1、Designation: D2196 10Standard Test Methods forRheological Properties of Non-Newtonian Materials byRotational (Brookfield type) Viscometer1This standard is issued under the fixed designation D2196; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、 of revision, 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 Department of Defense.1. Scope1.1 These test
3、methods cover the determination of theapparent viscosity and the shear thinning and thixotropicproperties of non-Newtonian materials in the shear rate rangefrom 0.1 to 50 s1.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1
4、.3 This standard does not purport to address the safetyconcerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1
5、ASTM Standards:2E1 Specification for ASTM Liquid-in-Glass Thermometers3. Summary of Test Method3.1 Test Method A consists of determining the apparentviscosity of coatings and related materials by measuring thetorque on a spindle rotating at a constant speed in the material.3.2 Test Methods B and C c
6、onsist of determining the shearthinning and thixotropic (time-dependent) rheological proper-ties of the materials.3The viscosities of these materials aredetermined at a series of prescribed speeds of a rotational-typeviscometer. The agitation of the material immediately preced-ing the viscosity meas
7、urements is carefully controlled.4. Significance and Use4.1 Test Method A is used for determining the apparentviscosity at a given rotational speed, although viscosities at twoor more speeds give better characterization of a non-Newtonianmaterial than does a single viscosity measurement.4.2 With Tes
8、t Methods B and C, the extent of shear thinningis indicated by the drop in viscosity with increasing viscometerspeed. The degree of thixotropy is indicated by comparison ofviscosities at increasing and decreasing viscometer speeds(Test Method B), viscosity recovery (Test Method B), orviscosities bef
9、ore and after high shear (combination of TestMethods B and C). The high-shear treatment in Test Method Capproximates shearing during paint application. The viscositybehavior measured after high shear is indicative of the char-acteristics of the paint soon after application.5. Apparatus5.1 Rotational
10、-type viscometers having at least four speeds,such as:5.1.1 Brookfield Dial-Reading (Analog) Viscometer,orequivalent having multiple rotational speeds with set ofspindles; or5.1.2 Brookfield Digital Viscometer, or equivalent havingmultiple rotational speeds, with set of spindles.5.2 ThermometerASTM
11、thermometer having a rangefrom 20 to 70C and conforming to the requirements forThermometer 49C as prescribed in Specification E1. In addi-tion, temperature measuring devices such as non-mercuryliquid-in-glass thermometers, thermocouples, or platinum re-sistance thermometers that provide equivalent o
12、r better accu-racy and precision, that cover the temperature range forthermometer 49C, may be used.5.3 Containers, round 0.5-L (1-pt) can, 85 mm (338 in.) indiameter, or 1-L (1-qt) can, 100 mm (4 in.) in diameter.5.4 Shaker, or equivalent machine capable of vigorouslyshaking the test specimen.1These
13、 test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.24 on Physical Properties of Liquid Paints andPaint Materials.Current edition approved July 1, 2010. Published July 2010. Orig
14、inally approvedin 1963. Last previous edition approved in 2005 as D2196 05. DOI: 10.1520/D2196-10.2For 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 the standards Docu
15、ment Summary page onthe ASTM website.3Pierce, P. E., “Measurement of Rheology of Thixotropic Organic Coatings andResins with the Brookfield Viscometer,” Journal of Paint Technology, Vol 43, No.557, 1971, pp. 3543.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, P
16、A 19428-2959, United States.6. Materials6.1 Standard Oils, calibrated in absolute viscosity, millipas-cal seconds.7. Calibration of Apparatus7.1 Select at least two standard oils of viscosities differingby at least 0.5 Pas (5P) within the viscosity range of thematerial being measured and in the rang
17、e of the viscometer.Condition the oils as closely as possible to 25.0C (or otheragreed-upon temperature) for1hina0.5-L (1-pt) can, 85 mm(338 in.) in diameter. Measure the viscosities of each oil asdescribed in Test Method B (Section 13) taking readings onlyat increasing speeds (13.4). Make certain t
18、hat the spindle iscentered in the container prior to taking measurements.NOTE 1The Brookfield LV and RV series viscometers are equippedwith a spindle guard leg. The spindle/speed multiplying factors (Table 1)are designed for use with the guard leg in place except for the followingconditions: RV seri
