ASTM D2162-99
(Test Method)Standard Test Method for Basic Calibration of Master Viscometers and Viscosity Oil Standards
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 mm 2/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 precautionary statements see Section 7.
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Designation: D 2162 – 99 An American National Standard
Standard Test Method for
Basic Calibration of Master Viscometers and Viscosity Oil
Standards
This standard is issued under the fixed designation D 2162; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number 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 3. Terminology
1.1 This test method covers the calibration of master vis- 3.1 Definitions of Terms Specific to This Standard:
cometers and viscosity oil standards, both of which may be 3.1.1 basic calibration, n—calibration based on the primary
used to calibrate routine viscometers as described in Test standard, water.
Method D 445 and Specifications D 446 over the temperature 3.1.1.1 Discussion—Pure water has a kinematic viscosity of
range from 15 to 100°C. 1.0034 mm /s (cSt) at 20°C. See ISO 3666.
2 2
1.2 The calibration constants in mm /s are to be regarded 3.1.2 master viscometer, n—glass capillary viscometer with
as the standard. The kinematic viscosities in mm /s are to be a liquid driving head of at least 400 mm.
regarded as the standard. 3.1.2.1 Discussion—It is specially designed to minimize
1.3 This standard does not purport to address all of the errors due to surface tension, kinetic energy, and capillary end
safety concerns, if any, associated with its use. It is the effects.
responsibility of the user of this standard to establish appro- 3.1.3 viscosity oil standard, n—stable Newtonian liquid, the
priate safety and health practices and determine the applica- kinematic viscosity of which has been related to the kinematic
bility of regulatory limitations prior to use. For specific viscosity of water through the step-up procedure described in
precautionary statements see Section 7. this test method.
2. Referenced Documents 4. Summary of Test Method
2.1 ASTM Standards: 4.1 Two or more master viscometers, having calibration
2 2
D 445 Test Method for Kinematic Viscosity of Transparent constants in the 0.001 to 0.003-mm /s (cSt/s) range, are
and Opaque Liquids (and the Calculation of Dynamic calibrated with water at 20°C. The kinematic viscosities of two
Viscosity) or more oil standards are measured at 40°C in these two master
D 446 Specifications and Operating Instructions for Glass viscometers. Corrections are made for buoyancy and, where
Capillary Kinematic Viscometers necessary, for temperature and surface tension.
D 1193 Specification for Reagent Water 4.2 A third master viscometer, with a calibration constant of
2 2
D 1250 Guide for Petroleum Measurement Tables 0.003 to 0.009 mm /s (cSt/s), is then calibrated at 40°C with
D 1480 Test Method for Density and Relative Density the two standard oils and its calibration factor calculated at
(Specific Gravity) of Viscous Materials by Bingham Pyc- standard conditions for water at 20°C. In like manner addi-
nometer tional viscosity oil standards and additional master viscometers
D 1590 Test Methods for Surface Tension of Water and are calibrated at 40°C using the average results from at least
Waste Water two master viscometers or two oil standards. Steps between
E 1 Specification for ASTM Thermometers successive calibration constants or viscosities increase by a
2.2 ISO Standard: factor of three or less until the desired viscosity range is
ISO 3666 Viscosity of Water covered.
4.3 Oils are calibrated at other temperatures using the
average result from at least two master viscometers.
This test method is under the jurisdiction of ASTM Committee D-2 on
5. Significance and Use
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.07 on Flow Properties.
5.1 Because there are surface tension or kinematic viscosity
Current edition approved June 10, 1999. Published August 1999. Originally
differences, or both, between the primary standard (7.4) and
published as D 2162 – 63 T. Last previous edition D 2162 – 93 (1998).
Annual Book of ASTM Standards, Vol 05.01.
kinematic viscosity standards (7.5), special procedures using
Annual Book of ASTM Standards, Vol 11.01.
master viscometers are required to “step-up” from the kine-
Annual Book of ASTM Standards, Vol 14.03.
5 matic viscosity of the primary standard to the kinematic
Available from American National Standards Institute, 11 W. 42nd St., 13th
viscosities of oil standards.
floor, New York, NY 10036.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 2162
5.2 Using master viscometers calibrated according to this masters are required with calibration constants in the 0.001 to
2 2
test method, an operator can calibrate kinematic viscometers in 0.003-mm /s (cSt/s) range. Additional masters have factors
accordance with Specifications D 446.
increasing in three-fold steps.
