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Astm D 445 - 03

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301 views10 pages

Astm D 445 - 03

Uploaded by

Jako Mishy
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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An American National Standard

Designation: D 445 – 03 British Standard 2000: Part 71:1990

Designation: 71/1/97

Standard Test Method for


Kinematic Viscosity of Transparent and Opaque Liquids
(and the Calculation of Dynamic Viscosity)1
This standard is issued under the fixed designation D 445; 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* priate safety and health practices and determine the applica-
1.1 This test method specifies a procedure for the determi- bility of regulatory limitations prior to use.
nation of the kinematic viscosity, n, of liquid petroleum 2. Referenced Documents
products, both transparent and opaque, by measuring the time
for a volume of liquid to flow under gravity through a 2.1 ASTM Standards:
calibrated glass capillary viscometer. The dynamic viscosity, h, D 446 Specifications and Operating Instructions for Glass
can be obtained by multiplying the kinematic viscosity, n, by Capillary Kinematic Viscometers2
the density, r, of the liquid. D 1193 Specification for Reagent Water3
D 1217 Test Method for Density and Relative Density
NOTE 1—For the measurement of the kinematic viscosity and viscosity (Specific Gravity) of Liquids by Bingham Pycnometer2
of bitumens, see also Test Methods D 2170 and D 2171.
D 1480 Test Method for Density and Relative Density
1.2 The result obtained from this test method is dependent (Specific Gravity) of Viscous Materials by Bingham Pyc-
upon the behavior of the sample and is intended for application nometer2
to liquids for which primarily the shear stress and shear rates D 1481 Test Method for Density and Relative Density
are proportional (Newtonian flow behavior). If, however, the (Specific Gravity) of Viscous Materials by Lipkin Bicap-
viscosity varies significantly with the rate of shear, different illary Pycnometer2
results may be obtained from viscometers of different capillary D 2162 Test Method for Basic Calibration of Master Vis-
diameters. The procedure and precision values for residual fuel cometers and Viscosity Oil Standards2
oils, which under some conditions exhibit non-Newtonian D 2170 Test Method for Kinematic Viscosity of Asphalts
behavior, have been included. (Bitumens)4
1.3 The range of kinematic viscosities covered by this test D 2171 Test Method for Viscosity of Asphalts by Vacuum
method is from 0.2 to 300 000 mm2/s (see Table A1.1) at all Capillary Viscometer4
temperatures (see 6.3 and 6.4). The precision has only been D 6074 Guide for Characterizing Hydrocarbon Lubricant
determined for those materials, kinematic viscosity ranges and Base Oils5
temperatures as shown in the footnotes to the precision section. D 6617 Practice for Laboratory Bias Detection Using
1.4 The values stated in SI units are to be regarded as the Single Test Result from Standard Material6
standard. E 1 Specification for ASTM Thermometers7
1.5 This standard does not purport to address all of the E 77 Test Method for the Inspection and Verification of
safety concerns, if any, associated with its use. It is the Thermometers7
responsibility of the user of this standard to establish appro- 2.2 ISO Standards:8

2
Annual Book of ASTM Standards, Vol 05.01.
1 3
This test method is under the jurisdiction of ASTM Committee D02 on Annual Book of ASTM Standards, Vol 11.01.
4
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Annual Book of ASTM Standards, Vol 04.03.
5
D02.07 on Flow Properties. Annual Book of ASTM Standards, Vol 05.03.
6
Current edition approved March 10, 2003. Published April 2003. Originally Annual Book of ASTM Standards, Vol 05.04.
7
approved in 1937. Last previous edition approved in 2001 as D 445–01. Annual Book of ASTM Standards, Vol 14.03.
8
In the IP, this test method is under the jurisdiction of the Standardization Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
Committee. 4th Floor, New York, NY 10036.

*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.