19、es when the factors are the same with or without theguard leg for spindles No. 3 through 7; or LV series when the factors arethe same with or without the guard leg for spindles No. 3 and 4.7.1.1 Calibration in a 0.5-L (1-pt) can is always possiblewith the LV series viscometer with the guard leg atta
20、ched.Calibration of the RV series viscometer in the 1-pt can must bedone with spindles No. 3 through 7 without the guard leg. If theNo. 1 or No. 2 spindles are to be used, calibration is carried outin the 1-L (1-qt) can with the guard leg attached.7.2 Combining the tolerance of the viscometer (61%,e
21、qual to the spindle/speed factor) and the tolerance of thetemperature control (typically 60.5C at 25C) it is reasonableto assume that a viscometer is calibrated if the calculatedviscosities are within 65 % of the stated values (seeTable 2 forexamples of the considerable change in viscosity with temp
22、era-ture exhibited by standard oils). If measurements are not madeat 25C, then the stated viscosities should be corrected to thetemperature at which they are measured. If the viscositiesdetermined in 7.1 differ from the stated values of the viscositystandard by more than 5 %, calculate new factors f
23、or eachspindle/speed combination as follows:f 5 V/s (1)where:f = new factor for converting scale reading to viscosity,mPas (cP),V = viscosity of standard oil, mPas, ands = scale reading of the viscometer.7.3 Prepare a table of new factors similar to that furnishedwith the viscometer (Table 1) for th
24、e spindle/speed combina-tions worked out in 7.2. Spindle/speed factors vary inverselywith speed.8. Preparation of Specimen8.1 Fill a 1-pt or 1-qt can with sample to within 25 mm (1in.) of the top with the sample and bring it as close as possibleto a temperature of 25C or other agreed-upon temperatur
25、eprior to test.8.2 Vigorously shake the specimen on the shaker or equiva-lent for 10 min, remove it from the shaker, and allow it to standundisturbed for 60 min at 25C prior to testing (Note 2). Startthe test no later than 65 min after removing the can from theshaker. Do not transfer the specimen fr
26、om the container inwhich it was shaken.NOTE 2Shake time may be reduced if necessary, or as agreed uponbetween the purchaser and manufacturer, but, in any case, should not beless than 3 min.TEST METHOD AAPPARENT VISCOSITY9. Procedure9.1 Make all measurements as close as possible to 25C, orother agree
27、d-upon temperature.9.2 Place the instrument on the adjustable stand. Lower theviscometer to a level that will immerse the spindle to the properdepth. Level the instrument using the attached spirit level.9.3 Tilt the selected spindle (Note 3), insert it into one sideof the center of the surface of th
28、e material, and attach thespindle to the instrument as follows: Firmly hold the uppershaft coupling with thumb and forefinger; screw left-handthread spindle coupling securely to the upper shaft couplingbeing very careful when connecting to avoid undue sidepressure which might affect alignment. Avoid
29、 rotating the dialso that pointer touches the stops at either extreme of the scale.NOTE 3Select the spindle/speed combination that will give a mini-mum scale reading of 10 but preferably in the middle or upper portion ofthe scale. The speed and spindle to be used may differ from this byagreement bet
30、ween user and producer.TABLE 1 Factors for Converting Brookfield Dial Readings toMillipascal Seconds (Centipoises)NOTE 1M = 1000.Speed, rpmRV Series Factors Spindles12345 6 70.5 200 800 2000 4000 8000 20M 80M1 100 400 1000 2000 4000 10M 40M2 50 200 500 1000 2000 5M 20M2.5 40 160 400 800 1600 4M 16M4
31、 25 100 250 500 1000 2.5M 10M5 20 80 200 400 800 2M 8M10 10 40 100 200 400 1M 4M20 5 20 50 100 200 500 2M50 2 8 20 40 80 200 800100 1 4 10 20 40 100 400Speed, rpmLV Series Factors Spindles123 40.3 200 1000 4000 20M0.6 100 500 2000 10M1.5 40 200 800 4M3.0 20 100 400 2M6 10 50 200 1M12 5 25 100 50030
32、2 10 40 20060 1 5 20 100TABLE 2 Viscosity Variation of Cannon Viscosity StandardsAbout the 25C Temperature PointCannon ViscosityStandardViscosity at 25C,mPas (cP)Viscosity Change With + 1Cat 25C, mPas (cP)S-600 1 400 87.7 (6.26 %)S-2000 4 900 332 (6.77 %)S-8000 20 000 1462.3 (7.31 %)D2196 1029.4 Low
33、er the viscometer until the groove (immersionmark) on the shaft just touches the material. Adjust theviscometer level if necessary. Move the container slowly in ahorizontal plane until the spindle is located in approximatelythe center of the container so that the test will be run in a regionundistur
34、bed by the lowering of the spindle.9.5 Dial-Reading ViscometerTurn on the viscometer. Ad-just the viscometer to the rpm selected (Note 3) for the materialunder test. Allow the viscometer to run until the pointer hasstabilized (Note 4).After the pointer has stabilized, depress theclutch and switch of
