Standard Test Method for Basic Calibration of Master Viscometers and Viscosity Oil Standards

SCOPE
1.1 This test method covers the calibration of master viscometers and viscosity oil standards, both of which may be used to calibrate routine viscometers as described in Test Method D 445 and Specifications D 446 over the temperature range from 15 to 100°C.
1.2 The calibration constants in mm2/s 2 are to be regarded as the standard. The kinematic viscosities in mm2/s are to be regarded as the standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see Section 7.

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ASTM D2162-99(2004) - Standard Test Method for Basic Calibration of Master Viscometers and Viscosity Oil Standards
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
An American National Standard
Designation:D2162–99 (Reapproved 2004)
Standard Test Method for
Basic Calibration of Master Viscometers and Viscosity Oil
Standards
This standard is issued under the fixed designation D2162; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript 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 2.2 ISO Standard:
ISO 3666 Viscosity of Water
1.1 This test method covers the calibration of master vis-
cometers and viscosity oil standards, both of which may be
3. Terminology
used to calibrate routine viscometers as described in Test
3.1 Definitions of Terms Specific to This Standard:
Method D445 and Specifications D446 over the temperature
3.1.1 basic calibration, n—calibrationbasedontheprimary
range from 15 to 100°C.
2 2 standard, water.
1.2 The calibration constants in mm /s are to be regarded
3.1.1.1 Discussion—Purewaterhasakinematicviscosityof
as the standard. The kinematic viscosities in mm /s are to be
1.0034 mm /s (cSt) at 20°C. See ISO 3666.
regarded as the standard.
3.1.2 master viscometer, n—glasscapillaryviscometerwith
1.3 This standard does not purport to address all of the
a liquid driving head of at least 400mm.
safety concerns, if any, associated with its use. It is the
3.1.2.1 Discussion—It is specially designed to minimize
responsibility of the user of this standard to establish appro-
errors due to surface tension, kinetic energy, and capillary end
priate safety and health practices and determine the applica-
effects.
bility of regulatory limitations prior to use. For specific
3.1.3 viscosity oil standard, n—stableNewtonianliquid,the
warning statements, see Section 7.
kinematic viscosity of which has been related to the kinematic
2. Referenced Documents viscosity of water through the step-up procedure described in
this test method.
2.1 ASTM Standards:
D445 Test Method for Kinematic Viscosity of Transparent
4. Summary of Test Method
and Opaque Liquids (and the Calculation of Dynamic
4.1 Two or more master viscometers, having calibration
Viscosity)
2 2
constants in the 0.001 to 0.003-mm /s (cSt/s) range, are
D446 Specifications and Operating Instructions for Glass
calibratedwithwaterat20°C.Thekinematicviscositiesoftwo
Capillary Kinematic Viscometers
ormoreoilstandardsaremeasuredat40°Cinthesetwomaster
D1193 Specification for Reagent Water
viscometers. Corrections are made for buoyancy and, where
D1250 Guide for Use of the Petroleum Measurement
necessary, for temperature and surface tension.
Tables
4.2 Athirdmasterviscometer,withacalibrationconstantof
D1480 Test Method for Density and Relative Density
2 2
0.003 to 0.009 mm /s (cSt/s), is then calibrated at 40°C with
(Specific Gravity) of Viscous Materials by Bingham Pyc-
the two standard oils and its calibration factor calculated at
nometer
standard conditions for water at 20°C. In like manner addi-
D1590 Test Methods for Surface Tension of Water and
3 tionalviscosityoilstandardsandadditionalmasterviscometers
Waste Water
are calibrated at 40°C using the average results from at least
E1 Specification forASTM Liquid-in-GlassThermometers
two master viscometers or two oil standards. Steps between
successive calibration constants or viscosities increase by a
factor of three or less until the desired viscosity range is
This test method is under the jurisdiction of ASTM Committee D02 on
covered.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.07 on Flow Properties.
4.3 Oils are calibrated at other temperatures using the
Current edition approved May 1, 2004. Published June 2004. Originally
average result from at least two master viscometers.
e1
approved in 1963. Last previous edition approved in 1999 as D2162–99 .
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
Withdrawn. 4th Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2162–99 (2004)
FIG. 1 Cannon Master Viscometer
5. Significance and Use 6. Apparatus
5 6
5.1 Because there are surface tension or kinematic viscosity 6.1 Master Viscometers: Cannon or Ubbelohde Type—
differences, or both, between the primary standard (7.4) and Acceptable viscometers are shown in Fig. 1 and Fig. 2. Two
kinematic viscosity standards (7.5), special procedures using masters are required with calibration constants in the 0.001 to
2 2
master viscometers are required to “step-up” from the kine- 0.003-mm /s (cSt/s) range. Additional masters have factors
matic viscosity of the primary standard to the kinematic increasing in three-fold steps.
viscosities of oil standards. 6.2 Thermometers—Kinematicviscositythermometershav-
5.2 Using master viscometers calibrated according to this ing a range from 18.5 to 21.5°C, or 38.5 to 41.5°C, and
testmethod,anoperatorcancalibratekinematicviscometersin
accordance with Specifications D446.
