1、Designation: D4402/D4402M 12D4402/D4402M 13Standard Test Method forViscosity Determination of Asphalt at ElevatedTemperatures Using a Rotational Viscometer1This standard is issued under the fixed designation D4402/D4402M; the number immediately following the designation indicates theyear 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 100 to 500F usinga rotational viscometer and a temperature-controlled thermal chamber for maintaining the test temperature.1.2 The values stated in either SI units or inch-pound units
4、are to be regarded separately as standard. The values stated in eachsystem may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from thetwo systems may result in non-conformance with the standard.1.3 This standard does not purport to address
5、 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 applicability of regulatorylimitations prior to use. See 10.6 for specific precautionary information.2. Referenced
6、 Documents2.1 ASTM Standards:2E644 Test Methods for Testing Industrial Resistance ThermometersE1137 Specification for Industrial Platinum 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.
7、1.2 filled asphalt, nan asphalt blend that contains finely dispersed insoluble mineral matter.3.1.3 Newtonian liquid, na liquid for 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 viscos
8、ity of a Newtonian liquid is therefore not dependenton its shear rate. If the ratio is not constant, the liquid is non-Newtonian. Many 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 th
9、e intermediate layers of the liquid move with respect to each other.Its unit of measure is the reciprocal second (sec-1).3.1.5 shear 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 v
10、iscosity, nthe ratio between the applied shear stress and 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). The centimetregram second (cgs) unit of viscosity is the pois
11、e (dynes/cm2) and is equivalent to 0.1 Pas. Frequently, centipoise (cP)equal toone millipascal second (mPas)is used as the viscosity unit.3.2 Definitions of Terms Specific to This Standard:1 This test method is under the jurisdiction ofASTM Committee D08 on Roofing and Waterproofing and is the direc
12、t responsibility of Subcommittee D08.03 on Surfacingand Bituminous Materials for Membrane Waterproofing and Built-up Roofing.Current edition approved July 1, 2012June 15, 2013. Published August 2012July 2013. Originally approved in 1984. Last previous edition approved in 20062012 asD4402 06.D4402 12
13、. DOI: 10.1520/D4402_D4402M-12.10.1520/D4402_D4402M-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This d
14、ocument 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 be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions
15、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 Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.1 apparatus-measuring geometry, nthe part of the e
16、quipment that is immersed in the asphalt sample, the dimensions ofwhich are used, in conjunction with the rotational resisting torque, 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
17、. Summary of Test Method4.1 A rotational viscometer, as described in this test method, is used to measure the apparent viscosity of asphalt at elevatedtemperatures. The torque on the apparatus-measuring geometry, rotating in a thermostatically controlled sample holder containinga sample of asphalt,
18、is used to measure the relative resistance to rotation. The torque and speed are used to determine the viscosityof the asphalt in 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,
19、or application temperatures.5.2 Some asphalts may exhibit non-Newtonian behavior under the conditions of this test method, or at temperatures within therange of this test method. Since non-Newtonian viscosity values are not absolute properties, but reflect the behavior of the fluidwithin the particu
20、lar measurement system, it should be recognized that measurements made by this test method may not alwayspredict field performance 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
21、 rate, and shear history.6. Apparatus6.1 Rotational Viscometer, capable of measuring the torque required to rotate the selected apparatus-measuring geometry at aselected constant speed while submerged in asphalt at constant desired test temperature, and with the capability to convert thetorque measu
22、rement to viscosity in pascal seconds, millipascal seconds, or centipoise. This calculation may need to be donemanually for some instruments.6.2 Apparatus-measuring geometry, of various shapes and sizes, for measurement of various viscosities of asphalt.6.3 Temperature-Controlled Thermal Chamber Hea
23、ter, for maintaining the sample of asphalt at the test temperature.6.4 Sample Chambers, reusable or disposable.6.5 Temperature Controller, capable of maintaining the specimen temperatures to 61.0C 62.0F for test temperaturesbetween 38 and 260C 100 to 150C 100 to 300F and to 62.0C 64.0F for test temp
24、eratures between 150 and 260C 300to 500F.6.6 Balance, readable to 0.1 g, for determining the mass of asphalt sample.6.7 Platinum Resistance Thermometer (PRT), with a probe which conforms to the requirements of Specification E1137. , formeasuring the temperature of the thermal chamber. The PRT shall
25、have a 3- or 4-wire connection configuration and overall sheathlength shall be at least 50 mm 2 in. greater than the immersion depth. Calibrate the PRT system (probe and readout) in accordancewith Test Methods E644.7. Reagents and Materials7.1 Solvents for cleaning sample chamber, apparatus-measurin
26、g geometry, and accessories.8. Preparation of Apparatus8.1 The rotational viscometer and thermal chamber heater shall be leveled and prepared as recommended by the instrumentmanufacturer.9. Calibration and Standardization9.1 The viscometer shall be zeroed before use, or as needed, or both, according
