1、Designation: D4402 06 D4402/D4402M 12Standard Test Method forViscosity Determination of Asphalt at ElevatedTemperatures Using a Rotational Viscometer1This standard is issued under the fixed designation D4402;D4402/D4402M; the number immediately following the designation indicatesthe year of original
2、 adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defens
3、e.1. Scope1.1 This test method outlines a procedure for measuring the apparent viscosity of asphalt from 38 to 260C (100100 to500F)500F using a rotational viscometer and a temperature-controlled thermal chamber for maintaining the test temperature.1.2 The values stated in either SI units or inch-pou
4、nd units are to be regarded separately as the standard. The values given incentimetre gram second (cgs) units and inch-pound units are for information only.stated in each system may not be exactequivalents; therefore, each system shall be used independently of the other. Combining values from the tw
5、o systems may resultin non-conformance with the standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicabilit
6、y of regulatorylimitations prior to use. See 10.6 for specific precautionary information.2. Referenced Documents2.1 ASTM Standards:2E220E644 Test Method for Calibration of Thermocouples By Comparison TechniquesMethods for Testing Industrial ResistanceThermometersE1137 Specification for Industrial Pl
7、atinum Resistance Thermometers3. Terminology3.1 Definitions:3.1.1 apparent viscosity, nthe ratio of shear stress to shear rate for a Newtonian or non-Newtonian liquid.3.1.2 filled asphalt, nan asphalt blend that contains finely dispersed insoluble mineral matter.3.1.3 Newtonian liquid, na liquid for
8、 which the rate of shear is proportional to the shearing stress. The constant ratio of theshearing stress to the rate of shear is the viscosity of the liquid. The viscosity of a Newtonian liquid is therefore not dependenton its shear rate. If the ratio is not constant, the liquid is non-Newtonian. M
9、any liquids exhibit both Newtonian and non-Newtonianbehavior, depending on the shear rate or temperature, or both.3.1.4 shear rate, nthe measure of the speed at which the intermediate layers of the liquid move with respect to each other.Its unit of measure is the reciprocal second (sec-1).3.1.5 shea
10、r stress, nthe force per unit area required to produce the shearing action. Its SI unit of measurement is the pascal,and its cgs unit of measurement is dynes/cm2.3.1.6 viscosity, nthe ratio between the applied shear stress and the rate of shear is called the coefficient of viscosity. Thiscoefficient
11、 is a measure of the resistance to flow of the liquid. The SI unit of viscosity is the pascal second (Pas). The centimetregram second (cgs) unit of viscosity is the poise (dynes/cm2) and is equivalent to 0.1 Pas. Frequently, centipoise (cP)equal toone millipascal second (mPas)is used as the viscosit
12、y unit.1 This test method is under the jurisdiction of ASTM Committee D08 on Roofing and Waterproofing and is the direct responsibility of Subcommittee D08.03 on Surfacingand Bituminous Materials for Membrane Waterproofing and Built-up Roofing.Current edition approved Dec. 1, 2006July 1, 2012. Publi
13、shed December 2006 August 2012. Originally approved in 1984. Last previous edition approved in 20022006as D4402 02.D4402 06. DOI: 10.1520/D4402-06.10.1520/D4402_D4402M-12.2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For A
14、nnual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not
15、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 standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Dri
16、ve, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2 Definitions of Terms Specific to This Standard:3.2.1 apparatus-measuring geometry, nthe part of the equipment that is immersed in the asphalt sample, the dimensions ofwhich are used, in conjunction with the rotational resisting tor
17、que, to calculate the apparent viscosity. This geometry may bereferred to by the equipment manufacturer as a spindle, bob, inner concentric cylinder, vane, and so forth.4. Summary of Test Method4.1 A rotational viscometer, as described in this test method, is used to measure the apparent viscosity o
18、f asphalt at elevatedtemperatures. The torque on the apparatus-measuring geometry, rotating in a thermostatically controlled sample holder containinga sample of asphalt, is used to measure the relative resistance to rotation. The torque and speed are used to determine the viscosityof the asphalt in
19、pascal seconds, millipascal seconds, or centipoise.5. Significance and Use5.1 This test method is used to measure the apparent viscosity of asphalts at handling, mixing, or application temperatures.5.2 Some asphalts may exhibit non-Newtonian behavior under the conditions of this test method, or at t
