1、Designation: D 4402 06Standard Test Method forViscosity Determination of Asphalt at ElevatedTemperatures Using a Rotational Viscometer1This standard is issued under the fixed designation D 4402; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test me
3、thod outlines a procedure for measuring theapparent viscosity of asphalt from 38 to 260C (100 to 500F)using a rotational viscometer and a temperature-controlledthermal chamber for maintaining the test temperature.1.2 The values stated in SI units are to be regarded as thestandard. The values given i
4、n centimetre gram second (cgs)units and inch-pound units are for information 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 d
5、etermine the applica-bility of regulatory limitations prior to use. See 10.6 forspecific precautionary information.2. Referenced Documents2.1 ASTM Standards:2E 220 Test Method for Calibration of Thermocouples ByComparison Techniques3. Terminology3.1 Definitions:3.1.1 apparent viscosity, nthe ratio o
6、f shear stress to shearrate for a Newtonian or non-Newtonian liquid.3.1.2 filled asphalt, nan asphalt blend that contains finelydispersed insoluble mineral matter.3.1.3 Newtonian liquid, na liquid for which the rate ofshear is proportional to the shearing stress. The constant ratioof the shearing st
7、ress to the rate of shear is the viscosity of theliquid. The viscosity of a Newtonian liquid is therefore notdependent on its shear rate. If the ratio is not constant, theliquid is non-Newtonian. Many liquids exhibit both Newtonianand non-Newtonian behavior, depending on the shear rate ortemperature
8、, or both.3.1.4 shear rate, nthe measure of the speed at which theintermediate layers of the liquid move with respect to eachother. Its unit of measure is the reciprocal second (sec-1).3.1.5 shear stress, nthe force per unit area required toproduce the shearing action. Its SI unit of measurement is
9、thepascal, and its cgs unit of measurement is dynes/cm2.3.1.6 viscosity, nthe ratio between the applied shear stressand the rate of shear is called the coefficient of viscosity. Thiscoefficient is a measure of the resistance to flow of the liquid.The SI unit of viscosity is the pascal second (Pas).
10、Thecentimetre gram second (cgs) unit of viscosity is the poise(dynes/cm2) and is equivalent to 0.1 Pas. Frequently, centi-poise (cP)equal to one millipascal second (mPas)is usedas the viscosity unit.3.2 Definitions of Terms Specific to This Standard:3.2.1 apparatus-measuring geometry, nthe part of t
11、heequipment that is immersed in the asphalt sample, the dimen-sions of which are used, in conjunction with the rotationalresisting torque, to calculate the apparent viscosity. Thisgeometry may be referred to by the equipment manufacturer asa spindle, bob, inner concentric cylinder, vane, and so fort
12、h.4. Summary of Test Method4.1 Arotational viscometer, as described in this test method,is used to measure the apparent viscosity of asphalt at elevatedtemperatures. The torque on the apparatus-measuring geom-etry, rotating in a thermostatically controlled sample holdercontaining a sample of asphalt
13、, is used to measure the relativeresistance to rotation. The torque and speed are used todetermine the viscosity of the asphalt in pascal seconds,millipascal seconds, or centipoise.5. Significance and Use5.1 This test method is used to measure the apparentviscosity of asphalts at handling, mixing, o
14、r application tem-peratures.5.2 Some asphalts may exhibit non-Newtonian behaviorunder the conditions of this test method, or at temperatures1This test method is under the jurisdiction ofASTM Committee D08 on Roofingand Waterproofing and is the direct responsibility of Subcommittee D08.03 onSurfacing
15、 and Bituminous Materials for Membrane Waterproofing and Built-upRoofing.Current edition approved Dec. 1, 2006. Published December 2006. Originallyapproved in 1984. Last previous edition approved in 2002 as D 4402 02.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact AST
16、M Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer 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.within the range of this test
17、 method. Since non-Newtonianviscosity values are not absolute properties, but reflect thebehavior of the fluid within the particular measurement system,it should be recognized that measurements made by this testmethod may not always predict field performance under theconditions of use.5.3 Comparison
18、s between non-Newtonian viscosity valuesshould be made only for measurements made with similarconditions of temperature, shear rate, and shear history.6. Apparatus6.1 Rotational Viscometer, capable of measuring the torquerequired to rotate the selected apparatus-measuring geometry ata selected const
