably not less th
19、an 500 g for normal mixtures.Thoroughly break up this sample to avoid larger lumps, andplace it in the still.7. Procedure for Determination of Moisture7.1 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 ap
20、paratus as illustratedin Fig. 6, choosing the trap in accordance with the expectedwater content of the sample and making all connections vaporand 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
21、 assure free drainage of waterinto the bottom of the trap. Insert a loose cotton plug in the tipof the condensor to prevent condensation of atmosphericmoisture 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
22、 after the heat has been applied and the condensersolvent will drip into the trap at a rate of 85 to 95 drops/min.Continue 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 distillation
23、continue for 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 Afte
24、r the sample 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 prescribedNOTE 1All dimensions are in millimetres.FIG. 3 Traps (Style C)NOTE 1A
25、ll dimensions are in millimetres.FIG. 4 Traps (Style D)D1461 113in 7.2, except that the gasket is moistened with solvent and thetrap used shall be 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
26、appliedand will drip from the condenser at the rate of 85 to 95 dropsper minute. In case the sample contains a large amount of veryvolatile solvent, it may be necessary to add a second water-cooled condenser above the first one or to reduce the rate ofdistillation somewhat to prevent escape of the s
27、olvent.8.3 Continue distillation until three successive readings ofthe upper and lower levels of the diluent at 15-min intervalsshow no increase in the quantity being collected. Then removethe source of heat and allow the trap and contents to reachroom temperature. Allow the trap to stand a minimum
28、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 described in9.2. Use the specific gravity of the diluent at 25C.9. Calculation9.1 Calculate the moisture content as follows:Water, % 5volume of water i
29、n trapweight of sample3 100 (1)9.2 Calculate the volatile distillate as follows:Diluent, % 5volume diluent in trap!sp gr diluent at 25C!weight of sample3 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
30、 the weight percentdiluent content in accordance with 9.2.NOTE 1Assume specific gravity of diluent based on knowledge ofdiluent type or values in the range of 0.85 to 0.90. This only definesvolatiles that are obtained at the maximum test temperature.11. Precision11.1 Precision for Determination of M
31、oistureThe follow-ing criteria should be used for judging the acceptability ofresults (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 Col
32、lected, mL0to1.0 0.1mL1.1 to 25 0.1 mL or 2 % of the mean,whichever is greater11.1.2 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,which
33、ever is greaterFIG. 5 Apparatus for Determining Volatile Fractions of the BitumenD1461 11411.2 Precision for Determination of Volatile DistillatesThe precision of this method as obtained by statistical exami-nation of interlaboratory test results is as follows:11.2.1 Repeatibility Duplicate determin
34、ations of volatiledistillates by the same operator should be considered suspect ifthey differ by more than 0.6 volume %.11.2.2 Reproducibility The results submitted 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 insi
35、de diameter.FIG. 6 Typical Assemblies with Metal StillD1461 115ASTM 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
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