1、Designation: D4957 18Standard Test Method forApparent Viscosity of Asphalt Emulsion Residues and Non-Newtonian Asphalts by Vacuum Capillary Viscometer1This standard is issued under the fixed designation D4957; 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 test method describes procedures primarily de-signed to determine the appa
3、rent viscosities of residues ob-tained by distilling asphalt emulsions according to Test MethodD6997. It is also recommended for use on non-Newtonianasphalts at any temperature within the capability of theapparatus. This test method is useful in characterizing rheo-logical properties of non-Newtonia
4、n asphalts as a function ofshear rate under the conditions of the test method. This test isrun in straight open-end tube viscometers, normally at 60 C,but is suitable for use at other temperatures. It is applicableover the range from 5 to 50 000 Pas.NOTE 1The precision for this test method is based
5、on determinationsmade at 60 C.1.2 The values stated in SI units are to be regarded as thestandard, except in reference to viscometer constant or calibra-tion factor (K).1.3 WarningMercury has been designated by the UnitedStates Environmental ProtectionAgency (EPA) and many stateagencies as a hazardo
6、us material that can cause central nervoussystem, kidney, and liver damage. Mercury or its vapor may behazardous to health and corrosive to materials. Caution shouldbe taken when handling mercury and mercury-containingproducts. See the applicable product Material Safety DataSheets (MSDS) for details
7、 and the EPAs website(www.epa.gov/mercury/faq.htm) for additional information.Users should be aware that selling mercury, mercury-containing products, or both, in your state may be prohibited bystate law.1.4 The text of this standard references notes and footnoteswhich provide explanatory material.
8、These notes and footnotes(excluding those in tables and figures) shall not be consideredas requirements of the standard.1.5 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-pr
9、iate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelo
10、pment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D2171 Test Method for Viscosity of Asphalts by VacuumCapillary ViscometerD3666 Specification for Minimum Requirem
11、ents for Agen-cies Testing and Inspecting Road and Paving MaterialsD6997 Test Method for Distillation of Emulsified AsphaltE1 Specification for ASTM Liquid-in-Glass ThermometersE77 Test Method for Inspection and Verification of Ther-mometersE644 Test Methods for Testing Industrial Resistance Ther-mo
12、metersE1137/E1137M Specification for Industrial Platinum Resis-tance ThermometersE2251 Specification for Liquid-in-Glass ASTM Thermom-eters with Low-Hazard Precision Liquids3. Terminology3.1 Definitions:3.1.1 apparent viscositythe determined viscosity obtainedby the test method under description. Vi
13、scosity is the resistanceto deformation or internal friction of a liquid expressed as theratio of the shear stress to shear rate, whether this ratio isconstant or not. The unit of viscosity obtained by dividing theshearing stress in N/m2by the rate of shear in reciprocalseconds is called the pascal
14、second (Pas). The English unit ofviscosity is the poise (P) with dimensions of 0.1Ns/m2(dynes/cm2/s), and is equivalent to 0.1 Pas.1This test method is under the jurisdiction of ASTM Committee D04 on Roadand Paving Materials and is the direct responsibility of Subcommittee D04.44 onRheological Tests
15、.Current edition approved Jan. 15, 2018. Published January 2018. Originallyapproved in 1989. Last previous edition approved in 2008 as D4957 08 which waswithdrawn January 2017 and reinstated in January 2018. DOI: 10.1520/D4957-18.2For referenced ASTM standards, visit the ASTM website, www.astm.org,
16、orcontact ASTM Customer Service 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
17、 standard was developed in accordance 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.1
18、3.1.2 Newtonian liquida liquid in which the rate of shearis proportional to the shearing stress. The constant ratio of theshearing stress to rate of shear is the viscosity of the liquid. Ifthe ratio is not constant, the liquid is non-Newtonian.NOTE 2A power law fluid is a material in which the relat
19、ion betweenthe log of the shear stress is linear with the log of the shear rate. The slopeof this relation is called the shear susceptibility, C.IfC is less than unity,the material is classified as pseudoplastic and the apparent viscositydecreases with increased stress. If C is greater than one, the
