1、Designation: D 2162 06An American National StandardStandard Practice forBasic Calibration of Master Viscometers and Viscosity OilStandards1This standard is issued under the fixed designation D 2162; 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. Scope*1.1 This pr
3、actice covers the calibration of master viscom-eters and viscosity oil standards, both of which may be used tocalibrate routine viscometers as described in Test MethodD 445 and Specifications D 446 over the temperature rangefrom 15 to 100C.1.2 The calibration constants in mm2/s2are to be regardedas
4、the standard. The kinematic viscosities in mm2/s are to beregarded as the standard.1.3 This standard does 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
5、determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see Section 7.2. Referenced Documents2.1 ASTM Standards:2D 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D 446 Specifications and Ope
6、rating Instructions for GlassCapillary Kinematic ViscometersD 1193 Specification for Reagent WaterD 1250 Guide for Use of the Petroleum MeasurementTablesD 1480 Test Method for Density and Relative Density(Specific Gravity) of Viscous Materials by Bingham Pyc-nometerD 1590 Test Methods for Surface Te
7、nsion of Water andWaste Water3E1 Specification for ASTM Liquid-in-Glass Thermometers2.2 ISO Standard:4ISO 3666 Viscosity of Water3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 basic calibration, ncalibration based on the primarystandard, water.3.1.1.1 DiscussionPure water has
8、 a kinematic viscosity of1.0034 mm2/s (cSt) at 20C. See ISO 3666.3.1.2 master viscometer, nglass capillary viscometer witha liquid driving head of at least 400 mm.3.1.2.1 DiscussionIt is specially designed to minimizeerrors due to surface tension, kinetic energy, and capillary endeffects.3.1.3 visco
9、sity oil standard, nstable Newtonian liquid, thekinematic viscosity of which has been related to the kinematicviscosity of water through the step-up procedure described inthis practice.4. Summary of Practice4.1 Two or more master viscometers, having calibrationconstants in the 0.001 to 0.003-mm2/s2(
10、cSt/s) range, arecalibrated with water at 20C. The kinematic viscosities of twoor more oil standards are measured at 40C in these two masterviscometers. Corrections are made for buoyancy and, wherenecessary, for temperature and surface tension.4.2 Athird master viscometer, with a calibration constan
11、t of0.003 to 0.009 mm2/s2(cSt/s), is then calibrated at 40C withthe two standard oils and its calibration factor calculated atstandard conditions for water at 20C. In like manner addi-tional viscosity oil standards and additional master viscometersare calibrated at 40C using the average results from
12、 at leasttwo master viscometers or two oil standards. Steps betweensuccessive calibration constants or viscosities increase by afactor of three or less until the desired viscosity range iscovered.4.3 Oils are calibrated at other temperatures using theaverage result from at least two master viscomete
13、rs.1This practice is under the jurisdiction of ASTM Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.07 onFlow Properties.Current edition approved May 1, 2006. Published May 2006. Originallyapproved in 1963. Last previous edition approved in 2004
14、 as D 216299(2004).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 Document Summary page onthe ASTM website.3Withdrawn.4Available from American Nation
15、al Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 Because there ar
16、e surface tension or kinematic viscositydifferences, or both, between the primary standard (7.4) andkinematic viscosity standards (7.5), special procedures usingmaster viscometers are required to “step-up” from the kine-matic viscosity of the primary standard to the kinematicviscosities of oil stand
17、ards.5.2 Using master viscometers calibrated according to thispractice, an operator can calibrate kinematic viscometers inaccordance with Specifications D 446.5.3 Using viscosity oil standards established in this practice,an operator can calibrate kinematic viscometers in accordancewith Specificatio
18、ns D 446.6. Apparatus6.1 Master Viscometers: Cannon5or Ubbelohde6TypeAcceptable viscometers are shown in Fig. 1 and Fig. 2.Twomasters are required with calibration constants in the 0.001 to0.003-mm2/s2(cSt/s) range. Additional masters have factorsincreasing in three-fold steps.6.2 ThermometersKinema
19、tic viscosity thermometers hav-ing a range from 18.5 to 21.5C, or 38.5 to 41.5C, and5Cannon, M. R., “Viscosity Measurement, Master Viscometers,” Industrial andEngineering Chemistry. Analytical Edition, Vol 16, 1944, p. 708.6Ubbelohde, L., “The Suspended Lever Viscometer,” Journal Institute Petro-leu
20、m Technologists (London), Vol 22, 1936, p. 37.FIG. 1 Cannon Master ViscometerD2162062conforming to the requirements for Thermometers 44C and120C, as prescribed in Specification E1, and calibrated to0.005C by the National Institute of Standards and Technologyor other qualified agency. A standard plat