Cannon, M. R., “Viscosity Measurement, Master Viscometers,” Industrial and
5.3 Using viscosity oil standards established in this test
Engineering Chemistry. Analytical Edition, Vol 16, 1944, p. 708.
method, an operator can calibrate kinematic viscometers in 6
Ubbelohde, L., “The Suspended Lever Viscometer,” Journal Institute Petro-
accordance with Specifications D446.
leum Technologists (London), Vol 22, 1936, p. 37.
D2162–99 (2004)
FIG. 2 Ubbelohde Master Viscometer
conforming to the requirements for Thermometers 44C and viscometer or from one viscometer position to another. The
120C, as prescribed in Specification E1, and calibrated to working section of the bath should be shielded from direct
0.005°CbytheNationalInstituteofStandardsandTechnology radiation from heaters and lights. A standard platinum resis-
or other qualified agency. A standard platinum resistance tance thermometer, approximately 450 mm in length, may be
thermometer together with a Mueller resistance bridge having usedtoensurethatthevariationintemperaturedoesnotexceed
equivalent or better accuracy is preferable, where available. 60.01°C. Firm supports should be provided to hold the master
Other Thermometers 46C, 121C, etc. as required for standard- viscometer in a rigid and reproducible position within 0° 15
izing oil viscosities at other temperatures may be used. min of vertical.
6.3 Bath—A thermostated bath containing water or other 6.4 Timer—Either a spring-wound or electric timer capable
transparent liquid deep enough to immerse the master viscom- ofmeasuringtimeintervalsof300to10000swithanaccuracy
eterssothattheupperfiducialmarkisatleast50mmbelowthe of 60.03%.The stop watch, fully but not tightly wound, must
surface.Theefficiencyofstirringandthebalancebetweenheat be used and tested in the same position. For example, if used
loss and input must be such that the temperature of the water at 45° inclination, it should have been tested previously in that
does not vary by more than 60.01°C over the length of the position. Electric timers must be operated on circuits, the
D2162–99 (2004)
frequencies of which are controlled. Commercial power 8.4.1 Connect a rubber tube to large arm J. Invert the
sources, the frequencies of which are intermittently and not viscometer and dip the end of small arm A into the beaker of
continuously controlled, are not satisfactory. Both mechanical water.Apply suction to arm J and draw liquid through bulbs B
and electric timers can be sensitive to abnormally low ambient and D to etched line E. Turn the viscometer back to its normal
temperature and should not be used when cold. vertical position, wipe tube A clean, insert the viscometer into
a holder and place it in the constant temperature bath.
NOTE 1—Time signals as broadcast by the National Institute of Stan-
8.4.2 Support the master viscometer firmly and align it in a
dardsandTechnologyareaconvenientandprimarystandardreferencefor
vertical position with the aid of a plumb bob with a length of
calibrating timing devices. The following can be used:
about560mm.Onecanbemadebyuseofacorktofitthelarge
WWV Fort Collins, CO 2.5, 5, 10, 15, 20 MHz
WWVH Kauai, HI 2.5, 5, 10, 15 MHz
tube J, a piece of thread, and an 18-mm length of 3-mm
CHU Ottawa, Canada 3.33, 7.335, 14.67 MHz
diameter solder lead. Remove the cork (or slot it) during the
Radio broadcast of voice and audio on a telephone line at phone 303-499-7111
test so that no back pressure is developed.
Additional time services are available from the National Institute of Standards
8.5 Charge the Ubbelohde master as follows:
and Technology.
8.5.1 Tilt the instrument about 30° from the vertical with
7. Reagents
bulb A below the capillary and then introduce enough water
7.1 Acetone, reagent grade. (Warning—Extremely flam-
into large arm 1 to bring the level up to the lower filling line.
mable.) The level should not be above the upper filling line when the
7.2 Chromic Acid Cleaning Solution— Carefully pour 1 L
viscometerisreturnedtotheverticalpositionandtheliquidhas
of concentrated sulfuric acid (H SO , relative density 1.84) been drained from tube 1. Charge the viscometer in such a
2 4
into 35 mL of a saturated solution of technical grade sodium
manner that the U-tube at the bottom fills completely without
dichromate (Na Cr O ) in water. Strongly oxidizing acid trapping air.
