1、Designation:D699704 Designation: D6997 12Standard Test Method forDistillation of Emulsified Asphalt1This standard is issued under the fixed designation D6997; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. 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 quantitative determination of residue and oil distillate in emulsified asphalts composedprincipally of
3、 a semisolid or liquid asphaltic base, water, and an emulsifying agent.1.21.2 The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.1.3 This test method does not purport to address all of the safety concerns, if any, associated
4、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.2. Referenced Documents2.1 ASTM Standards:2E1 Specification for ASTM Liquid-in-Glass Thermometers E11Specifica
5、tion for Woven Wire Test Sieve Cloth and Test SievesE11 Specification for Woven Wire Test Sieve Cloth and Test SievesD7403 Test Method for Determination of Residue of Emulsified Asphalt by Low Temperature Vacuum DistillationD7497 Practice for Recovering Residue from Emulsified Asphalt Using Low Temp
6、erature Evaporative Technique3. Summary of Method3.1 A sample of emulsified asphalt is heated in an aluminum-alloy still to 260 6 5C and the volumes of distillate and waterobtained are measured. The residue from the distillation, and also any oil portion of the distillate, may be tested as required.
7、4. Significance and Use4.1This test method can be used for quantitative determination of residue and oil distillates in emulsified asphalts forspecification acceptance, service evaluation, control, and research. This test method can also be used to obtain residue and oildistillate for further testin
8、g.4.1 This test method can be used for quantitative determination of residue and oil distillates in emulsified asphalts forspecification acceptance, service evaluation, control, and research. This test method can also be used to obtain residue and oildistillate for further testing. This method may n
9、ot be appropriate for emulsified asphalts containing latex or polymer, however somespecifying agencies may utilize this method and stipulate a lowered distillation temperature. By stipulating a lowered distillationtemperature, the precision and bias statement may not be considered valid. Low tempera
10、ture methods such as Test Method D7403and Practice D7497 are options for obtaining residue for latex or polymer modified emulsified asphalts.5. Apparatus5.1 Aluminum-Alloy Stillapproximately 240241 mm in height by 95 mm in inside diameter with cover and clamp as shownin Fig. 1. A variety of gasket m
11、aterials may be used to seal the still providing they withstand the maximum temperature reachedduring distillation. . The dimensions as noted in Fig. 1 are provided as reference for the ease of the user and are considerednoncritical dimensions.NOTE 1Residue by distillation results obtained with iron
12、 stills are acceptable.5.2 Gasket a variety of gasket materials may be used to seal the still providing they withstand the maximum temperaturereached during distillation.1This test method is under the jurisdiction ofASTM Committee D04 on Road and Paving Materials and is the direct responsibility of
13、Subcommittee D04.42 on EmulsifiedAsphalt Tests.Current edition approved Aug. 1, 2004. Published August 2004. DOI: 10.1520/D6997-04.on Emulsified Asphalt Test.Current edition approved Feb. 1, 2012. Published February 2012. Last previous version published 2004 as D699704. DOI: 10.1520/D6997-12.2For re
14、ferenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.1This document is not an ASTM standard and is intended only to pro
15、vide the user of an ASTM standard an indication of what changes have been made to the previous version. 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
16、 standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.NOTE 2Use of a gasket is optional if the joint can be ground to a tight fit or only residue recovery is required
17、and further analysis on the water oroil distillate is not needed.5.3 Heat Sourcesone ring burner, approximately 125 mm inside diameter, having holes on the inner periphery and havingthree spacers, to ensure centering of burner around the still (see having holes on the inner periphery and having thre
18、e spacers,to ensure centering of burner around the still (see Fig. 2); one Bunsen burner equipped with optional wing tip as shown in ). Thedimensions as noted in Fig. 2 are provided for reference for the ease of the user and are considered non-critical dimensions.NOTE 3Optional use of a Bunsen burne
19、r (equipped with optional wing tip) as shown in Fig. 35.3.5.4 Connection Apparatusconsisting of a 12.5 6 0.5approximately 12 mm glass or metal connecting tube, tin shield (asdetailed in Fig. 3), and a water-cooled glass condenser tube with a metal or borosilicate glass jacket. The metal connecting t