20、emperatures within therange of this test method. Since non-Newtonian viscosity values are not absolute properties, but reflect the behavior of the fluidwithin the particular measurement system, it should be recognized that measurements made by this test method may not alwayspredict field performance
21、 under the conditions of use.5.3 Comparisons between non-Newtonian viscosity values should be made only for measurements made with similar conditionsof temperature, shear rate, and shear history.6. Apparatus6.1 Rotational Viscometer, capable of measuring the torque required to rotate the selected ap
22、paratus-measuring geometry at aselected constant speed while submerged in asphalt at constant desired test temperature, and with the capability to convert thetorque measurement to viscosity in pascal seconds, millipascal seconds, or centipoise. This calculation may need to be donemanually for some i
23、nstruments.6.2 Apparatus-measuring geometry, of various shapes and sizes, for measurement of various viscosities of asphalt.6.3 Temperature-Controlled Thermal Chamber Heater, for maintaining the sample of asphalt at the test temperature.6.4 Sample Chambers, reusable or disposable.6.5 Temperature Con
24、troller, capable of maintaining the specimen temperatures to 61.0C (62.0F)62.0F for testtemperatures between 38 and 260C (100100 to 500F).500F.6.6 Balance, readable to 0.1 g, for determining the mass of asphalt sample.6.7 Calibration Device, Platinum Resistance Thermometer (PRT), with a probe which
25、conforms to the requirements ofSpecification E1137. The PRT shall have a 3- or 4-wire connection configuration and overall sheath length shall be at least 50 mm2 in. greater than the immersion depth. Calibrate the PRT system (probe and readout) in accordance with MethodTestE220Methods E644for calibr
26、ating the temperature controller7. Reagents and Materials7.1 Solvents for cleaning sample chamber, apparatus-measuring geometry, and accessories.8. Preparation of Apparatus8.1 The rotational viscometer and thermal chamber heater shall be leveled and prepared as recommended by the instrumentmanufactu
27、rer.9. Calibration and Standardization9.1 The viscometer shall be zeroed before use, or as needed, or both, according to the manufacturers instructions.9.2 The accuracy of the viscometer shall be checked at least annually using a certified reference fluid of known viscosity atvarious temperatures, u
28、sing the method described by the supplier of the reference fluid. The reference fluid shall be certified to beNewtonian in behavior over the full range of expected test temperatures and shear rates. The reference fluid shall be certified ata temperature within 50C (90F)90F of the temperature(s) to b
29、e used during the test. The viscosity measured shall be within62 % of the certified value, or the viscometer requires recalibration.9.3 The accuracy of the temperature reading and the temperature stability of the temperature controller are to be checked at leastevery six months by placing an asphalt
30、 sample or high flash point oil in the test chamber, and equilibrating to a temperature within50C (90F)90F of the temperature(s) to be used during the test. The sample temperature shall then be measured to within60.1C (60.2F)60.2F by using a NIST traceable measuring device, as described in Method Te
31、st Methods E220E644. If anytemperature differential is indicated, the set point of the temperature controller shall be offset accordingly.D4402/D4402M 12210. Procedure10.1 Follow the manufacturers instructions for the operation of the instrument.10.2 Allow the instrument electronics to warm up for a
32、t least five minutes before conducting any calibrations or analyses.10.3 Set the temperature controller to the desired test temperature, taking into account any offset determined in 9.3.10.4 Select an apparatus-measuring geometry that will develop a resisting torque between 10 and 98 % of the instru
33、mentcapacity at the selected speed. Generally, measurements will be more accurate at higher torque readings.10.5 Preferably, preheat the sample chamber and the selected apparatus-measuring geometry until temperature equilibrium hasbeen obtained for at least 15 min. If filled asphalts are being measu
34、red, this step is mandatory.10.6 Add the volume of sample specified by the manufacturer for the apparatus-measuring geometry to be used to the samplechamber. A convenient way for measuring the volume is by weighing out the amount calculated from approximate density datafor the sample and then return
