1、Designation: D4741 17Standard Test Method forMeasuring Viscosity at High Temperature and High ShearRate by Tapered-Plug Viscometer1This standard is issued under the fixed designation D4741; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, 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.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope*1.1 This test me
3、thod2covers the laboratory determination ofthe viscosity of oils at 150 C and 1 106s1and at 100 C and1106s1, using high shear rate tapered-plug viscometermodels BE/C or BS/C.1.2 Newtonian calibration oils are used to adjust the work-ing gap and for calibration of the apparatus. These calibrationoils
4、 cover a range from approximately 1.4 mPas to 5.9 mPas(cP) at 150 C and 4.2 mPas to 18.9 mPas (cP) at 100 C.Thistest method should not be used for extrapolation to higherviscosities than those of the Newtonian calibration oils used forcalibration of the apparatus. If it is so used, the precisionstat
5、ement will no longer apply. The precision has only beendetermined for the viscosity range 1.48 mPas to 5.07 mPas at150 C and from 4.9 mPas to 11.8 mPas at 100 C for thematerials listed in the precision section.1.3 A non-Newtonian reference oil is used to check that theworking conditions are correct.
6、 The exact viscosity appropriateto each batch of this oil is established by testing on a numberof instruments in different laboratories. The agreed value forthis reference oil may be obtained from the chairman of theCoordinating European Council (CEC) Surveillance Group forCEC L-36-90, or from the d
7、istributor.1.4 Applicability to products other than engine oils has notbeen determined in preparing this test method.1.5 This test method uses the millipascal seconds, mPas, asthe unit of viscosity. For information, the equivalent cgs unit,centipoise, cP, is shown in parentheses.1.6 This standard do
8、es 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 determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Sta
9、ndards:3D91 Test Method for Precipitation Number of LubricatingOilsD4683 Test Method for Measuring Viscosity of New andUsed Engine Oils at High Shear Rate and High Tempera-ture by Tapered Bearing Simulator Viscometer at 150 CD5481 Test Method for Measuring Apparent Viscosity atHigh-Temperature and H
10、igh-Shear Rate by Multicell Cap-illary ViscometerD6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsD6708 Practice for Statistical Assessment and Improvementof Expected Agreement Between Two Test Methods thatPurport to Measure the S
11、ame Property of a Material2.2 Coordinating European Council (CEC) Standard:4CEC L-36-90 The Measurement of Lubricant Dynamic Vis-cosity under Conditions of High Shear (Ravenfield)2.3 Energy Institute:5IP 370 Test Method for the Measurement of LubricantDynamicViscosity Under Conditions of High Shear
12、Usingthe Ravenfield Viscometer3. Terminology3.1 Definitions:3.1.1 apparent viscosity, nviscosity of a non-Newtonianliquid determined by this test method at a particular shear rateand shear stress.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, an
13、d Lubricants and is the direct responsibility ofSubcommittee D02.07 on Flow Properties.Current edition approved Jan. 1, 2017. Published February 2017. Originallyapproved in 1987. Last previous edition approved in 2013 as D4741 13. DOI:10.1520/D4741-17.2This test method is technically identical to th
14、at described in CEC L-36-90(under the jurisdiction of the CEC Engine Lubricants Technical Committee) and inIP 370.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to th
15、e standards Document Summary page onthe ASTM website.4Available from Coordinating European Council (CEC), Services provided byKellen Europe, Avenue Jules Bordet 142 - 1140, Brussels, Belgium, http:/www.cectests.org.5Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K.*A Summar
16、y of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established i
17、n the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13.1.2 density, nmass per unit volume of the test liquid at agiven temperature.3.1.2.1 DiscussionIn SI notation, t
18、he unit of density is thekilogram per cubic metre. However, for practical use, gram percubic centimetre is customarily used and is equivalent to103kg/m3.3.1.3 kinematic viscosity, nratio of the viscosity (dynamic,absolute) to the density of the liquid. It is a measure of theresistance to flow of a l
19、iquid where the shear stress (forcecausing flow) is applied by gravity. Kinematic viscosity valuesare thus affected by both the dynamic viscosity (absoluteviscosity) of the liquid and its density.3.1.3.1 DiscussionIn SI, the unit of kinematic viscosity isthe metre squared per second, often convenien