20、ubeFIG. 1 Aluminum-Alloy StillFIG. 2 Ring Burner with 125-mm Inside DiameterD6997 122may be secured to the lid by a threaded compressing fitting. Glass connecting tube may be secured to the lid by means of a corkor silicone stopper. Other condensers of 12.5 6 0.5 approximately 12 mm glass or metal t
21、ubing may be used, providing that thewetted length is 400 to 550 mm. The dimensions as noted in Fig. 3 are provided for reference for the ease of the user and areconsidered non-critical dimensions.5.45.5 Graduated Cylinder100-mL, with graduation intervals of 1.0 mL.5.55.6 ThermometerASTM 7C thermome
22、ter, as prescribed in Specification E1, or any other thermometric device of equalaccuracy.5.65.7 Balancecapable of weighing 3500 g to within 60.1 g.5.75.8 StoppersCork (wrapped in foil) or silicone stoppers to seal holes in still cover, maintain temperature measuring deviceposition, and secure conne
23、cting tube to still cover.5.85.9 Rubber Tubingheat resistant tubing of adequate size to secure glass to glass joint of connecting tube and condenser.5.95.10 SieveA sieve having a 76.2-mm frame conforming to Specification E11, and having a 300-m wire sieve cloth. 300micron sieve to capture foreign ma
24、terials when suspected.NOTE2For 4For details of the assembly of apparatus for the distillation test, see Fig. 3.6. Sample Conditioning for Testing6.1 All emulsified asphalts shall be properly stirred to achieve homogeneity before testing.6.2 All emulsified asphalts with viscosity testing requirement
25、s of 50C shall be heated to 50 6 3C in the original samplecontainer in a water bath or oven. The container should be vented to relieve pressure. After the sample reaches 50 6 3C, stir thesample to achieve homogeneity.6.3Emulsified asphalts with viscosity testing requirements of 25C should be mixed o
26、r stirred at 25 6 3C in the original samplecontainer to achieve homogeneity.6.3 Emulsified asphalts with viscosity testing requirements of 25C shall be conditioned to 25 6 3C in the original samplecontainer to achieve homogeneity. After the sample reaches 25 6 3C, stir the sample to achieve homogene
27、ity.NOTE 35Emulsified asphalts with viscosity testing requirements of 25C may be heated and stirred as specified in 6.2, if necessary. In the event the, if necessary.6.4 Emulsified asphalts presented for testing from a storage tank may be tested at the storage tank temperature. Conditioningas in 6.2
28、 method is used, the sample should be cooled to 25 6 3C before testing. and 6.3 is not required.FIG. 3 Apparatus Assembly for Distillation Test of Emulsified AsphaltsD6997 1237. Procedure7.1 Weigh 200 6 0.1 g of a representative sample of the emulsified asphalt in the previously weighed aluminum-all
29、oy still(including lid, clamp, temperature measuring device, small stopper, and gasket, if gasket is used).7.2Use a gasket of suitable material between the still and its cover, or grind the joint to a tight fit. Securely clamp the cover onthe still.7.3Insert a thermometer, or other thermometric devi
30、ce, through a cork or silicone stopper, in one of the small holes providedin the cover, seal the other hole with a cork or silicone stopper. Adjust the temperature measuring device so that the end of thebulb is approximately 6 mm from the bottom of the still. Determine the mass of the aluminum-alloy
31、 still. Include in thisdetermination the still, cover, clamp, temperature measuring device(s), small stopper (if used) and gasket (if used).7.2 Add 200 +/- 1.0 g of a representative sample of the emulsified asphalt. Record this mass.NOTE4A second temperature measuring device may be used in the secon
32、d small hole, with the bulb placed approximately 165 mm from the bottomof the still. A sudden change in temperature reading of upper temperature measuring device indicates foam on bulb. Remove heat until foaming ceases.7.4Place the ring burner around the still about 150 mm from the bottom of the sti
33、ll. Apply heat by lighting this burner andadjusting to low flame. Also apply just enough heat from a bunsen burner to the connecting tube to prevent condensation of waterin this tube.7.5When the temperature can be read on the thermometer, or at approximately 215C, move the ring burner approximately
34、levelwith the bottom of the still. Increase the temperature to 260 6 5C, maintaining it at this temperature for 15 min. Complete thetotal distillation in 60 6 15 min from the first application of heat. 6If additional residue is needed for further testing, the samplesize may be increased. A total sam