5.3 Using viscosity oil standards established in this test
6.2 Thermometers—Kinematic viscosity thermometers hav-
method, an operator can calibrate kinematic viscometers in
ing a range from 18.5 to 21.5°C, or 38.5 to 41.5°C, and
accordance with Specifications D 446.
conforming to the requirements for Thermometers 44C and
120C, as prescribed in Specification E 1, and calibrated to
6. Apparatus
0.005°C by the National Institute of Standards and Technology
6 7
6.1 Master Viscometers: Cannon or Ubbelohde Type—
or other qualified agency. A standard platinum resistance
Acceptable viscometers are shown in Fig. 1 and Fig. 2. Two
thermometer together with a Mueller resistance bridge having
equivalent or better accuracy is preferable, where available.
Cannon, M. R., “Viscosity Measurement, Master Viscometers,” Industrial and
Other Thermometers 46C, 121C, etc. as required for standard-
Engineering Chemistry. Analytical Edition, Vol 16, 1944, p. 708.
izing oil viscosities at other temperatures may be used.
Ubbelohde, L., “The Suspended Lever Viscometer,” Journal Institute Petro-
leum Technologists (London), Vol 22, 1936, p. 37.
6.3 Bath—A thermostated bath containing water or other
FIG. 1 Cannon Master Viscometer
D 2162
FIG. 2 Ubbelohde Master Viscometer
transparent liquid deep enough to immerse the master viscom- of 60.03 %. The stop watch, fully but not tightly wound, must
eters so that the upper fiducial mark is at least 50 mm below the be used and tested in the same position. For example, if used
surface. The efficiency of stirring and the balance between heat at 45° inclination, it should have been tested previously in that
loss and input must be such that the temperature of the water position. Electric timers must be operated on circuits, the
does not vary by more than 60.01°C over the length of the frequencies of which are controlled. Commercial power
viscometer or from one viscometer position to another. The sources, the frequencies of which are intermittently and not
working section of the bath should be shielded from direct continuously controlled, are not satisfactory. Both mechanical
radiation from heaters and lights. A standard platinum resis- and electric timers can be sensitive to abnormally low ambient
tance thermometer, approximately 450 mm in length, may be temperature and should not be used when cold.
used to ensure that the variation in temperature does not exceed
NOTE 1—Time signals as broadcast by the National Institute of Stan-
60.01°C. Firm supports should be provided to hold the master
dards and Technology are a convenient and primary standard reference for
viscometer in a rigid and reproducible position within 0° 15
calibrating timing devices. The following can be used:
min of vertical.
WWV Fort Collins, CO 2.5, 5, 10, 15, 20 MHz
6.4 Timer—Either a spring-wound or electric timer capable WWVH Kauai, HI 2.5, 5, 10, 15 MHz
CHU Ottawa, Canada 3.33, 7.335, 14.67 MHz
of measuring time intervals of 300 to 10 000 s with an accuracy
D 2162
Radio broadcast of voice and audio on a telephone line at phone 303-499-7111
diameter solder lead. Remove the cork (or slot it) during the
Additional time services are available from the National Institute of Standards
test so that no back pressure is developed.
and Technology.
8.5 Charge the Ubbelohde master as follows:
7. Reagents 8.5.1 Tilt the instrument about 30° from the vertical with
bulb A below the capillary and then introduce enough water
7.1 Acetone, reagent grade.
into large arm 1 to bring the level up to the lower filling line.
NOTE 2—Warning: Extremely flammable.
The level should not be above the upper filling line when the
7.2 Chromic Acid Cleaning Solution— Carefully pour 1 L viscometer is returned to the vertical position and the liquid has
been drained from tube 1. Charge the viscometer in such a
of concentrated sulfuric acid (H SO , relative density 1.84)
2 4
into 35 mL of a saturated solution of technical grade sodium manner that the U-tube at the bottom fills completely without
trapping air.
dichromate (Na Cr O ) in water. Strongly oxidizing acid
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
constant temperature bath. Align the large tube 1 in a vertical
tuted to avoid disposal problems of chromium-containing
solutions. position with a plumb bob as described for the Cannon master.
8.6 Allow the charged viscometer to stand in the bath long
NOTE 3—Warning: Causes severe burns.
enough for the sample to reach bath temperature. Fifteen
7.3 Petroleum Spirit, or other solvent completely miscible
minutes are usually sufficient.
with petroleum oils.