19、ant speed while submerged in asphalt atconstant desired test temperature, and with the capability toconvert the torque measurement to viscosity in pascal seconds,millipascal seconds, or centipoise. This calculation may needto be done manually for some instruments.6.2 Apparatus-measuring geometry, of
20、 various shapes andsizes, for measurement of various viscosities of asphalt.6.3 Temperature-Controlled Thermal Chamber Heater, formaintaining the sample of asphalt at the test temperature.6.4 Sample Chambers, reusable or disposable.6.5 Temperature Controller, capable of maintaining thespecimen tempe
21、ratures to 61.0C (62.0F) for test tempera-tures between 38 and 260C (100 to 500F).6.6 Balance, readable to 0.1 g, for determining the mass ofasphalt sample.6.7 Calibration Device, in accordance with Method E 220for calibrating the temperature controller.7. Reagents and Materials7.1 Solvents for clea
22、ning sample chamber, apparatus-measuring geometry, and accessories.8. Preparation of Apparatus8.1 The rotational viscometer and thermal chamber heatershall be leveled and prepared as recommended by the instru-ment manufacturer.9. Calibration and Standardization9.1 The viscometer shall be zeroed befo
23、re use, or as needed,or both, according to the manufacturers instructions.9.2 The accuracy of the viscometer shall be checked at leastannually using a certified reference fluid of known viscosity atvarious temperatures, using the method described by thesupplier of the reference fluid. The reference
24、fluid shall becertified to be Newtonian in behavior over the full range ofexpected test temperatures and shear rates. The reference fluidshall be certified at a temperature within 50C (90F) of thetemperature(s) to be used during the test. The viscositymeasured shall be within 62 % of the certified v
25、alue, or theviscometer requires recalibration.9.3 The accuracy of the temperature reading and the tem-perature stability of the temperature controller are to bechecked at least every six months by placing an asphalt sampleor high flash point oil in the test chamber, and equilibrating toa temperature
26、 within 50C (90F) of the temperature(s) to beused during the test. The sample temperature shall then bemeasured to within 60.1C (60.2F) by using a NIST trace-able measuring device, as described in Method E 220.Ifanytemperature differential is indicated, the set point of thetemperature controller sha
27、ll be offset accordingly.10. Procedure10.1 Follow the manufacturers instructions for the opera-tion of the instrument.10.2 Allow the instrument electronics to warm up for atleast five minutes before conducting any calibrations or analy-ses.10.3 Set the temperature controller to the desired testtempe
28、rature, taking into account any offset determined in 9.3.10.4 Select an apparatus-measuring geometry that will de-velop a resisting torque between 10 and 98 % of the instrumentcapacity at the selected speed. Generally, measurements will bemore accurate at higher torque readings.10.5 Preferably, preh
29、eat the sample chamber and the se-lected apparatus-measuring geometry until temperature equi-librium has been obtained for at least 15 min. If filled asphaltsare being measured, this step is mandatory.10.6 Add the volume of sample specified by the manufac-turer for the apparatus-measuring geometry t
30、o be used to thesample chamber. A convenient way for measuring the volumeis by weighing out the amount calculated from approximatedensity data for the sample and then returning the samplechamber to the temperature controlled chamber heater. Thor-oughly stir filled asphalts to obtain a representative
31、 samplebefore weighing.NOTE 1Exercise caution to avoid sample overheating, and to avoidthe ignition of samples with low flash points.10.7 Do not overfill the sample chamber, but ensure that themeasuring portion of the apparatus-measuring geometry willbe completely immersed. Follow the manufacturers
32、instruc-tions. The sample volume is critical to meet the systemcalibration standard.10.8 Insert the selected preheated apparatus-measuring ge-ometry into the liquid in the chamber, and couple it to theviscometer, following the manufacturers instructions forproper alignment.10.9 Bring the asphalt sam
33、ple to the desired temperaturewithin 30 min and allow it to equilibrate at the desired testtemperature for a minimum of 10 min before beginning themeasurement. In the case of filled asphalts, start the motorrotation immediately.10.10 Start the motor rotation of the viscometer at a speedthat will dev
34、elop a resisting torque that is between 10 and 98 %of the full-scale instrument capacity. Maintain this speed andallow the sample to equilibrate for an additional 5 min.Temperature should not deviate more than 61.0C (62.0F)during this conditioning period.10.11 Measure either the viscosity or the tor