35、ple mass between 200 to 300 g will be considered acceptable. This mass must be recorded andused in calculations 8.1 and 8.2 The precision data of this method was developed using 200 g samples and may not apply to othersample sizes.7.3 Securely clamp the cover on the still. If a gasket is used, inser
36、t between the still and the cover prior to clamping.7.4 Insert the temperature measuring device first through a cork or silicone stopper, and then in one of the small holes providedin the cover. Seal the other hole with a cork or silicone stopper. Adjust the temperature measuring device so that the
37、end of theprobe or bulb is approximately 6 mm from the bottom of the still.NOTE5The location of the burner at the start of the test is flexible. It may be raised to decrease chance of foam-over or lowered to middle of stillfor emulsion containing no solvent. The ring burner may be gradually lowered
38、as the distillation proceeds to ensure that the time requirements of thistest method are satisfied.7.6Immediately at the 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 g more than at 260C. C
39、orrect for this error by adding 1.5 g to grossweight obtained prior to calculating the percentage of residue by distillation. Calculate and report the percentage residue bydistillation. Record the volume of oil distillate to the nearest 0.5 ml. Calculate and report the oil distillate as a volume per
40、centageof the total emulsified asphalt. 7A second temperature measuring device may be used in the second small hole, with the probeor bulb placed approximately 165 mm from the bottom of the still. A sudden change in temperature reading of upper temperaturemeasuring device indicates foaming. Remove h
41、eat until foaming ceases.7.5 Place the ring burner around the still approximately 150 mm from the bottom of the still. Apply heat by lighting this burnerand adjusting to low flame.Also apply just enough heat from bunsen burner to the connecting tube to prevent condensation of waterin this tube.NOTE6
42、For purposes of this test result calculation, assume a 1:1 mass to volume relationship of distillate to emulsified asphalt.7.7Remove the cover from the still, stir, and immediately pour suitable portions of the residue into a container or suitable moldsfor making any required tests. If there is fore
43、ign matter in the residue, the material shall be poured through a 300-mm sieve priorto pouring into the test molds and containers. 8Use of the Bunsen burner is optional.7.6 When the temperature reaches approximately 215C, move the ring burner approximately level with the bottom of the still.Increase
44、 the temperature to 260 6 5C, maintaining it at this temperature for 15 min. Complete the total distillation in 60 6 15min from the first application of heat.NOTE 9The ring burner may be raised to decrease chance of foam-over or lowered to the middle of still for emulsified asphalts containing no so
45、lvent.The ring burner may be gradually lowered as the distillation proceeds to ensure that the time requirements of this test method are satisfied. It is alsoacceptable to incorporate 2 ring burners rather than moving a single ring burner. If a secondary ring burner is used, only one ring burner is
46、to be operationalat any given point during the distillation.7.7 Immediately at the expiration of the heating period, turn off the flame and again weigh the still and accessories as describedin 7.1. The aluminum-alloy still at ambient temperature (7.1) weighs 1.5 g more than at 260C. Correct for this
47、 error by adding1.5 g to gross weight obtained prior to calculating the percentage of residue by distillation. Calculate per 8.1 and report thepercentage residue by distillation. Record the volume of oil distillate to the nearest 0.5 mL. Calculate per 8.2 and report the oildistillate as a volume per
48、centage of the total emulsified asphalt based upon the sample weight as recorded in 7.2.7.8 Stir the still contents by gently agitating the residue. This may be done using a swirling motion or stirring with a long glassor steel rod to obtain consistent material prior to pouring. Remove the cover fro
49、m the still and immediately pour suitable portionsof the residue into a container or molds required for residue testing. If there is foreign matter suspected in the residue, pour theD6997 124material through a sieve prior to pouring into the test molds and container(s).8. Calculation8.1 Calculate the percentage of residue in the sample as follows:Sample residue, % 5 B 2 A!/C! 3 100 (1)D6997-12_1where:A = weightmass of empty still (7.1) assembly before test, g, andB = weightmass of still assembly (7.67.7) after test (with added 1.5 g),
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