1、Designation: D7403 09 (Reapproved 2017)Standard Test Method forDetermination of Residue of Emulsified Asphalt by Low-Temperature Vacuum Distillation1This standard is issued under the fixed designation D7403; the number immediately following the designation indicates the year oforiginal adoption or,
2、in the case of revision, the 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.1. Scope1.1 This method covers the quantitative determination ofresidue in emulsified asphalt
3、s composed principally of asemisolid or liquid asphaltic base, water, and an emulsifyingagent. The emulsified asphalts will generally contain polymericmaterials. It is especially suitable for emulsified asphalt residueproperties that may be altered at the high-temperature 260 C(500 F) distillation.
4、Since there is currently not a precisionstatement for this procedure, it is recommended to the user thatthis procedure not be used for buy/sell purposes at the presenttime.1.2 The values stated in SI units are to be regarded as thestandard. Values in parentheses in inch-pound units are pro-vided for
5、 informational purposes only.1.3 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 establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regula
6、tory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Org
7、anization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D6997 Test Method for Distillation of Emulsified AsphaltE1 Specification for ASTM Liquid-in-Glass Thermometers3. Significance and Use3.1 This test method can be used for quantitative determi-nation of res
8、idue in emulsified asphalts at a temperature of135 C (275 F) with a 60-min distillation test using currentdistillation apparatus. This method is suitable to obtain resi-dues for service evaluation, quality control, and research. Thisdistillation method is not intended to produce residues equiva-lent
9、 to the Test Method D6997 260 C (500 F) distillationprocedure.4. Apparatus4.1 Aluminum Alloy Still, conforming to Test MethodD6997 except that a 13-mm (12-in.) diameter hole is drilledbetween the two existing 13-mm (12-in.) thermometer holes forthe connection of a vacuum gauge (see Fig. 1). The join
10、tbetween the still and lid shall be airtight with the gasket inplace. Other heating devices may be used provided theyemploy the intended control of temperature during the distil-lation procedure.4.2 Connection Apparatus, Test Method D6997, with modi-fications as shown in Fig. 2. Connection tubing ma
11、y be ofsuitable materials provided the intended vacuum, temperature,and method are maintained. Other forms of condensers may beused provided they have an equivalent or greater interiorsurface area for condensation of distillate.NOTE 1Silicone rubber stoppers are recommended.4.3 Thermometric Device,
12、ASTM 7C (7F) thermometers, orthermocouple devices calibrated at 135 C (275 F). The ther-mocouple probe, Type T with exposed junction, should be ofsufficient length (approximately 300 mm (12 in.) to bepositioned approximately 6 mm (0.25 in.) off the bottom of theassembled still. Use of equivalent the
13、rmometric devices ispermitted.4.4 Balance, capable of weighing 3500 g to 60.1 g.4.5 Vacuum Pump, rotary vane type, capable of maintaininga vacuum of 88 kPa below gauge pressure or greater.NOTE 288 kPa below gauge pressure is equal to 26 in. Hg (660 mm)below atmospheric pressure.4.6 Gasket, of silico
14、ne rubber, 3 mm (18 in.) thick, cut to fitflanged opening on still. Other gasket materials may be usedprovided they withstand the maximum temperature reached1This test method is under the jurisdiction of ASTM Committee D04 on Roadand Paving Materials and is the direct responsibility of Subcommittee
15、D04.42 onEmulsified Asphalt Test.Current edition approved Oct. 1, 2017. Published October 2017. Originallyapproved in 2009. Last previous edition approved in 2009 as D7403 09. DOI:10.1520/D7403-09R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Servic
16、e at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in acc
17、ordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1during distillation and are ab
18、le to maintain the specifiedvacuum within the still.4.7 Vacuum Gauges, dial type or other suitable type con-nected to vacuum tubing and/or fittings to allow attachment toboth vacuum pump and to still apparatus and capable ofreading a minimum vacuum of 88 kPa below gauge pressure(660 mm or 26 in. Hg
19、below atmospheric pressure).4.8 Freezer, maintained at approximately 10 C.4.9 Disposable Plastic Drink Cups, of convenient size andmake to serve as a container during freezing of emulsifiedasphalt.5. Hazards5.1 WarningMercury has been designated by the UnitedStates Environmental Protection Agency (E
