ASTM D2171-2001 Standard Test Method for Viscosity of Asphalts by Vacuum Capillary Viscometer《用真空毛细管粘度计测定沥青粘度的标准试验方法》.pdf

1、Designation: D 2171 01Designation: 222/84 (89)Standard Test Method forViscosity of Asphalts by Vacuum Capillary Viscometer1This standard is issued under the fixed designation D 2171; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,

2、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.This test method has been approved b

3、y the sponsoring committees and accepted by the cooperating societies in accordance withestablished procedures.1. Scope1.1 This test method covers procedures for the determina-tion of viscosity of asphalt (bitumen) by vacuum capillaryviscometers at 60C (140F). It is applicable to materialshaving vis

4、cosities in the range from 0.0036 to over 20 000 Pa s (0.036 to over 200 000 P).NOTE 1This test method is suitable for use at other temperatures, butthe precision is based on determinations on asphalt cements at 60C(140F).1.2 This standard does not purport to address all of thesafety concerns, if an

5、y, 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. Referenced Documents2.1 ASTM Standards:E1 Specification for ASTM Thermometers2E11 Specific

6、ation for Wire-Cloth and Sieves for TestingPurposes3E77 Test Method for Inspection and Verification of Ther-mometers23. Terminology3.1 Definitions:3.1.1 Newtonian liquida liquid in which the rate of shearis proportional to the shearing stress. The constant ratio of theshearing stress to the rate of

7、shear is the viscosity of the liquid.If the ratio is not constant, the liquid is non-Newtonian.3.1.2 viscositythe ratio between the applied shear stressand rate of shear is called the coefficient of viscosity. Thiscoefficient is thus a measure of the resistance to flow of theliquid. It is commonly c

8、alled the viscosity of the liquid. The SIunit of viscosity is 1 Pas(1Ns/m2) and is called aPascal-second. The cgs unit of viscosity is 1 g/cms (1dynes/cm2) and is called a poise (P). 1 Pasisequivalent to10 P.4. Summary of Test Method4.1 The time is measured for a fixed volume of the liquid tobe draw

9、n up through a capillary tube by means of vacuum,under closely controlled conditions of vacuum and tempera-ture. The viscosity in Pascal-seconds is calculated by multi-plying the flow time in seconds by the viscometer calibrationfactor.NOTE 2The rate of shear decreases as the liquid moves up the tub

10、e,or it can also be varied by the use of different vacuum or different sizeviscometer. Thus, this method is suitable for the measurement of viscosi-ties of Newtonian (simple) and non-Newtonian (complex) liquids.5. Significance and Use5.1 The viscosity at 60C (140F) characterizes flow behav-ior and m

11、ay be used for specification requirements for cutbacksand asphalt cements.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. In the IP this test method is under the jurisdiction of

12、 theStandardization Committee.Current edition approved Aug. 10, 2001. Published October 2001. Originallypublished as D 2171 63 T. Last previous edition D 2171 94.2Annual Book of ASTM Standards, Vol 14.03.3Annual Book of ASTM Standards, Vol 14.02.1Copyright ASTM International, 100 Barr Harbor Drive,

13、PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Apparatus6.1 Viscometers, capillary-type, made of borosilicate glass,annealed, suitable for this test are as follows:6.1.1 Cannon-Manning Vacuum Viscometer (CMVV), asdescribed in Appendix X1.6.1.2 Asphalt Institute Vacuum Viscometer (AI

14、VV), as de-scribed in Appendix X2.6.1.3 Modified Koppers Vacuum Viscometer (MKVV), asdescribed in Appendix X3. Calibrated viscometers are avail-able from commercial suppliers. Details regarding calibrationof viscometers are given in Appendix X4.NOTE 3The viscosity measured in a CMVV may be from 1 to

15、 5 %lower than either the AIVV or MKVV having the same viscosity range.This difference, when encountered, may be the result of non-Newtonianflow.46.2 Thermometers Calibrated liquid-in-glass thermom-eters (see Table X5.1) of an accuracy after correction of 0.02C(0.04F) can be used or any other thermo

16、metric device of equalaccuracy. ASTM Kinematic Viscosity Thermometers 47C and47F are suitable for the most commonly used temperature of60C (140F).6.2.1 The specified thermometers are standardized at“ totalimmersion,” which means immersion to the top of the mercurycolumn with the remainder of the ste

17、m and the expansionchamber at the top of the thermometer 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 completes

18、ubmergence 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 on the thermometer.6.2.2 It is essential that liquid-in

19、-glass thermometers becalibrated periodically using the technique given in TestMethod E77(see Appendix X5).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 liqu

20、id 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 losses and heat input must be such that the temperature ofthe bath medium does not vary by more than 60.03C(60.05F

21、) over the length of the viscometer, or from viscom-eter to viscometer in the various bath positions.6.4 Vacuum System A vacuum system5capable of main-taining a vacuum to within 60.5 mm of the desired level up toand including 40.0 kPa 300 mm Hg. The essential system isshown schematically in Fig. 1.

