1、Designation: D 6997 04Standard Test Method forDistillation of Emulsified Asphalt1This standard is issued under the fixed designation D 6997; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in par
2、entheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the quantitative determinationof residue and oil distillate in emulsified asphalts composedprincipally of a semisolid or li
3、quid asphaltic base, water, andan emulsifying agent.1.2 This test method 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 establish appro-priate safety and health practices and determine the applica-bility
4、 of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E 1 Specification for ASTM ThermometersE 11 Specification for Wire Cloth and Sieves for TestingPurposes3. Summary of Method3.1 A sample of emulsified asphalt is heated in analuminum-alloy still to 260 6 5C and the vol
5、umes of distillateand water obtained are measured. The residue from thedistillation, and also any oil portion of the distillate may betested as required.4. Significance and Use4.1 This test method can be used for quantitative determi-nation of residue and oil distillates in emulsified asphalts forsp
6、ecification acceptance, service evaluation, control, and re-search. This test method can also be used to obtain residue andoil distillate for further testing.5. Apparatus5.1 Aluminum-Alloy Stillapproximately 240 mm in heightby 95 mm in inside diameter with cover and clamp as shownin Fig. 1. A variet
7、y of gasket materials may be used to seal thestill providing they withstand the maximum temperaturereached during distillation.NOTE 1Residue by distillation results obtained with iron stills areacceptable.5.2 Heat Sourcesone ring burner, approximately 125 mminside diameter, having holes on the inner
8、 periphery and havingthree spacers, to ensure centering of burner around the still (seeFig. 2); one Bunsen burner equipped with optional wing tip asshown in Fig. 35.3 Connection Apparatusconsisting of a 12.5 6 0.5 mmglass or metal connecting tube, tin shield (as detailed in Fig. 3),and a water-coole
9、d glass condenser tube with a metal or1This test method is under the jurisdiction of ASTM Committee D04 on Roadand Paving Materials and is the direct responsibility of Subcommittee D04.42 onEmulsified Asphalt Tests.Current edition approved Aug. 1, 2004. Published August 2004.2For referenced ASTM sta
10、ndards, 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.FIG. 1 Aluminum-Alloy Still1Copyright ASTM International, 100 Barr Harbor Drive, PO B
11、ox C700, West Conshohocken, PA 19428-2959, United States.borosilicate glass jacket. The metal connecting tube may besecured to the lid by a threaded compressing fitting. Glassconnecting tube may be secured to the lid by means of a corkor silicone stopper. Other condensers of 12.5 6 0.5 mm glassor me
12、tal tubing may be used, providing that the wetted lengthis 400 to 550 mm.5.4 Graduated Cylinder100-mL, with graduation inter-vals of 1.0 mL.5.5 ThermometerASTM 7C thermometer, as prescribedin Specification E 1, or any other thermometric device of equalaccuracy.5.6 Balancecapable of weighing 3500 g t
13、o within 60.1 g.5.7 StoppersCork (wrapped in foil) or silicone stoppers toseal holes in still cover, maintain temperature measuring deviceposition, and secure connecting tube to still cover.5.8 Rubber Tubingheat resistant tubing of adequate sizeto secure glass to glass joint of connecting tube and c
14、ondenser.5.9 SieveA sieve having a 76.2-mm frame conforming toSpecification E 11, and having a 300-m wire sieve cloth.NOTE 2For details of the assembly of apparatus for the distillationtest, see Fig. 3.6. Sample Conditioning for Testing6.1 All emulsified asphalts shall be properly stirred toachieve
15、homogeneity before testing.6.2 All emulsified asphalts with viscosity testing require-ments of 50C shall be heated to 50 6 3C in the originalsample container in a water bath or oven. The container shouldbe vented to relieve pressure. After the sample reaches 50 63C, stir the sample to achieve homoge
16、neity.6.3 Emulsified asphalts with viscosity testing requirementsof 25C should be mixed or stirred at 25 6 3C in the originalsample container to achieve homogeneity.NOTE 3Emulsified asphalts with viscosity testing requirements of25C may be heated and stirred as specified in 6.2, if necessary. In the
17、event the 6.2 method is used, the sample should be cooled to 25 6 3Cbefore testing.7. Procedure7.1 Weigh 200 6 0.1 g of a representative sample of theemulsified asphalt in the previously weighed aluminum-alloystill (including lid, clamp, temperature measuring device, smallstopper, and gasket, if gas