21、inum resistancethermometer together with a Mueller resistance bridge havingequivalent or better accuracy is preferable, where available.Other Thermometers 46C, 121C, etc. as required for standard-izing oil viscosities at other temperatures may be used.6.3 BathA thermostated bath containing water or
22、othertransparent liquid deep enough to immerse the master viscom-eters so that the upper fiducial mark is at least 50 mm below thesurface. The efficiency of stirring and the balance between heatloss and input must be such that the temperature of the waterdoes not vary by more than 60.01C over the le
23、ngth of theviscometer or from one viscometer position to another. Theworking section of the bath should be shielded from directradiation from heaters and lights. A standard platinum resis-tance thermometer, approximately 450 mm in length, may beused to ensure that the variation in temperature does n
24、ot exceed60.01C. Firm supports should be provided to hold the masterviscometer in a rigid and reproducible position within 0 15min of vertical.6.4 TimerEither a spring-wound or electric timer capableof measuring time intervals of 300 to 10 000 s with an accuracyof 60.03 %. The stop watch, fully but
25、not tightly wound, mustbe used and tested in the same position. For example, if usedat 45 inclination, it should have been tested previously in thatposition. Electric timers must be operated on circuits, theFIG. 2 Ubbelohde Master ViscometerD2162063frequencies of which are controlled. Commercial pow
26、ersources, the frequencies of which are intermittently and notcontinuously controlled, are not satisfactory. Both mechanicaland electric timers can be sensitive to abnormally low ambienttemperature and should not be used when cold.NOTE 1Time signals as broadcast by the National Institute of Stan-dar
27、ds and Technology are a convenient and primary standard reference forcalibrating timing devices. The following can be used:WWV Fort Collins, CO 2.5, 5, 10, 15, 20 MHzWWVH Kauai, HI 2.5, 5, 10, 15 MHzCHU Ottawa, Canada 3.33, 7.335, 14.67 MHzRadio broadcast of voice and audio on a telephone line at ph
28、one number: 303-499-7111. Additional time services are available from the National Institute ofStandards and Technology.7. Reagents7.1 Acetone, reagent grade. (WarningExtremely flam-mable.)7.2 Chromic Acid Cleaning Solution Carefully pour 1 Lof concentrated sulfuric acid (H2SO4, relative density 1.8
29、4)into 35 mL of a saturated solution of technical grade sodiumdichromate (Na2Cr2O7) in water. Strongly oxidizing acidcleaning solutions containing no chromium7may be substi-tuted to avoid disposal problems of chromium-containingsolutions. (WarningCauses severe burns.)7.3 Petroleum Spirit, or other s
30、olvent completely misciblewith petroleum oils. (WarningCombustible. Vapor harm-ful.)7.4 Primary Standard Water, deionized or distilled, thendistilled fresh the same day of use. Store in a glass-stopperedchromic acid-cleaned bottle of borosilicate glass. See Specifi-cation D 1193.7.5 Viscosity Oil St
31、andardsStable petroleum oils selectedto cover the desired kinematic viscosity range. They should betransparent and have vapor pressures below 10 mmHg at 40C.Store away from heat and light in suitable containers, prefer-ably glass.8. Calibration of Master Viscometers with Water at 20C8.1 Maintain the
32、 water bath at 20 6 0.01C applying thenecessary thermometer corrections. Two check thermometersare recommended to detect any change in calibration.8.2 Clean a master viscometer having a calibration constantof 0.001 to 0.003 mm2/s2(cSt/s) with chromic acid cleaningsolution to remove organic deposits,
33、 rinse thoroughly withdistilled water and acetone and dry with a stream of filtered air.8.3 Clean a 50-mL Erlenmeyer flask with cleaning solutionand rinse thoroughly with distilled water. Add freshly distilledprimary standard water and bring to a boil to remove dissolvedgases. Cover the flask to pre
34、vent entrance of dust and allow tocool. If a Cannon master viscometer is being calibrated, coolthe water to 20 6 3C.8.4 Charge the Cannon master as follows:8.4.1 Connect a rubber tube to large arm J. Invert theviscometer and dip the end of small arm A into the beaker ofwater. Apply suction to arm J
35、and draw liquid through bulbs Band D to etched line E. Turn the viscometer back to its normalvertical position, wipe tube A clean, insert the viscometer intoa holder and place it in the constant temperature bath.8.4.2 Support the master viscometer firmly and align it in avertical position with the a
36、id of a plumb bob with a length ofabout 560 mm. One can be made by use of a cork to fit the largetube J, a piece of thread, and an 18-mm length of 3-mmdiameter solder lead. Remove the cork (or slot it) during thetest so that no back pressure is developed.8.5 Charge the Ubbelohde master as follows:8.