22、Glass tubing of 6.35-mm(14-in.) inside diameter should be used, and all glass jointsshould be airtight so that when the system is closed, no loss ofvacuum is indicated by the open-end mercury manometerhaving 1-mm graduations. A vacuum or aspirator pump issuitable for the vacuum source.6.5 TimerA sto

23、p watch or other timing device graduatedin divisions of 0.1 s or less and accurate to within 0.05 % whentested over intervals of not less than 15 min.6.6 Electrical Timing Devices may be used only on electri-cal circuits, the frequencies of which are controlled to anaccuracy of 0.05 % or better.6.6.

24、1 Alternating currents, the frequencies of which areintermittently and not continuously controlled, as provided bysome public power systems, can cause large errors, particularlyover short timing intervals, when used to actuate electricaltiming devices.7. Sample Preparations7.1 Heat the sample with c

25、are to prevent local overheatinguntil it has become sufficiently fluid to pour, occasionallystirring the sample to aid heat transfer and to assure uniformity.7.2 Transfer a minimum of 20 mL into a suitable containerand heat to 135 6 5.5C (275 6 10F), stirring occasionally toprevent local overheating

26、 and taking care to avoid the entrap-ment of air.NOTE 4If it is suspected that the sample may contain solid material,strain the melted sample into the container through a No. 50 (300-m)sieve conforming to No. 50 Specification E11.8. Procedure8.1 The specific details of operation vary somewhat for th

27、evarious types of viscometers. See the detailed descriptions of4Supporting data are available from ASTM Headquarters, 100 Barr HarborDrive, West Conshohocken, PA 19428-2959. Request RR:D04-1003.5The vacuum control system marketed by Cannon Instrument Co., P. O. Box 16,State College, PA 16801, has be

28、en found satisfactory for this purpose.FIG. 1 Suggested Vacuum System for Vacuum CapillaryViscometersD2171012viscometers in Appendix X1-Appendix X3 for instructions forusing the type of viscometer selected. In all cases, however,follow the general procedure described in 8.1.1-8.1.9.8.1.1 Maintain th

29、e bath at the test temperature within60.03C (0.05F). Apply the necessary corrections, if any, to allthermometer readings.8.1.2 Select a clean, dry viscometer that will give a flowtime greater than 60 s, and preheat to 135 6 5.5C (275610F).8.1.3 Charge the viscometer by pouring the preparedsample to

30、within 62 mm of fill line E (Fig. 2, Fig. 3, and Fig.4).8.1.4 Place the charged viscometer in an oven or bathmaintained at 135 6 5.5C (275 6 10F) for a period of 10 62 min, to allow large air bubbles to escape.8.1.5 Remove the viscometer from the oven or bath and,within 5 min, insert the viscometer

31、in a holder, and position theviscometer vertically in the bath so that the upper most timingmark is at least 20 mm below the surface of the bath liquid.8.1.6 Establish a 40.0 6 0.07 kPa (300 6 0.5 mm Hg)vacuum below atmospheric pressure in the vacuum system andconnect the vacuum system to the viscom

32、eter with the togglevalve or stopcock closed in the line leading to the viscometer.8.1.7 After the viscometer has been in the bath for 30 6 5min, start the flow of asphalt in the viscometer by opening thetoggle valve or stopcock in the line leading to the vacuumsystem.8.1.8 Measure to within 0.1 s t

33、he time required for theleading edge of the meniscus to pass between successive pairsof timing marks. Report the first flow time which exceeds 60 sbetween a pair of timing marks, noting the identification of thepair of timing marks.8.1.9 Upon completion of the test, clean the viscometerthoroughly by

34、 several rinsings with an appropriate solventcompletely miscible with the sample, followed by a completelyvolatile solvent. Dry the tube by passing a slow stream offiltered dry air through the capillary for 2 min, or until the lasttrace of solvent is removed. Alternatively, the viscometer maybe clea

35、ned in a glass-cleaning oven, at a temperature not toexceed 500C (932F), followed by rinses with distilled ordeionized water, residue-free acetone, and filtered dry air.Periodically clean the instrument with a strong acid cleaningsolution to remove organic deposits, rinse thoroughly withdistilled wa

36、ter and residue-free acetone, and dry with filtereddry air.8.1.9.1 Chromic acid cleaning solution may be prepared byadding, with the usual precautions, 800 mL of concentratedsulphuric acid to a solution of 92 g of sodium dichromate in458 mL of water. The use of similar commercially availablesulphuri