20、 material isdilatant and the apparent viscosity increases with stress. If C is unity thematerial shows Newtonian flow. Most real materials show some non-Newtonian behavior and the apparent viscosity, computed as stressdivided by the shear rate, is reported.3.1.3 rheograma rheological diagram which s
21、hows howthe apparent viscosity of a material varies with the shear rate.An apparent viscosity at a specific shear rate, normally 1 s1,can be estimated from this plot. A typical rheogram with anexample is shown in Fig. 1.4. Summary of Test Method4.1 The time is measured for a fixed volume of the liqu
22、id tobe drawn up through a straight, open-end capillary tube bymeans of vacuum, under closely controlled conditions ofvacuum and temperature. The apparent viscosity in poises iscalculated by multiplying the flow time in seconds by theappropriate viscometer calibration factor or calculated viscom-ete
23、r constant.5. Significance and Use5.1 This test method is useful for characterizing the flowbehavior of asphalt emulsion residues and non-Newtonianasphalts. However, since non-Newtonian viscosity values de-pend on the level of shearing stress, its duration, and the shearhistory of the material, a no
24、n-Newtonian viscosity is not aunique material property. Instead, it is a parameter which ischaracteristic of the fluid-viscometer system under the condi-tions of the measurement procedure.Therefore, comparisons ofnon-Newtonian material behavior should only be made usingapparent viscosities determine
25、d in similar viscometers undersimilar conditions of shearing stress and stress history. Proce-dures of sample preparation are especially important forrepeatability or reproducibility of test results.NOTE 3The quality of the results produced by this standard aredependent on the competence of the pers
26、onnel performing the procedureand the capacity, calibration, and maintenance of the equipment used.Agencies that meet the criteria of Specification D3666 are generallyconsidered capable of competent and objective testing, sampling,inspection, etc. Users of this standard are cautioned that compliance
27、 withSpecification D3666 alone does not completely ensure reliable results.Reliable results depend on many factors; following the suggestions ofSpecification D3666 or some similar acceptable guideline provides ameans of evaluating and controlling some of those factors.6. Apparatus6.1 ViscometersCapi
28、llary types, made of borosilicateglass, annealed, suitable for this test are as follows:6.1.1 Modified Koppers Vacuum Viscometer, as described inAnnexA1. Calibrated viscometers are available from commer-cial suppliers. Details regarding calibration of viscometers aregiven in A1.3.6.2 ThermometersCal
29、ibrated liquid-in-glass thermom-eters of an accuracy after correction of 0.02 C can be used, orany other thermometric device of equal accuracy. ASTMKinematic Viscosity Thermometers 47C conforming to Speci-fication E1 are suitable for the most commonly used tempera-ture of 60 C. See Test Method D2171
30、, Table X5.1 onKinematic Viscosity Test Thermometers for details on specificthermometers.6.2.1 The specified thermometers are standardized at “totalimmersion,” which means immersion to the top of the mercurycolumn with the remainder of the stem and the expansionchamber at the top of the thermometer
31、exposed to roomtemperature. The practice of completely submerging the ther-mometer is not recommended. When thermometers are com-pletely submerged, corrections for each individual thermom-eter based on calibration under conditions of completeFIG. 1 Typical Log-Log Rheogram Plot with ExampleD4957 182
32、submergence must be determined and applied. If the thermom-eter is completely submerged in the bath during use, thepressure of the gas in the expansion chamber will be higher orlower than during standardization, and may cause high or lowreadings of the thermometer.6.2.2 It is essential that liquid-i
33、n-glass thermometers becalibrated periodically using the technique given in TestMethod E77 (see Appendix X1).6.3 BathA bath suitable for immersion of the viscometerso that the liquid reservoir or the top of the capillary, whicheveris uppermost, is at least 20 mm below the upper surface of thebath li
34、quid, and with provisions for visibility of the viscometerand the thermometer. Firm supports for the viscometer shall beprovided.The efficiency of the stirring and the balance betweenheat loss and heat input must be such that the temperature ofthe bath medium does not vary by more than 0.03 C over t