20、tly expressed asmillimetre squared per second and termed the centiStoke.3.1.4 Newtonian oil or liquid, noil or liquid that at a giventemperature exhibits a constant viscosity at all shear rates andshear stresses.3.1.5 non-Newtonian oil or liquid, noil or liquid thatexhibits a viscosity that varies w
21、ith changing shear stress andshear rate.3.1.6 shear rate, nvelocity gradient in liquid flow inmillimetres per second per millimetre (mm/s per mm) resultingfrom applied shear stress; the System International (SI) unit forshear rate is reciprocal seconds, s-1.3.1.7 shear stress, nforce per unit area c
22、ausing liquid flowover the area where viscous shear is being caused; in SI, theunit of shear stress is the Pascal (Pa).3.1.8 viscosity, nratio of applied shear stress and theresulting rate of shear. It is sometimes called dynamic orabsolute viscosity (in contrast to kinematic viscosity, see3.1.3). V
23、iscosity is a measure of the resistance to flow of theliquid at a given temperature.3.1.8.1 DiscussionIn SI, the unit of viscosity is thePascalsecond (Pas), often conveniently expressed asmilliPascalsecond (mPas), which has the English systemequivalent of the centipoise (cP).3.2 Definitions of Terms
24、 Specific to This Standard:3.2.1 calibration oils, nNewtonian oils used to establishthe reference framework of viscosity versus torque in thisinstrument from which the test oil viscosity is determined.3.2.2 non-Newtonian check oil, nnon-Newtonian oil usedto check that the gap or distance between the
25、 rotor and statorwill produce the desired operating shear rate of1106s1.3.2.2.1 DiscussionCheck oil is an acceptable name fornon-Newtonian reference oil.3.2.3 test oil, nany oil for which apparent viscosity is tobe determined.4. Summary of Test Method4.1 The lubricant under test fills the annulus be
26、tween aclose-fitting rotor and stator. The rotor and stator have a slight,matching taper to allow adjustment of the gap and hence theshear rate.The rotor is spun at a known speed, and the lubricantviscosity is determined from measurements of the reactiontorque by reference to a curve prepared using
27、Newtoniancalibration oils.5. Significance and Use5.1 Viscosity measured under the conditions of this testmethod is considered to be representative of that at thetemperatures and shear rates but not the pressures in the journalbearings of internal combustion engines under operating con-ditions.5.2 Th
28、e relevance of these conditions to the measurement ofengine-oil viscosity has been discussed in many publications.65.3 The high temperature high shear (HTHS) viscosity atthis shear rate can be measured at other temperatures using thisapparatus. This is achieved by the use of a different range ofNewt
29、onian calibration fluids. . The precision has not beenstudied for any temperature or viscosity range not noted in theprecision section.6. Apparatus6.1 Tapered-Plug High Shear Rate Viscometer, Model BE/C(single speed) or BS/C (multi-speed).7The viscometer uses arotating tapered plug in a matched stat
30、or.NOTE 1Model BE/C has a restricted torque range and may not becapable of measuring higher viscosities at 100 C.6.2 Vacuum Extract Pipe, to ensure constant oil level. Theextract pipe is supplied with all current models.6.3 Calibration Weight (supplied with instrument).6.4 Thermostatically Controlle
31、d Heating Bath, with fluidcirculator. For acceptable temperature control and recoverytime, the temperature difference between the bath and mea-surement head should be targeted at 4 C and shall not exceed8 C. This temperature difference is influenced by the natureand rate of flow of the circulating f
32、luid; the length and bore ofthe heating pipes; and the viscosity of the bath fluid.NOTE 2Bath oil with kinematic viscosity not greater than 10 mm2/s at150 C is recommended.6.5 A means of measuring temperature is not necessary forcurrent instruments since a precision temperature sensor is nowbuilt-in
33、. For older instruments still in the field, a device with aprecision not worse than 60.20 C is necessary.6.6 The use of an ultrasonic cleaner is recommended.6.7 The manufacturer offers a package incorporating all theabove and including the necessary calibration oils, referenceoils, and bath oil.6.8
34、Vacuum Pump, with suitable liquid trap.6For a comprehensive review, see “The Relationship Between High-Temperature Oil Rheology and Engine Operation,” ASTM Data Series Publication62 (out of print).7The sole source of supply of the apparatus known to the committee at this timeis Cannon Instrument Co.
