1、Designation: D1461 11D1461 17Standard Test Method forMoisture or Volatile Distillates in Bituminous Paving AsphaltMixtures1This 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, t
2、he year of last 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 U.S. Department of Defense.1. Scope1.1 This test method cove
3、rs the determination, by direct measurement, of moisture or volatile fractions of the bitumenasphaltin bituminous paving asphalt mixtures.1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.Noother units of measurement are in
4、cluded in this standard.1.3 The text of this standard references notes and footnotes which provide explanatory material. These notes and footnotes(excluding those in tables and figures) shall not be considered as requirements of the standard.1.4 This standard does not purport to address all of the s
5、afety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.1.5 This international standard was developed in accordance with internatio
6、nally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D979D979/D97
7、9M Practice for Sampling Bituminous Paving MixturesD3666 Specification for Minimum Requirements for Agencies Testing 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 the amount o
8、f moisture or the amount of volatile petroleum distillates inbituminous paving asphalt mixtures.3.2 Applicable standards are those in which measurements or calibrations are made, samples are procured, or products areselected.34. Apparatus4.1 Metal StillA vertical cylindrical still, similar to that u
9、sed in Test MethodsMethod D6997, having a faced flange at the topto which the head is tightly attached by means of a clamp. The head shall be of metal, preferably of copper or brass, and shall havea tube opening of 25.4 mm (1 in) of inside diameter to facilitate attachment of the specified trap/cond
10、enser assembly.1 This test method is under the jurisdiction of ASTM Committee D04 on Road and Paving Materials and is the direct responsibility of Subcommittee D04.25 on Analysisof Asphalt Mixtures.Current edition approved Dec. 15, 2011June 1, 2017. Published December 2011June 2017. Originally appro
11、ved in 1956. Last previous edition approved in 20062011 asD1461 85 (2006).D1461 11. DOI: 10.1520/D1461-11.10.1520/D1461-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, ref
12、er to the standards Document Summary page on the ASTM website.3 The quality of the results produced by this standard are dependent on the competence of the personnel performing the procedure and the capacity, calibration, andmaintenance of the equipment used. Agencies that meet the criteria of Speci
13、fication D3666 are generally considered capable of competent and objective testing, sampling,inspection, etc. Users of this standard are cautioned that compliance with Specification D3666 alone does not completely ensure reliable results. Reliable results depend onmany factors; following the suggest
14、ions of Specification D3666 or some similar acceptable guideline provides a means of evaluating and controlling some of those factors.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous versio
15、n. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International
16、, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.2 Condenser, of the water-cooled reflux glass-tube type, having a condenser jacket not less than 400 mm (15 34 in.) long withan inner tube 9.5 to 12.7 mm (38 to 12 in.) in outside diameter. The end of the condens
17、er inserted in the trap shall be ground offat an angle of 30 from the vertical axis of the condenser. For mixtures with very volatile solvents, it may be necessary tosupplement this water-cooled condenser with a second water-cooled condenser of approximately the same dimensions.4.3 Trap, of well-ann
18、ealed glass, of one of the following types depending upon the purpose of the test:4.3.1 For determination of water in bituminous paving asphalt mixtures, a glass trap of 1010- or 25-mL capacity shall be used.The trap shall be graduated in 0.1-mL divisions with 60.05-mL maximum error below 1 mL, and
19、in 0.2-mL divisions with a60.1-mL maximum error above 1 mL, as specified in Table 1 and Fig. 1Figs. 1-4, Fig. 2, Fig. 3, and Fig. 4. Tapered Ballball trapsrequire adaptors for connection to the metal still.4.3.2 For determination of the volatile fractions of the bitumen,asphalt, the trap shall confo
20、rm to the dimensions shown in Fig.5.4.4 SolventFor general use, an aromatic solvent is preferred, since it has high solvency and dispersing power for mostbituminousasphalt materials. Xylene, or a blend of 20 % toluene and 80 % xylene, is recommended. For asphalts and similarpetroleum products, a pet
21、roleum distillate, 5 % boiling between 90 and 100C,100 C, and 90 % distilling below 210C210 C maybe used. For coal-tar, coal tar, water-gas tar, and similar materials, the aromatic solvent must be used.4.5 Heating Device Any satisfactory source of heat that will be capable of maintaining a rate of d
22、istillation of 85 to 9595 dropsdrops/min.min.5. Sampling5.1 Sampling shall be carried out in accordance with the procedures set forth in Test MethodsMethod D979D979/D979M.5.2 The sample shall be representative of the material and shall be of such size as practical to fill the container in which it i
23、stransported to the laboratory. For duplicate tests, a 1.9-L (12-gal) friction-top tin pail full of the material would be satisfactory.6. Test Specimen and Sample6.1 Thoroughly mix the sample and weigh out an amount estimated to show a percentage of moisture or diluent within thecapacity of the trap