35、helength of the viscometer or from viscometer to viscometer inthe various bath positions.6.4 Vacuum SystemA vacuum system3capable of main-taining a vacuum to within 667 Pa of the desired level up toand including 40.0 kPa. The essential system is shown sche-matically in Fig. 2. Tubing of 6.35 mm insi
36、de diameter shouldbe used, and all joints should be airtight so that when thesystem is closed, no loss of vacuum is indicated by the pressuregauge. A vacuum or aspirator pump is suitable for the vacuumsource. The vacuum measuring system for this test methodmust be standardized at least every six mon
37、ths.6.5 TimerAstopwatch or other timing device graduated indivisions of 0.1 s or less and accurate to within 0.05 % whentested over intervals of not less than 15 min shall be used.Electrical timing devices may be used only on electricalcircuits, the frequencies of which are controlled to an accuracy
38、of 0.05 % or better.6.5.1 Alternating-current frequencies that are intermittentlyand not continuously controlled, as provided by some publicpower systems, can cause large errors, particularly over shorttiming intervals, when used to actuate electrical timing devices.6.6 Sample Preparation OvenA suit
39、able oven for semi-continuous operations with control of temperature up to 202 62 C is required. It should have a fast heating rate capability inorder not to delay testing when needed on short notice.7. Sample Preparation7.1 Asphalt Emulsion ResidueIf the sample is the residualproduct from the emuls
40、ion distillation test at 260 C, pour asuitable portion of the total residue into a 50-mL beaker andallow to cool to 180 6 5 C. Then stir this portion of thesample at 1 r/s for 10 s. Following this, pour the proper amountinto the viscometer as in Section 8. Alternatively, allow thisportion of the res
41、idue to cool completely and set aside forfuture testing. This material should then be handled as in 7.2.7.2 Ambient SampleHeat the sample in an oven main-tained at 195 6 2 C. Stir the sample occasionally untilhomogeneous and pour into a 50-mL preheated beaker. Stir thesample at approximately 1 r/s f
42、or 10 s.NOTE 4Because of the nature of some asphalts and asphalt emulsionresidues, their shear and thermal history prior to testing may causevariations in test results. Careful sample preparation is most important forconsistent test results.NOTE 5In cases where the asphalt is not sufficiently fluid
43、to pour at180 6 5 C or too fluid to pour without splattering during transfer into theviscometer, other pouring temperatures may be used providing there isagreement between interested parties.8. Procedure8.1 Follow the general procedure described as follows,however, the specific details of the modifi
44、ed Koppers viscom-eter are described in Annex A1.8.1.1 Maintain the bath at the test temperatures to within60.03 C. Apply the necessary corrections, if any, to allthermometer readings.8.1.2 Select a clean, dry viscometer that will give a flowtime between 50 and 200 s for the C zone of a modified3The
45、 sole source of supply of the apparatus known to the committee at this timeis Cannon Instrument Co., P.O. Box 16, State College, PA, 16801. If you are awareof alternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at
46、 a meeting of theresponsible technical committee,1which you may attend.FIG. 2 Suggested Vacuum System for Vacuum Capillary ViscometersD4957 183Koppers viscometer. Preheat the viscometer filling tube andcapillary tube separately in the oven at 195 6 2 C for 5 minto assist in eliminating air bubbles w
47、hen the sample is poured.8.1.3 Charge the viscometer filling tube by pouring theprepared sample to within 62 mm of the fill line.NOTE 6In cases where highly viscous materials are being tested, thepossibility of air entrapment in the sample is greater. To alleviate thisproblem, a slight vacuum on the
48、 fill tube before the capillary tube is placedin position is suggested. This can be accomplished using a light vacuumsource attached to the fill tube for 30 s. A simple cork and tube shouldsuffice to achieve the desired effects.8.1.4 Place the charged viscometer filling tube in an ovenmaintained at
49、195 6 2 C for a period of 10 6 2 min to allowlarge air bubbles to escape.8.1.5 Remove the viscometer filling tube and capillary tubefrom the oven and then properly position the capillary tube intothe filling tube. Insert the viscometer in a holder and positionthe viscometer in the bath so that the uppermost timing mark isat least 20 mm below the surface of the bath liquid.NOTE 7Capillary action on certain small-diameter viscometer tubesmay cause a rise of the sample above the first timing mark. If this is aproblem, the capillary tube should be
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