37、5.1 Tilt the instrument about 30 from the vertical withbulb A below the capillary and then introduce enough waterinto large arm 1 to bring the level up to the lower filling line.The level should not be above the upper filling line when theviscometer is returned to the vertical position and the liqui
38、d hasbeen drained from tube 1. Charge the viscometer in such amanner that the U-tube at the bottom fills completely withouttrapping air.8.5.2 Place the viscometer into a holder and place it in theconstant temperature bath. Align the large tube 1 in a verticalposition with a plumb bob as described fo
39、r the Cannon master.8.6 Allow the charged viscometer to stand in the bath longenough for the sample to reach bath temperature. Fifteenminutes are usually sufficient.8.7 With gentle vacuum or pressure, force the liquid about5 mm above the upper timing mark. Avoid splashing liquid inthe upper bulb or
40、forming any bubbles in the liquid. Whenusing a Ubbelohde viscometer, hold a finger over the upper endof tube 3 during this operation; then remove it and immediatelyplace it over tube 2 until the liquid drops away from the lowerend of the capillary.8.8 Measure the efflux of water from upper to lower
41、timingmark (which should be 300 s or more) to the nearest 0.1 s.Repeat this measurement two additional times and average ifthe lowest and highest times agree within 0.1 %. If themeasurements do not agree within this tolerance, repeat theprocedure paying particular attention to cleaning the viscom-et
42、er, filtering the sample, avoiding contamination during fillingand afterwards, checking the temperature control and thetiming device.8.9 Clean the viscometer and dry with filtered air. Reloadthe viscometer and measure the efflux time in triplicate.Average if the lowest and highest times agree within
43、 0.1 %.8.10 If the two average times fall within 0.1 %, average thetwo to obtain an average of the two fills.8.11 Calculate the viscometer constant as follows:c 5 1.0034/t (1)where:c = calibration constant of the viscometer with water at20C, mm2/s2(cSt/s), andt = efflux time, s.8.12 Repeat the opera
44、tions described in 8.1 through 8.8 witha second master viscometer having a constant not greater than0.003 mm2/s2(cSt/s2).7The sole source of supply of non-chromium containing cleaning solutionknown to the committee at this time is Godax Laboratories Inc., 480 Canal Street,New York, NY 10013. If you
45、are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.D2162064NOTE 2Normally master viscometers are calibrated and used in thesame
46、 location. If subsequently the viscometer is used at a laboratory otherthan the calibrating one, the c constant should be corrected for thedifference in the acceleration of gravity, g at the two locations as follows:c25 g2/ g1! 3 c1(2)where:c2and g2= calibration constant and gravity at the new locat
47、ions,andc1and g1= calibration constant and gravity at the original location.Certificates for viscometers should state the value of g at the location ofthe calibrating laboratory. Failure to correct a viscometer constant forchange of gravity can result in errors as high as 0.2 %, which is twice theer
48、ror permitted between checks in this test method.9. Calibration of Viscosity Oil Standards at 40C9.1 Choose an oil with a kinematic viscosity of about 3mm2/s (cSt/s) at 40C. Filter a portion into a clean beakerthrough a 200-mesh (75-m) sieve, or other suitable filter, toremove dirt or sediment. If n
49、ecessary, adjust the temperature ofthe oil to within 3C of 20C.9.2 Adjust the temperature of the bath to 40 6 0.01Capplying the necessary thermometer corrections.NOTE 3The procedure is given for 40C because kinematic viscosi-ties of petroleum oils are traditionally measured at this temperature and soviscosity oil standards at 40C are in common use. Master viscometersmay, however, be calibrated at any convenient bath temperature and used,with any necessary corrections, at other temperatures.9.3 Charge one of the master viscometers, already
