1、Designation: D 2196 05Standard Test Methods forRheological Properties of Non-Newtonian Materials byRotational (Brookfield type) Viscometer1This standard is issued under the fixed designation D 2196; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se of revision, 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.1. Scope1.1 These te
3、st 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 informationonl
4、y.1.3 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
5、.1 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
6、C consist 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 m
7、easurements 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
8、Test 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
9、before 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 Rotatio
10、nal-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 ThermometerA
11、STM thermometer having a rangefrom 20 to 70C and conforming to the requirements forThermometer 49C as prescribed in Specification E1.5.3 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 vigorous
12、lyshaking the test specimen.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
13、e of the viscometer.Condition the oils as closely as possible to 25.0C (or other1These 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 Pain
14、ts andPaint Materials.Current edition approved July 1, 2005. Published August 2005. Originallyapproved in 1963. Last previous edition approved in 1999 as D 2196 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Boo
15、k of ASTMStandards volume information, refer to the standards Document 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 Inter
16、national, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.agreed-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).
17、Make certain that 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 followingcondi
18、tions: RV series 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
19、guard leg attached.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 vis
20、cometer (61%,equal 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 visco
21、sity with tempera-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
22、 new factors for 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 (T
23、able 1) for the 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-u
24、pon temperatureprior 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 t
25、he specimen from 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,
26、 orother agreed-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
27、 surface of the 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 al
28、ignment. Avoid 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 b
29、yagreement between user and producer.9.4 Lower the viscometer until the groove (immersionmark) on the shaft just touches the material. Adjust theTABLE 1 Factors for Converting Brookfield Dial Readings toMillipascal Seconds (Centipoises)NOTE 1M = 1000.Speed, rpmRV Series Factors Spindles12345 6 70.5
30、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 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 Factor
31、s 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 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
32、 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 %)D2196052viscometer 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 r
33、egionundisturbed 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
34、and switch off 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 d
35、irect reading 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 viscomete
36、r should be agreed 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:
37、V = viscosity 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
38、 specimen temperature 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 BV
39、ISCOSITY UNDER 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 slowes
40、t rotational 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 rec
41、ord thescale 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.N
42、OTE 7It is preferable 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 s
43、peed andrecord 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
44、.2.1 Shear Thinning 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 betweenproduce
45、r and user. The 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-thi
46、nning behavior 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 vis
47、cositytaken with 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
48、the following 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
49、 than that specified.D219605315.2 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 viscosi-ties, for both increasing and decreasing speeds; or ratio of thelowest speed viscosities before and after the rest period, andspeed at which they were measured (14.3).16. Precision and Bias16.1 PrecisionSee Section 23 for precision, including thatfor measurement of the shear thinn
