1、Designation: D 7403 09Standard Test Method forDetermination of Residue of Emulsified Asphalt by LowTemperature Vacuum Distillation1This standard is issued under the fixed designation D 7403; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, 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 asphalts composed princi
3、pally 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 260C(500F) distillation. Since there is curr
4、ently 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 informational purp
5、oses 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 and health practices and determine the applica-bility of regulatory limitations prior to use.2. Re
6、ferenced Documents2.1 ASTM Standards:2D 6997 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 residue in emulsified asphalts at a temperature of135C (275F
7、) with a 60 minute 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 to the Test Method D 6997 260C (500F) distillationproce
8、dure.4. Apparatus4.1 Aluminum Alloy Still, conforming to Test MethodD 6997 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 jointbetween the still and lid shall be air tight with the g
9、asket 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 D 6997, with modi-fications as shown in Fig. 2. Connection tubing may be ofsuitable materials provided the intended vacuum
10、, temperature,and method is 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, ASTM 7C (7F) thermometers, orthermocouple devices calib
11、rated at 135C (275F). 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 thermometric devices ispermitted.4.4 Balance, capable of wei
12、ghing 3500 grams to 6 0.1gram.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 silicone rubber, 3 mm (18 in.) thick, cut to fitflanged
13、opening on still. Other gasket materials may be usedprovided they withstand the maximum temperature reachedduring distillation and are able to maintain the specifiedvacuum within the still.1This test method is under the jurisdiction of ASTM Committee D04 on Roadand Paving Materials and is the direct
14、 responsibility of Subcommittee D04.42 onEmulsified Asphalt Test.Current edition approved June 1, 2009. Published July 2009.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, r
15、efer 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.4.7 Vacuum Gauges, dial type or other suitable type con-nected to vacuum tubing and/or fittings to allow attachment toboth
16、 vacuum pump and to still apparatus and capable ofreading a minimum vacuum of 88 kPa below gauge pressure(660 mm or 26 in. Hg below atmospheric pressure).4.8 Freezer, maintained at approximately 10C.4.9 Disposable Plastic Drink Cups, of convenient size andmake to serve as a container during freezing
17、 of emulsifiedasphalt.5. Hazards5.1 WarningMercury has been designated by the UnitedStates Environmental Protection Agency (EPA) and many stateagencies as a hazardous material that can cause central nervoussystem, kidney and liver damage. Mercury, or its vapor, may behazardous to health and corrosiv
18、e to materials. Caution shouldbe taken when handling mercury and mercury containingproducts. See the applicable product Material Safety DataSheet (MSDS) for details and EPAs website (www.epa.gov/FIG. 1 Aluminum Alloy Still Lid Showing Location of the Hole for Vacuum Gauge ConnectionFIG. 2 Connection
19、 Apparatus SchematicD7403092mercury/faq.htm) for additional information. Users should beaware that selling mercury and/or mercury containing productsinto your state may be prohibited by state law.6. Procedure6.1 Weigh 200 to 201 grams of a representative sample ofthe emulsified asphalt into the disp
20、osable plastic drink cup.Place cup and sample in freezer until thoroughly frozen.NOTE 3Typically 0.5 grams of frozen emulsion is lost in handling thefrozen emulsified asphalt. If the desired amount of frozen emulsifiedasphalt to be tested is 200.0 grams then weigh into the drink cup 200.5grams.6.2 P
21、repare still by inserting thermometer and thermocoupleprobe through size #00 rubber stoppers, and then into the 13mm (12 in.) holes 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 deviceshou
22、ld be adjusted to 165 mm (6.5 in.) from the bottom of thestill.6.3 Prepare the frozen emulsified asphalt sample by splittingedge of cup and partially peeling sides away from sample.Place frozen sample in previously weighed still apparatus(including lid, clamp, thermometric devices, stoppers, andgask
23、et) and weigh to 0.1 gram.6.4 Assemble apparatus and insert vacuum gauge withtubing and stopper attachment into the 13 mm (12 in.) holelocated between the thermometer holes. Immediately apply aminimum vacuum of 88 kPa below gauge (atmospheric) to thestill and contents. Maintain this vacuum throughou
24、t the distil-lation. The elapsed time from removing the sample from thefreezer to applying vacuum should not exceed two minutes.6.5 After 10 minutes apply heat from a ring burner or othersuitable heating device. The ring burner at the beginning of theheating period shall be positioned around the sti
25、ll 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 or other suitable heating device. Other heating devicesmay require a different procedure to apply heat in the intendedmanner.NOTE 4The location of the ring burne
26、r or heating device at the startof the test is flexible.6.6 As the temperature rises to approximately 149C(300F) on the upper thermometric device, lower the burnerand continue heating until the lower thermocouple reads 135 65C (275 6 10F). This temperature should be achieved within45 minutes of init
27、ially applying the heat.6.7 Maintain the temperature of the still contents at 135 65C (275 6 10F) for 15 minutes.NOTE 5Cooling of the outside of the still may be done to preventtemperature overshoot. This can be performed by application of watersoaked toweling momentarily applied to base of the stil
28、l with dueprecaution.6.8 At the end of the heating period immediately reweighthe still apparatus and residue. The aluminum alloy still atroom temperature weighs 0.8 grams more than at 135C(275F). Correct for this error by adding 0.8 grams to the grossweight before calculating the percentage of resid
29、ue by distil-lation. Record results.6.9 Remove the lid from the still and if the residue issufficiently fluid, stir, and transfer suitable portions of theresidue into molds or containers for further testing. If theresidue is not sufficiently fluid for pouring without the incor-poration of air, quick
30、ly heat the sample to the lowest tempera-ture at which this can be achieved. Record the pouringtemperature.7. Calculation7.1 Calculate the residue content as follows:Emulsified asphalt residue, % 5SABD3 100 (1)where:A = weight of residue, grams, andB = weight of emulsified asphalt, grams.8. Report8.
31、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, and8.1.5 Distillation test method.9. Precision and Bias9.1 PrecisionThe research necessary to report precisionhas not been conducted.9.2 BiasTh
32、e research necessary to report bias has notbeen conducted.10. Keywords10.1 asphalt; distillation; emulsified asphalt; emulsion; low-temperature; vacuumD7403093ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this stand
33、ard. 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 responsibility.This standard is subject to revision at any time by the responsible technical committee and must be review
34、ed 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 ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible
35、 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 address 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).D7403094