2 2 7
cleaning solutions containing no chromium may be substi-
8.5.2 Place the viscometer into a holder and place it in the
tuted to avoid disposal problems of chromium-containing
constant temperature bath. Align the large tube 1 in a vertical
solutions. (Warning—Causes severe burns.)
position with a plumb bob as described for the Cannon master.
7.3 Petroleum Spirit, or other solvent completely miscible
8.6 Allow the charged viscometer to stand in the bath long
with petroleum oils. (Warning—Combustible. Vapor harm-
enough for the sample to reach bath temperature. Fifteen
ful.)
minutes are usually sufficient.
7.4 Primary Standard Water, deionized or distilled, then
8.7 Withgentlevacuumorpressure,forcetheliquidabout5
distilled fresh the same day of use. Store in a glass-stoppered
mmabovetheuppertimingmark.Avoidsplashingliquidinthe
chromic acid-cleaned bottle of borosilicate glass. See Specifi-
upper bulb or forming any bubbles in the liquid.When using a
cation D1193.
Ubbelohdeviscometer,holdafingerovertheupperendoftube
7.5 Viscosity Oil Standards—Stable petroleum oils selected
3 during this operation; then remove it and immediately place
to cover the desired kinematic viscosity range.They should be
itovertube2untiltheliquiddropsawayfromthelowerendof
transparentandhavevaporpressuresbelow10mmHgat40°C.
the capillary.
Store away from heat and light in suitable containers, prefer-
8.8 Measure the efflux of water from upper to lower timing
ably glass.
mark (which should be 300 s or more) to the nearest 0.1 s.
Repeat this measurement two additional times and average if
8. Calibration of Master Viscometers with Water at 20°C
the lowest and highest times agree within 0.1%. If the
8.1 Maintain the water bath at 20 6 0.01°C applying the
measurements do not agree within this tolerance, repeat the
necessary thermometer corrections. Two check thermometers
procedure paying particular attention to cleaning the viscom-
are recommended to detect any change in calibration.
eter,filteringthesample,avoidingcontaminationduringfilling
8.2 Clean a master viscometer having a calibration constant
and afterwards, checking the temperature control and the
2 2
of 0.001 to 0.003 mm /s (cSt/s) with chromic acid cleaning
timing device.
solution to remove organic deposits, rinse thoroughly with
8.9 Clean the viscometer and dry with filtered air. Reload
distilledwaterandacetoneanddrywithastreamoffilteredair.
the viscometer and measure the efflux time in triplicate.
8.3 Clean a 50-mL Erlenmeyer flask with cleaning solution
Average if the lowest and highest times agree within 0.1%.
and rinse thoroughly with distilled water.Add freshly distilled
8.10 If the two average times fall within 0.1%, average the
primarystandardwaterandbringtoaboiltoremovedissolved
two to obtain an average of the two fills.
gases. Cover the flask to prevent entrance of dust and allow to
8.11 Calculate the viscometer constant as follows:
cool. If a Cannon master viscometer is being calibrated, cool
the water to 20 6 3°C. c 51.0034/t (1)
8.4 Charge the Cannon master as follows:
where:
c = calibration constant of the viscometer with water at
2 2
20°C, mm /s (cSt/s), and
The sole source of supply of non-chromium containing cleaning solution
known to the committee at this time is Godax Laboratories Inc., 480 Canal Street, t = efflux time, s.
NewYork, NY10013. If you are aware of alternative suppliers, please provide this
8.12 Repeattheoperationsdescribedin8.1through8.8with
information to ASTM International Headquarters. Your comments will receive
a second master viscometer having a constant not greater than
careful consideration at a meeting of the responsible technical committee , which
2 2 2
you may attend. 0.003 mm /s (cSt/s ).
D2162–99 (2004)
NOTE 2—Normally master viscometers are calibrated and used in the
d = density of oil at the test temperature, g/mL.
oT
samelocation.Ifsubsequentlytheviscometerisusedatalaboratoryother
10.1.2 Determine the density of the oil standard at 40°C in
than the calibrating one, the c constant should be corrected for the
accordance with Test Method D1480. Alternatively, deter-
difference in the acceleration of gravity, g at the two locations as follows:
mine the relative density of the oil at some convenient
c 5 ~g / g ! 3 c (2)
2 2 1 1
temperature and obtain the relative density at 40°C in accor-
dance with Guide D1250. Relative density is close enough to
where:
c and g = calibration constant and gravity at the new locations, density for the purposes of this correction.
2 2
and
10.1.3 Calculate the buoyancy correction by the equation
c and g = calibration constant and gravity at the original location.
1 1
given in 10.1.1, inserting the determined oil density at 40°C
Certificatesforviscometersshouldstatethevalueof gatthelocationof
andthedensityofairat40°CfromTable1.Formostpetroleum
the calib
...

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