27、 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, using the method described by the supplier of the reference fluid. The reference fluid shall be certified to beNewtoni
28、an in behavior over the full range of expected test temperatures and shear rates. The reference fluid shall be certified ata temperature within 50C 90F of the temperature(s) to be used during the test. The viscosity measured shall be within 62 %of the certified value, or the viscometer requires reca
29、libration.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 sample or high flash point oil in the test chamber, and equilibrating to a temperature within50C 90F of the temperature(s
30、) to be used during the test. The sample temperature shall then be measured to within 60.1C60.2F by using a NIST traceable measuring device, as described in Test Methods E644. If any temperature differential isindicated, the set point of the temperature controller shall be offset accordingly.D4402/D
31、4402M 13210. Procedure10.1 Follow the manufacturers instructions for the operation of the instrument.10.2 Allow the instrument electronics to warm up for at least five minutes before conducting any calibrations or analyses.10.3 Set the temperature controller to the desired test temperature, taking i
32、nto 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 instrumentcapacity at the selected speed. Generally, measurements will be more accurate at higher torque readings.10.5 Preferably, preheat the sample c
33、hamber and the selected apparatus-measuring geometry until temperature equilibrium hasbeen obtained for at least 15 min. If filled asphalts are being measured, 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 sa
34、mplechamber. A convenient way for measuring the volume is by weighing out the amount calculated from approximate density datafor the sample and then returning the sample chamber to the temperature controlled chamber heater. Thoroughly stir filled asphaltsto obtain a representative sample before weig
35、hing.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, but ensure that the measuring portion of the apparatus-measuring geometry will becompletely immersed. Follow the manufacturers instructions. Th
36、e sample volume is critical to meet the system calibrationstandard.10.8 Insert the selected preheated apparatus-measuring geometry into the liquid in the chamber, and couple it to the viscometer,following the manufacturers instructions for proper alignment.10.9 Bring the asphalt sample to the desire
37、d 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 case of filled asphalts, start the motor rotation immediately.10.10 Start the motor rotation of the viscometer at a speed that will develop a resist
38、ing 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 min. Temperatureshould not deviate more than 61.0C 62.0F during this conditioning period.10.11 Measure either the viscosity or the torque at 1-min
39、intervals for a total of three minutes. The instrument may perform thismeasurement automatically.10.12 Repeat steps 10.9-10.11 for each test temperature required. If filled asphalts are being measured, a new, freshly stirredsample will be required for each test temperature.10.13 If torque readings a
40、re above 98 % of the instrument capacity at the lowest test temperature, decrease the speed of rotationof the apparatus-measuring geometry and continue 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
41、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 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
42、 torque readings by the appropriate factor toobtain the viscosity values.11. Calculation11.1 If the instrument does not automatically average three readings, then calculate the result as the arithmetic average of thethree readings taken at 1-min intervals, rounded to three significant figures. If th
43、e rotational viscometer has a digital outputdisplaying viscosity in centipoise (cP), multiply by 0.001 to obtain the viscosity in pascal seconds (Pas). For instruments that offerautomation, the results of a 3-min integration shall be acceptable.12. Report12.1 Report test temperature, apparatus-measu
44、ring 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 (Pas), 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 V
45、iscosity at 400F = 240 cPwith Brookfield spindle number 31, 48 % torque at 60 r/min.13. Precision and Bias13.1 Unfilled Roofing AsphaltThe following criteria shall be used for judging the acceptability of any result (95 % confidencelevel).13.1.1 Single-Operator Precision (Repeatability)Duplicate val
46、ues by the same operator using the same test equipment, in theshortest practical period of time shall be considered not equivalent if the difference in the two results, expressed as a percent oftheir mean, exceeds 3.5 %.D4402/D4402M 13313.1.2 Multilaboratory Precision (Reproducibility)The values rep
47、orted by each of two laboratories, representing thearithmetic average of duplicate determinations, shall be considered not equivalent if they differ by more than 14.5 %.13.2 Filled Roofing AsphaltAn interlaboratory study was conducted in 2004 comparing three filled roofing asphalts from threediffere
48、nt suppliers, tested in triplicate at 205C 400F by nine different laboratories. The data was used to calculate precisionestimates for filled asphalt. The following criteria shall be used for judging the acceptability of any result (95 % confidence level).13.2.1 The single-operator precision (repeata
49、bility) 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 multilaboratory precision (reproducibility) standard deviation has been determined to be 33.2 %. Therefore, tworesults submitted by two different operators testing the s
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