37、c acid cleaning solutions is acceptable. Nonchromium-containing, strongly oxidizing acid cleaning solutions6may besubstituted so as to avoid the disposal problems of chromium-containing solutions.6Acommercial source for a nonchromium-containing cleaning solution is GodaxLaboratories Inc., 480 Canal

38、St., New York, NY 10013.All dimensions are in millimeters.FIG. 2 Cannon-Manning Vacuum Capillary ViscometerAll dimensions are in millimeters.FIG. 3 Asphalt Institute Vacuum Capillary ViscometerD21710138.1.9.2 Use of alkaline glass cleaning solutions may resultin a change of viscometer calibration, a

39、nd is not recommended.9. Calculation9.1 Select the calibration factor that corresponds to the pairof timing marks used for the determination, as prescribed in8.1.8. Calculate and report the viscosity to three significantfigures using the following equation:Viscosity, Pa s 5 Kt! (1)where:K = selected

40、 calibration factor, Pa s/s, andt = flow time, s.NOTE 5If the viscometer constant or calibration factor (Kcgs)isknown in cgs units (Poise/s) calculate the calibration factor (Ksi) in SIunits (pascalseconds/second) as follows:Ksi 5 Pa s/s! 5 Kcgs/10 or P/s!/10 (2)10. Report10.1 Always report the test

41、 temperature and vacuum withthe viscosity test result. For example, viscosity at 60C (140F)and 300 mm Hg vacuum, in Pa s.11. Precision and Bias11.1 The following criteria (see Note 1) should be used forjudging the acceptability of results (95 % probability):11.1.1 Repeatability Duplicate results by

42、the same opera-tor using the same viscometer should not be considered suspectunless they differ by more than 7 % of their mean.11.1.2 Reproducibility The results submitted by each oftwo laboratories should not be considered suspect unless thetwo results differ by more than 10 % of their mean.APPENDI

43、XES(Nonmandatory Information)X1. CANNON-MANNING VACUUM CAPILLARY VISCOMETER (CMVV)X1.1 ScopeX1.1.1 The Cannon-Manning vacuum capillary viscometer(CMVV)7,8is available in eleven sizes (Table X1.1) coveringa range from 0.0036 to 8 000 Pa s (0.036 to 80 000 P). Sizes10 through 14 are best suited to vis

44、cosity measurements ofasphalt cements at 60C (140F).X1.2 ApparatusX1.2.1 Details of the design and construction of Cannon-Manning vacuum capillary viscometers are shown in Fig. 2.The size numbers, approximate bulb factors, K, and viscosity7Griffith, J. M. and Puzinauskas, P., “Relation of Empirical

45、Tests to FundamentalViscosity ofAsphalt Cement and the Relative Precision of Data Obtained by VariousTests Methods,” Symposium on Fundamental Viscosity of Bituminous Materials,ASTM STP 328, Am. Soc. Testing Mats., ASTTA, 1962, pp. 2044.8Manning, R. E., “Comments on Vacuum Viscometers for Measuring t

46、heViscosity ofAsphalt Cements,” Symposium on Fundamental Viscosity of BituminousMaterials, ASTM STP No. 328, Am. Soc. Testing Mats., ASTTA, 1962, pp. 4447.All dimensions are in millimeters.FIG. 4 Modified Koppers Vacuum Capillary ViscometerTABLE X1.1 Standard Viscometer Sizes, Approximate Calibratio

47、nFactors, K and Viscosity Ranges for Cannon-Manning VacuumCapillary ViscometersViscometerSize NumberApproximate CalibrationFactor, K,A40 kPa (300mm Hg) Vacuum,Pa s/s (P/s/10)Viscosity Range,Pa sBViscosity Range,PBBulb B Bulb C4 0.0002 0.00006 0.0036 to 0.08 0.036 to 0.85 0.0006 0.0002 0.012 to 0.24

48、0.12 to 2.46 0.002 0.0006 0.036 to 0.8 0.36 to 87 0.006 0.002 0.12 to 2.4 1.2 to 248 0.02 0.006 0.36 to 8 3.6 to 809 0.06 0.02 1.2 to 24 12 to 24010 0.2 0.06 3.6 to 80 36 to 80011 0.6 0.2 12 to 240 120 to 2 40012 2.0 0.6 36 to 0.8 360 to 813 6.0 2.0 120 to 2 400 1 200 to 24 00014 20.0 6.0 360 to 8 0

49、00 3 600 to 80 000AExact calibration factors must be determined with viscosity standards.BThe viscosity ranges shown in this table correspond to a filling time of 60 to 400s. Longer flow times (up to 1000 s) may be used.D2171014ranges for the series of Cannon-Manning vacuum capillaryviscometers are given in Table X1.1.X1.2.2 For all viscometer sizes, the volume of measuringbulb C is approximately three times that of bulb B.X1.2.3 A convenient holder can be made by drilling twoholes, 22 and 8 mm in diameter, respect