35、, State College, PA 16803, http:/. If you are aware of alternative suppliers, pleaseprovide this information to ASTM International Headquarters. Your comments willreceive careful consideration at a meeting of the responsible technical committee,1which you may attend.D4741 1727. Materials7.1 Newtonia
36、n Calibration Oils8CEC Reference Oils RL102, RL 103, RL 104, RL 105, RL 106, and RL 107. CannonCertified Viscosity Reference Standard HT22 (nominal viscos-ity of 1.5 mPas at 150 C).7.2 Non-Newtonian Reference Oil8CEC Reference Oil RL232.7.3 Washing SolventASTM precipitation naphtha asspecified inTes
37、t Method D91 or a suitable replacement solvent.(WARNING Extremely flammable. Vapors may cause flashfire. See Annex A1.)7.4 Flushing SolventWhile spirit or Stoddard solvent.8. Sampling8.1 Test oils that are visually free from haze and particulatesneed not be filtered before evaluation.Asample shall b
38、e free ofparticles larger than 3 m. If heavy concentration of smallerparticles is still visible after filtration through a filter of poresize 3 m, it is recommended to reduce their concentration byfurther filtration. This will reduce the possibility of the par-ticles wedging in the measurement gap a
39、nd so causing erosionof the rotor/stator or erroneous readings. Do not filter formu-lated oils through pore sizes below 1 m because certainlubricant additives may be removed.8.2 Used oils may also be tested in these instruments,though no precision statement is available for these materials.8.2.1 Fil
40、ter used oils through a suitable filter such asWhatman GF/C fibreglass filter. The process of filtration isgreatly accelerated by either warming or applying pressure.Procedures shall be such that all risk of particulate contamina-tion is avoided.NOTE 3Suggestions have been made that the process of f
41、iltration mayitself cause a change of viscosity by the removal of particles. No doubt ifthere is a very heavy concentration of particles greater than 3 m, this willbe so. It is not expected or intended that this test method will be used forsuch oils. Evidence to date is that filtration of used oils
42、from normalengines in normal periods of use is acceptable. It is, however, advisable touse pressure filtration rather than vacuum filtration so that volatilecomponents will not be removed. No precision statement is available forused oils.9. Initial Preparation of Apparatus9.1 These instructions rela
43、te to instruments incorporating acomputer, in other words, Models BE/C and BS/C. Changesfrom earlier editions of this test method are those given in10.1.5, 10.5.1, 10.5.2, 11.1.2, and 11.1.3 and the use of avacuum extract pipe to ensure constant oil level (see 6.2).9.2 Set up the apparatus in accord
44、ance with the manufac-turers manual. Attach the funnel to the side arm, using therubber sleeve provided.NOTE 4The funnel has a larger bore than stock funnels in order toincrease the rate of flow of oil samples.9.3 It is recommended that the instrument is NOT mountedin a fume cupboard since this draw
45、s in dirt particles. Localextraction over the heating bath is all that is necessary since themanufacturers bath is practically sealed.9.4 When setting up the apparatus, a torque calibration shallbe performed following the instructions in the manufacturersmanual.9.5 The instrument is supplied by the
46、manufacturer with allother functions already calibrated and set up. It is recom-mended that these other initial settings be accepted untilsufficient familiarity is obtained with the use of the apparatus.When it is desired to modify the initial settings, full instruc-tions will be found in the manufa
47、cturers manual.9.6 It is advisable to gain access to the list of calibration oilsheld in the memory of the instrument in order to be familiarwith its contents and to check that it is in accordance with thestandards actually supplied.9.7 Preparation of Apparatus on All Other Occasions:9.7.1 Turn on t
48、he heating bath.9.7.2 Flush out the measurement chamber using washingsolvent.9.7.3 Refill the measurement chamber with Reference OilRL 232.9.7.4 Leave for not less than half an hour for temperature tostabilise.9.7.4.1 If the bath does not reach correct temperature in thistime, then either extend thi
49、s period or, preferably, address theproblem of why heating is slow.10. Procedure10.1 Outline of Method:10.1.1 The lubricant under test fills the annulus between aclose-fitting rotor and stator. The rotor and stator have agradual matching taper to allow adjustment of the gap andhence the shear rate. Spin the rotor at a known speed anddetermine the lubricant viscosity from measurements of thereaction torque by reference to a line prepared using Newto-nian calibration oils.10.1.2 Use N