20、PA) and many stateagencies as a hazardous material that can cause central nervousFIG. 1 Aluminum Alloy Still Lid Showing Location of the Hole for Vacuum Gauge ConnectionFIG. 2 Connection Apparatus SchematicD7403 09 (2017)2system, kidney, and liver damage. Mercury, or its vapor, maybe hazardous to he
21、alth and corrosive to materials. Cautionshould be taken when handling mercury and mercury-containing products. See the applicable product MaterialSafety Data Sheet (MSDS) for details and the EPAs website(www.epa.gov/mercury/faq.htm) for additional information.Users should be aware that selling mercu
22、ry and/or mercury-containing products in your state may be prohibited by statelaw.6. Procedure6.1 Weigh 200 to 201 g of a representative sample of theemulsified asphalt into the disposable plastic drink cup. Placecup and sample in freezer until thoroughly frozen.NOTE 3Typically, 0.5 g of frozen emul
23、sion is lost in handling thefrozen emulsified asphalt. If the desired amount of frozen emulsifiedasphalt to be tested is 200.0 g, then weigh into the drink cup 200.5 g.6.2 Prepare still by inserting thermometer and thermocoupleprobe through size #00 rubber stoppers, and then into the13-mm (12-in.) h
24、oles provided for in the still cover. Adjust thethermometric device so the end is 6 mm (0.25 in.) from thebottom of the still. The bulb of the second thermometric deviceshould be adjusted to 165 mm (6.5 in.) from the bottom of thestill.6.3 Prepare the frozen emulsified asphalt sample by splittingedg
25、e of cup and partially peeling sides away from sample.Place frozen sample in previously weighed still apparatus(including lid, clamp, thermometric devices, stoppers, andgasket) and weigh to 0.1 g.6.4 Assemble apparatus and insert vacuum gauge withtubing and stopper attachment into the 13-mm (12-in.)
26、 holelocated between the thermometer holes. Immediately apply aminimum vacuum of 88 kPa below gauge (atmospheric) to thestill and contents. Maintain this vacuum throughout the distil-lation. The elapsed time from removing the sample from thefreezer to applying vacuum should not exceed 2 min.6.5 Afte
27、r 10 min, apply heat from a ring burner or othersuitable heating device. The ring burner at the beginning of theheating period shall be positioned around the still approxi-mately 200 mm (8 in.) from the bottom of the still. Also applya small amount of heat to the connecting tube from a Bunsenburner
28、or other suitable heating device. Other heating devicesmay require a different procedure to apply heat in the intendedmanner.NOTE 4The location of the ring burner or heating device at the startof the test is flexible.6.6 As the temperature rises to approximately 149 C(300 F) on the upper thermometri
29、c device, lower the burnerand continue heating until the lower thermocouple reads 135 65 C (275 6 10 F). This temperature should be achievedwithin 45 min of initially applying the heat.6.7 Maintain the temperature of the still contents at 135 65 C (275 6 10 F) for 15 min.NOTE 5Cooling of the outside
30、 of the still may be done to preventtemperature overshoot. This can be performed by application of water-soaked toweling momentarily applied to base of the still with dueprecaution.6.8 At the end of the heating period, immediately reweighthe still apparatus and residue. The aluminum alloy still atro
31、om temperature weighs 0.8 g more than at 135 C (275 F).Correct for this error by adding 0.8 g to the gross weight beforecalculating the percentage of residue by distillation. Recordresults.6.9 Remove the lid from the still and, if the residue issufficiently fluid, stir and transfer suitable portions
32、 of theresidue into molds or containers for further testing. If theresidue is not sufficiently fluid for pouring without the incor-poration of air, quickly heat the sample to the lowest tempera-ture at which this can be achieved. Record the pouringtemperature.7. Calculation7.1 Calculate the residue
33、content as follows:Emulsified asphalt residue, % 5SABD3100 (1)where:A = weight of residue, g, andB = weight of emulsified asphalt, g.8. Report8.1 Report the following information:8.1.1 Sample identification,8.1.2 Date of test,8.1.3 Pouring temperature,8.1.4 Emulsified asphalt residue weight percent,
34、 and8.1.5 Distillation test method.9. Precision and Bias9.1 PrecisionThe research necessary to report precisionhas not been conducted.9.2 BiasThe research necessary to report bias has not beenconducted.10. Keywords10.1 asphalt; distillation; emulsified asphalt; emulsion; low-temperature; vacuumD7403
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