8.7 With gentle vacuum or pressure, force the liquid about 5
mm above the upper timing mark. Avoid splashing liquid in the
NOTE 4—Warning: Combustible. Vapor harmful.
upper bulb or forming any bubbles in the liquid. When using a
7.4 Primary Standard Water, deionized or distilled, then
Ubbelohde viscometer, hold a finger over the upper end of tube
distilled fresh the same day of use. Store in a glass-stoppered
3 during this operation; then remove it and immediately place
chromic acid-cleaned bottle of borosilicate glass. See Specifi-
it over tube 2 until the liquid drops away from the lower end of
cation D 1193.
the capillary.
7.5 Viscosity Oil Standards—Stable petroleum oils selected
8.8 Measure the efflux of water from upper to lower timing
to cover the desired kinematic viscosity range. They should be
mark (which should be 300 s or more) to the nearest 0.1 s.
transparent and have vapor pressures below 10 mmHg at 40°C.
Repeat this measurement two additional times and average if
Store away from heat and light in suitable containers, prefer-
the lowest and highest times agree within 0.1 %. If the
ably glass.
measurements do not agree within this tolerance, repeat the
procedure paying particular attention to cleaning the viscom-
8. Calibration of Master Viscometers with Water at 20°C
eter, filtering the sample, avoiding contamination during filling
8.1 Maintain the water bath at 20 6 0.01°C applying the
and afterwards, checking the temperature control and the
necessary thermometer corrections. Two check thermometers
timing device.
are recommended to detect any change in calibration.
8.9 Clean the viscometer and dry with filtered air. Reload
8.2 Clean a master viscometer having a calibration constant
the viscometer and measure the efflux time in triplicate.
2 2
of 0.001 to 0.003 mm /s (cSt/s) with chromic acid cleaning
Average if the lowest and highest times agree within 0.1 %.
solution to remove organic deposits, rinse thoroughly with
8.10 If the two average times fall within 0.1 %, average the
distilled water and acetone and dry with a stream of filtered air.
two to obtain an average of the two fills.
8.3 Clean a 50-mL Erlenmeyer flask with cleaning solution
8.11 Calculate the viscometer constant as follows:
and rinse thoroughly with distilled water. Add freshly distilled
c 5 1.0034/t (1)
primary standard water and bring to a boil to remove dissolved
gases. Cover the flask to prevent entrance of dust and allow to
where:
cool. If a Cannon master viscometer is being calibrated, cool
c 5 calibration constant of the viscometer with water at
the water to 20 6 3°C. 2 2
20°C, mm /s (cSt/s), and
8.4 Charge the Cannon master as follows:
t 5 efflux time, s.
8.4.1 Connect a rubber tube to large arm J. Invert the
8.12 Repeat the operations described in 8.1-8.8 with a
viscometer and dip the end of small arm A into the beaker of
second master viscometer having a constant not greater than
water. Apply suction to arm J and draw liquid through bulbs B 2 2 2
0.003 mm /s (cSt/s ).
and D to etched line E. Turn the viscometer back to its normal
NOTE 5—Normally master viscometers are calibrated and used in the
vertical position, wipe tube A clean, insert the viscometer into
same location. If subsequently the viscometer is used at a laboratory other
a holder and place it in the constant temperature bath.
than the calibrating one, the c constant should be corrected for the
8.4.2 Support the master viscometer firmly and align it in a
difference in the acceleration of gravity, g at the two locations as follows:
vertical position with the aid of a plumb bob with a length of
c 5 ~g / g ! 3 c (2)
about 560 mm. One can be made by use of a cork to fit the large 2 2 1 1
tube J, a piece of thread, and an 18-mm length of 3-mm
where:
c and g 5 calibration constant and gravity at the new locations,
2 2
and
8 c and g 5 calibration constant and gravity at the original location.
1 1
A commercial source for a non-chromium containing cleaning solution is
Godax Laboratories Inc., 480 Canal Street, New York, NY 10013. Certificates for viscometers should state the value of g at the location of
D 2162
the calibrating laboratory. Failure to correct a viscometer constant for
dance with Guide D 1250. Relative density is close enough to
change of gravity can result in errors as high as 0.2 %, which is twice the
density for the purposes of this correction.
error permitted between checks in this test method.
10.1.3 Calculate the buoyancy correction by the equation
given in 10.1.1, inserting the determined oil density at 40°C
9. Calibration of Viscosity Oil Standards at 40°C
and the density of air at 40°C from Table 1. For most petroleum
9.1 Choose an oil with a kinematic viscosity of about 3
oils the approximate buoyancy correction is − 0.0002 when
mm /s (cSt/s) at 40°C. Filter a portion into a clean beaker
correcting from water at 20°C to oil at 40°C.
through a 20
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