35、ing the sample chamber to the temperature controlled chamber heater. Thoroughly stir filled asphaltsto obtain a representative sample before weighing.NOTE 1Exercise caution to avoid sample overheating, and to avoid the ignition of samples with low flash points.10.7 Do not overfill the sample chamber
36、, but ensure that the measuring portion of the apparatus-measuring geometry will becompletely immersed. Follow the manufacturers instructions. The sample volume is critical to meet the system calibrationstandard.10.8 Insert the selected preheated apparatus-measuring geometry into the liquid in the c
37、hamber, and couple it to the viscometer,following the manufacturers instructions for proper alignment.10.9 Bring the asphalt sample to the desired temperature within 30 min and allow it to equilibrate at the desired test temperaturefor a minimum of 10 min before beginning the measurement. In the cas
38、e of filled asphalts, start the motor rotation immediately.10.10 Start the motor rotation of the viscometer at a speed that will develop a resisting torque that is between 10 and 98 % ofthe full-scale instrument capacity. Maintain this speed and allow the sample to equilibrate for an additional 5 mi
39、n. Temperatureshould not deviate more than 61.0C (62.0F)62.0F during this conditioning period.10.11 Measure either the viscosity or the torque at 1-min intervals for a total of three minutes. The instrument may perform thismeasurement automatically.10.12 Repeat steps 10.9-10.11 for each test tempera
40、ture required. If filled asphalts are being measured, a new, freshly stirredsample will be required for each test temperature.10.13 If torque readings are above 98 % of the instrument capacity at the lowest test temperature, decrease the speed of rotationof the apparatus-measuring geometry and conti
41、nue with the test, or repeat steps 10.5-10.11 with a smaller diameter geometry andthe appropriate volume of sample.10.14 If the torque reading is below 10 % of the instrument capacity at the highest test temperature, increase the speed ofrotation of the apparatus geometry, or repeat steps 10.5-10.11
42、 with a larger diameter geometry and the appropriate volume ofsample.10.15 If the instrument does not read out directly in viscosity units, multiply the torque readings by the appropriate factor toobtain the viscosity values.11. Calculation11.1 If the instrument does not automatically average three
43、readings, then calculate the result as the arithmetic average of thethree readings taken at 1-min intervals, rounded to three significant figures. If the rotational viscometer has a digital outputdisplaying viscosity in centipoise (cP), multiply by 0.001 to obtain the viscosity in pascal seconds (Pa
44、s). For instruments that offerautomation, the results of a 3-min integration shall be acceptable.12. Report12.1 Report test temperature, apparatus-measuring geometry type and size, torque in mNm or percent of instrument capacity,and speed in sec-1 or r/min with viscosity results in pascal seconds (P
45、as), millipascal seconds (mPas), or centipoise (cP). Forexample, Viscosity at 135C = 0.455 Pas with Bohlin 25 mm bob, 8.3 mNm of torque at 10 sec-1 or Viscosity at 400F = 240 cPwith Brookfield spindle number 31, 48 % torque at 60 r/min.13. Precision and Bias13.1 Unfilled Roofing AsphaltThe following
46、 criteria shall be used for judging the acceptability of any result (95 % confidencelevel).13.1.1 Single-Operator Precision (Repeatability)Duplicate values by the same operator using the same test equipment, in theshortest practical period of time shall be considered not equivalent if the difference
47、 in the two results, expressed as a percent oftheir mean, exceeds 3.5 %.D4402/D4402M 12313.1.2 Multilaboratory Precision (Reproducibility)The values reported by each of two laboratories, representing thearithmetic average of duplicate determinations, shall be considered not equivalent if they differ
48、 by more than 14.5 %.13.2 Filled Roofing AsphaltAn interlaboratory study was conducted in 2004 comparing three filled roofing asphalts from threedifferent suppliers, tested in triplicate at 205C (400F)400F by nine different laboratories. The data was used to calculateprecision estimates for filled a
49、sphalt. The following criteria shall be used for judging the acceptability of any result (95 %confidence level).13.2.1 The single-operator precision (repeatability) standard deviation has been determined to be 21.0 %. Therefore, two resultsobtained in the same laboratory, by the same operator using the same equipment, in the shortest practical period of time, shouldbe considered not equivalent if the difference in the two results, expressed as a percent of their mean, exceeds 59.4 %.13.2.2 The multilaborator