35、que at 1-minintervals for a total of three minutes. The instrument mayperform this measurement automatically.10.12 Repeat steps 10.9-10.11 for each test temperaturerequired. If filled asphalts are being measured, a new, freshlystirred sample will be required for each test temperature.D440206210.13 I
36、f torque readings are above 98 % of the instrumentcapacity at the lowest test temperature, decrease the speed ofrotation of the apparatus-measuring geometry and continuewith the test, or repeat steps 10.5-10.11 with a smaller diametergeometry and the appropriate volume of sample.10.14 If the torque
37、reading is below 10 % of the instrumentcapacity at the highest test temperature, increase the speed ofrotation of the apparatus geometry, or repeat steps 10.5-10.11with a larger diameter geometry and the appropriate volume ofsample.10.15 If the instrument does not read out directly in viscos-ity uni
38、ts, multiply the torque readings by the appropriate factorto obtain the viscosity values.11. Calculation11.1 If the instrument does not automatically average threereadings, then calculate the result as the arithmetic average ofthe three readings taken at 1-min intervals, rounded to threesignificant
39、figures. If the rotational viscometer has a digitaloutput displaying viscosity in centipoise (cP), multiply by0.001 to obtain the viscosity in pascal seconds (Pas). Forinstruments that offer automation, the results of a 3-minintegration shall be acceptable.12. Report12.1 Report test temperature, app
40、aratus-measuring geom-etry type and size, torque in mNm or percent of instrumentcapacity, and speed in sec-1or r/min with viscosity results inpascal seconds (Pas), millipascal seconds (mPas), or centi-poise (cP). For example, Viscosity at 135C = 0.455 Pas withBohlin 25 mm bob, 8.3 mNm of torque at 1
41、0 sec-1or Viscosityat 400F = 240 cP with Brookfield spindle number 31, 48 %torque at 60 r/min.13. Precision and Bias13.1 Unfilled Roofing AsphaltThe following criteria shallbe used for judging the acceptability of any result (95 %confidence level).13.1.1 Single-Operator Precision (Repeatability)Dupl
42、icate values by the same operator using the same testequipment, in the shortest practical period of time shall beconsidered not equivalent if the difference in the two results,expressed as a percent of their mean, exceeds 3.5 %.13.1.2 Multilaboratory Precision (Reproducibility)Thevalues reported by
43、each of two laboratories, representing thearithmetic average of duplicate determinations, shall be con-sidered not equivalent if they differ by more than 14.5 %.13.2 Filled Roofing AsphaltAn interlaboratory study wasconducted in 2004 comparing three filled roofing asphalts fromthree different suppli
44、ers, tested in triplicate at 205C (400F)by nine different laboratories. The data was used to calculateprecision estimates for filled asphalt. The following criteriashall be used for judging the acceptability of any result (95 %confidence level).13.2.1 The single-operator precision (repeatability) st
45、andarddeviation has been determined to be 21.0 %. Therefore, tworesults obtained in the same laboratory, by the same operatorusing the same equipment, in the shortest practical period oftime, should be considered not equivalent if the difference inthe two results, expressed as a percent of their mea
46、n, exceeds59.4 %.13.2.2 The multilaboratory precision (reproducibility) stan-dard deviation has been determined to be 33.2 %. Therefore,two results submitted by two different operators testing thesame material in different laboratories shall be considered notequivalent if the difference in the two r
47、esults, expressed as apercent of their mean, exceeds 94.0 %.13.3 Unfilled Paving AsphaltThe precision estimatesgiven are based on the analysis of test results from eight pairsof AMRL proficiency samples. The data analyzed consisted ofresults from 142 to 202 laboratories for each of the eight pairsof
48、 samples. The details of this analysis are in NCHRP FinalReport, NCHRP Project No. 9-26, Phase 3. The followingcriteria shall be used for judging the acceptability of any result(95 % confidence level).13.3.1 The single-operator precision (repeatability) coeffi-cient of variation (1s %) has been dete
49、rmined to be 1.2 %.Therefore, two results obtained in the same laboratory, by thesame operator using the same equipment, in the shortestpractical period of time, should be considered not equivalent ifthe difference in the two results, expressed as a percent of theirmean, exceeds 3.5 % (d2s %).13.3.2 The multilaboratory precision (reproducibility) coef-ficient of variation (1s %) has been determined to be 4.3 %.Therefore, two results submitted by two different operatorstesting the same material in different laboratories shall beconsidered no