18、ket is used).FIG. 2 Ring Burner with 125-mm Inside DiameterFIG. 3 Apparatus Assembly for Distillation Test of Emulsified AsphaltsD69970427.2 Use a gasket of suitable material between the still and itscover, or grind the joint to a tight fit. Securely clamp the coveron the still.7.3 Insert a thermome
19、ter, or other thermometric device,through a cork or silicone stopper, in one of the small holesprovided in the cover, seal the other hole with a cork or siliconestopper. Adjust the temperature measuring device so that theend of the bulb is approximately 6 mm from the bottom of thestill.NOTE 4A secon
20、d temperature measuring device may be used in thesecond small hole, with the bulb placed approximately 165 mm from thebottom of the still. A sudden change in temperature reading of uppertemperature measuring device indicates foam on bulb. Remove heat untilfoaming ceases.7.4 Place the ring burner aro
21、und the still about 150 mmfrom the bottom of the still. Apply heat by lighting this burnerand adjusting to low flame. Also apply just enough heat froma bunsen burner to the connecting tube to prevent condensationof water in this tube.7.5 When the temperature can be read on the thermometer,or at appr
22、oximately 215C, move the ring burner approxi-mately level with the bottom of the still. Increase the tempera-ture to 260 6 5C, maintaining it at this temperature for 15min. Complete the total distillation in 60 6 15 min from thefirst application of heat.NOTE 5The location of the burner at the start
23、of the test is flexible. Itmay be raised to decrease chance of foam-over or lowered to middle ofstill for emulsion containing no solvent. The ring burner may be graduallylowered as the distillation proceeds to ensure that the time requirements ofthis test method are satisfied.7.6 Immediately at the
24、expiration of the heating period,again weigh the still and accessories as described in 7.1. Thealuminum-alloy still at ambient temperature (7.1) weighs 1.5 gmore than at 260C. Correct for this error by adding 1.5 g togross weight obtained prior to calculating the percentage ofresidue by distillation
25、. Calculate and report the percentageresidue by distillation. Record the volume of oil distillate to thenearest 0.5 ml. Calculate and report the oil distillate as avolume percentage of the total emulsified asphalt.NOTE 6For purposes of this test result calculation, assume a 1:1 massto volume relatio
26、nship of distillate to emulsified asphalt.7.7 Remove the cover from the still, stir, and immediatelypour suitable portions of the residue into a container or suitablemolds for making any required tests. If there is foreign matterin the residue, the material shall be poured through a 300-mmsieve prio
27、r to pouring into the test molds and containers.8. Calculation8.1 Calculate the percentage of reside in the sample asfollows:Sample residue, % 5 B 2 A!/C! 3 100 (1)where:A = weight of empty still (7.1) assembly before test, g, andB = weight of still assembly (7.6) after test (with added 1.5g), g, an
28、dC = weight of emulsified asphalt added to still, g.9. Report9.1 Report the percentage of residue in the sample.10. Precision and Bias10.1 The following criteria should be used for judging theacceptability of results (95 % probability):10.1.1 Duplicate results by the same operator should not beconsi
29、dered suspect unless they differ by more than the follow-ing amount:Residue by Repeatability, weight %Distillation, weight %50 to 70 1.010.1.2 The results submitted by each of two laboratoriesshould not be considered suspect unless they differ by morethan the following amount:Residue by Repeatabilit
30、y, weight %Distillation, weight %50 to 70 2.010.2 The bias of this test method cannot be determinedbecause no material having an accepted reference value isavailable11. Keywords11.1 asphalt emulsion; cationic emulsified asphalt; distilla-tion; emulsified asphalt; residueASTM International takes no p
31、osition 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 patent rights, and the riskof infringement of such rights, are entirely their own responsib
32、ility.This standard is subject to revision at any time by the responsible technical 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
33、ASTM International Headquarters. Your comments will receive careful consideration 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 addre
34、ss shown below.This standard is copyrighted by ASTM International, 100 Barr 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(www.astm.org).D6997043