35、f the motor so that when it stops, thepointer will be in view (Note 5).9.6 Digital ViscometerTurn on the viscometer. Adjust theviscometer to the rpm selected for the material under test.Allow the viscometer to run until the digital reading hasstabilized. The digital viscometer gives a direct reading
36、 incentipoises, mPa.NOTE 4In thixotropic paints, the pointer or digital reading does notalways stabilize. On occasion it reaches a peak and then gradually declinesas the structure is broken down. In these cases, the time of rotation ornumber of revolutions prior to reading the viscometer should be a
37、greed tobetween user and manufacturer.NOTE 5Always release the clutch while the spindle is still immersedso that the pointer will float, rather than snap back to zero.10. Calculation (Dial Reading Viscometer)10.1 Calculate the apparent viscosity at each speed, asfollows:V 5 fs (2)where:V = viscosity
38、 of sample in centipoises, mPas,f = scale factor furnished with instrument (see Table 1),ands = scale reading of viscometer.11. Report11.1 Report the following information:11.1.1 The viscometer manufacturer, model and spindle,11.1.2 The viscosity at the spindle/speed utilized,11.1.3 The specimen tem
39、perature in degrees Celsius, and11.1.4 The shake time and rest period, if other than speci-fied.12. Precision and Bias12.1 PrecisionSee Section 23 for precision, including thatfor measurement at a single speed.12.2 BiasNo statement of bias is possible with this testmethod.TEST METHOD BVISCOSITY UNDE
40、R CHANGINGSPEED CONDITIONS, DEGREE OF SHEARTHINNING AND THIXOTROPY13. Procedure13.1 Make all measurements with the viscometer as close aspossible to 25C, or other agreed upon temperature.13.2 Adjust the instrument and attach the spindle as in9.2-9.4.13.3 Set the viscometer at the slowest rotational
41、speed (Note5 and Note 6). Start the viscometer and record the scale readingafter ten revolutions (or other agreed-upon number of revolu-tions).NOTE 6A higher initial rotational speed may be used upon agreementbetween producer and user.13.4 Increase the viscometer speed step-wise and record thescale
42、reading after ten revolutions (or equivalent time for eachspindle/speed combination) at each speed.After an observationhas been made at the top speed, decrease the speed in steps tothe slowest speed, recording the scale reading after ten revo-lutions (or equivalent time) at each speed.NOTE 7It is pr
43、eferable to change speed when the motor is running.13.5 After the last reading has been taken at the slowestspeed, shut off the viscometer and allow it and the specimen tostand undisturbed for an agreed-upon rest period.At the end ofthe rest period, start the viscometer at the slowest speed andrecor
44、d the scale reading after ten revolutions (or other agreed-upon number of revolutions).14. Calculations and Interpretation of Results14.1 Calculate the apparent viscosity at each speed asshown in Section 9.14.2 If desired, determine the degree of shear thinning bythe following method:14.2.1 Shear Th
45、inning Index (sometimes erroneously calledthe thixotropic index)Divide the apparent viscosity at a lowrotational speed by the viscosity at a speed ten times higher.Typical speed combinations are 2 and 20 rpm, 5 and 50 rpm, 6and 60 rpm but selection is subject to agreement betweenproducer and user. T
46、he resultant viscosity ratio is an index ofthe degree of shear thinning over that range of rotational speedwith higher ratios indicating greater shear thinning.14.2.2 A regular or log-log plot of viscosity versus viscom-eter speed in rpm may also be useful in characterizing theshear-thinning behavio
47、r of the material. Such plots may beused for making comparisons between paints or other materi-als.14.3 If desired, estimate the degree of thixotropy (underconditions of limited shearing-out of structure) by one of thefollowing methods:14.3.1 Calculate the ratio of the slowest speed viscositytaken w
48、ith increasing speed to that with decreasing speed. Thehigher the ratio, the greater the thixotropy.14.3.2 Calculate the ratio of the slowest speed viscositytaken after the rest period to that before the rest period. Thehigher the ratio, the greater the thixotropy.15. Report15.1 Report the following
49、 information:15.1.1 The viscometer manufacturer, model and spindle,15.1.2 The viscosities at increasing and decreasing spindlespeeds,15.1.3 The rest period time and the viscosity at the end ofthat time,15.1.4 The specimen temperature in degrees Celsius, and15.1.5 The shake time if other than that specified.D2196 10315.2 Optional Reporting:15.2.1 Degree of Shear ThinningShear thinning index andspeeds over which it was measured (14.2).15.2.2 Estimated Degree of Thixotropy (under conditions ofshearing-out of structure)Ratio of the lowest speed