24、 calibration. Keep the remainder of the sample in its tightly covered container. The weighed sample should bepreferably not less than 500 g for normal mixtures. Thoroughly break up this sample to avoid larger lumps, and place it in the still.7. Procedure for Determination of Moisture7.1 After the sa
25、mple has been placed in the still, add 200 mL of the solvent and quickly stir it into the sample.7.2 Assemble the components of the apparatus as illustrated in Fig. 6, choosing the trap in accordance with the expected watercontent of the sample and making all connections vapor and liquid tight. Inse
26、rt a gasket of heavy paper, moistened with waterbetween the still body and cover. The condenser tube and trap must be chemically clean to assureensure free drainage of waterinto the bottom of the trap. Insert a loose cotton plug in the tip of the condensorcondenser to prevent condensation of atmosph
27、ericmoisture inside it. Circulate cold water through the jacket of the condenser.7.3 Apply heat at such a rate that refluxing will start within 5 to 10 min after the heat has been applied and the condenser solventwill drip into the trap at a rate of 85 to 95 drops/min. Continue the distillation unti
28、l three successive readings of the trap at 15-minintervals show no increase in the amount of water being condensed, except that in no case shall distillation continue for more than112 h.7.4 Allow the contents of the trap to reach room temperature and read the volume of water in the trap to the neare
29、st scaledivision. Record the volume of water and calculate in weight percent as described in 9.1.TABLE 1 Dimensions and Sizes of TrapsStyleDescriptionFigureSize ofTrap,mLRange, mLSmall-estScaleDivision,mLScaleErrormax, mLTop ofGraduatedTubeBottom ofGraduatedTubeBottom ofVaporTubeA $ joint conical $
30、joint 7 100 to 1.0over 1.0 to 10.00.10.20.050.1BCD joint$ jointplainconicalconicalconical jointplainplain8910 250 to 1.0over 1.0 to 250.10.20.050.1E $ joint round $ joint 115100 to 5.00 to 10.00.10.10.050.1D1461 1728. Procedure for Determination of Volatile Distillates8.1 After the sample has been p
31、laced in the still, add 350 mL of water and approximately 3 g of sodium carbonate (Na2CO3)and quickly stir into the sample. Firmly attach the still cover and assemble the trap and condenser in the manner prescribed in 7.2,except that the gasket is moistened with solvent and the trap used shall be th
32、e dilution trap specified in 4.3.2.NOTE 1All dimensions are in millimetres.FIG. 1 TrapsTraps (Style A)NOTE 1All dimensions are in millimetres.FIG. 2 TrapsTraps (Style B)NOTE 1All dimensions are in millimetres.FIG. 3 TrapsTraps (Style C)D1461 1738.2 Apply heat at such a rate that the water and solven
33、t will begin to reflux in 5 to 10 min after the heat has been applied andwill drip from the condenser at the rate of 85 to 9595 drops drops per minute. min. In case the sample contains a large amountof very volatile solvent, it may be necessary to add a second water-cooled condenser above the first
34、one or to reduce the rate ofdistillation somewhat to prevent escape of the solvent.8.3 Continue distillation until three successive readings of the upper and lower levels of the diluent at 15-min intervals showno increase in the quantity being collected. Then remove the source of heat and allow the
35、trap and contents to reach roomtemperature. Allow the trap to stand a minimum of 12 h to permit the solvent to separate.NOTE 1All dimensions are in millimetres.FIG. 4 TrapsTraps (Style D)FIG. 5 Apparatus Apparatus for Determining Volatile Fractions of the BitumenAsphaltD1461 1748.4 Record the volume
36、 of diluent in the trap to the nearest scale division and calculate in weight percent as described in 9.2.Use the specific gravity of the diluent at 25C.25 C.9. Calculation9.1 Calculate the moisture content as follows:Water,%5volume of water in trapweight of sample 3100 (1)9.2 Calculate the volatile
37、 distillate as follows:Diluent,%5volume diluent in trap!sp gr diluent at 25C!weight of sample 3100 (2)Diluent,%5volume diluent in trap!sp gr diluent at 25 C!weight of sample 3100 (2)NOTE 1Trap shall be 15 to 16 mm in inside diameter.FIG. 6 TypicalTypical Assemblies with Metal StillD1461 17510. Repor
38、t10.1 Report the moisture content as the weight percent water content in accordance with 9.1.10.2 Report the volatile distillates as the weight percent diluent content in accordance with 9.2.NOTE 1Assume specific gravity of diluent based on knowledge of diluent type or values in the range of 0.85 to
39、 0.90. This only defines volatiles thatare obtained at the maximum test temperature.11. Precision11.1 Precision for Determination of MoistureThe following criteria should be used for judging the acceptability of results(95 % probability) when using the 10-mL or 25-mL traps.11.1.1 RepeatabilityDuplic
40、ate determination of water by the same operator should be considered suspect if they differ by morethan the following amounts:Water Collected, mL0 to 1.0 0.1 mL1.1 to 25 0.1 mL or 2 % of the mean,whichever is greater11.1.2 ReproducibilityThe results submitted by each of two laboratories should be co
41、nsidered suspect if they differ by morethan the following amounts:Water Collected, mL0 to 1.0 0.2 mL1.1 to 25 0.2 mL or 10 % of the mean,whichever is greater11.2 Precision for Determination of Volatile DistillatesThe precision of this method as obtained by statistical examination ofinterlaboratory t
42、est results is as follows:11.2.1 RepeatibilityDuplicate determinations of volatile distillates by the same operator should be considered suspect if theydiffer by more than 0.6 volume %.11.2.2 ReproducibilityThe results submitted by each of two laboratories should be considered suspect if they differ
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