1
D 445 – 03
ISO 3104 Petroleum Products—Transparent and Opaque fixed volume of fluid is directly proportional to its kinematic
Liquids—Determination of Kinematic Viscosity and Cal- viscosity, n, where n = h/r, and h is the dynamic viscosity
culation of Dynamic Viscosity coefficient.
ISO 3105 Glass Capillary Kinematic Viscometers— Speci-
fication and Operating Instructions 4. Summary of Test Method
ISO 3696 Water for Analytical Laboratory Use— 4.1 The time is measured for a fixed volume of liquid to
Specification and Test Methods flow under gravity through the capillary of a calibrated
ISO 5725 Accuracy (trueness and precision) of measure- viscometer under a reproducible driving head and at a closely
ment methods and results. controlled and known temperature. The kinematic viscosity
ISO 9000 Quality Management and Quality Assurance (determined value) is the product of the measured flow time
Standards—Guidelines for Selection and Use and the calibration constant of the viscometer. Two such
determinations are needed from which to calculate a kinematic
ISO/IEC 17025 General Requirements for the Competence viscosity result that is the average of two acceptable deter-
of Testing and Calibration Laboratories mined values.
2.3 NIST Standard:
NIST Technical Note 1297, Guideline for Evaluating and 5. Significance and Use
Expressing the Uncertainty of NIST Measurement Re-
5.1 Many petroleum products, and some non-petroleum
sults9
materials, are used as lubricants, and the correct operation of
the equipment depends upon the appropriate viscosity of the
3. Terminology
liquid being used. In addition, the viscosity of many petroleum
3.1 Definitions of Terms Specific to This Standard: fuels is important for the estimation of optimum storage,
3.1.1 automated viscometer, n—apparatus which, in part or handling, and operational conditions. Thus, the accurate deter-
in whole, has mechanized one or more of the procedural steps mination of viscosity is essential to many product specifica-
indicated in 11 or 12 without changing the principle or tions.
technique of the basic manual apparatus. The essential ele-
ments of the apparatus in respect to dimensions, design and 6. Apparatus
operational characteristics are not changed. The measured
6.1 Viscometers—Use only calibrated viscometers of the
result from the apparatus does not require correction to bring it
glass capillary type, capable of being used to determine
into correlation with the basic manual apparatus. The precision
kinematic viscosity within the limits of the precision given in
of the apparatus shall be of statistical equivalence to, or better
the precision section.
(has less variability) than the manual apparatus.
6.1.1 Viscometers listed in Table A1.1, whose specifications
3.1.1.1 Discussion—Automated viscometers have the capa-
meet those given in Specifications D 446 and in ISO 3105 meet
bility to mimic some operation of the test method while
these requirements. It is not intended to restrict this test method
reducing or removing the need for manual intervention or
to the use of only those viscometers listed in Table A1.1. Annex
interpretation. Apparatus which determine kinematic viscosity
A1 gives further guidance.
by physical techniques that are different than those used in this
6.1.2 Automated Viscometers—Automated apparatus may
test method are not considered to be Automated Viscometers.
be used as long as they mimic the physical conditions,
3.1.2 density, n—the mass per unit volume of a substance at
operations or processes of the manual apparatus they replace.
a given temperature.
Any viscometer, temperature measuring device, temperature
3.1.3 dynamic viscosity, n—the ratio between the applied
control, temperature controlled bath or timing device incorpo-
shear stress and rate of shear of a liquid.
rated in the automated apparatus shall conform to the specifi-
3.1.3.1 Discussion—It is sometimes called the coefficient of
cation for these components as stated in 6 of this test method.
dynamic viscosity or, simply, viscosity. Thus dynamic viscos-
The automated apparatus shall be capable of determining
ity is a measure of the resistance to flow or deformation of a
kinematic viscosity of a certified viscosity reference standard
liquid.
within the limits stated in 9.2.1 and Section 17.
3.1.3.2 Discussion—The term dynamic viscosity can also
6.2 Viscometer Holders—Use viscometer holders to enable
be used in a different context to denote a frequency-dependent
all viscometers which have the upper meniscus directly above
quantity in which shear stress and shear rate have a sinusodial
the lower meniscus to be suspended vertically within 1° in all
time dependence.
directions. Those viscometers whose upper meniscus is offset
3.1.4 kinematic viscosity, n—the resistance to flow of a fluid
from directly above the lower meniscus shall be suspended
under gravity.
vertically within 0.3° in all directions (see Specifications D 446
3.1.4.1 Discussion—For gravity flow under a given hydro-
and ISO 3105).
static head, the pressure head of a liquid is proportional to its
6.2.1 Viscometers shall be mounted in the constant tempera-
density, r. For any particular viscometer, the time of flow of a
ture bath in the same manner as when calibrated and stated on
the certificate of calibration. See Specifications D 446, see
Operating Instructions in Annexes A1–A3. For those viscom-
9
Available from National Institute of Standards and Technology (NIST), 100 eters which have Tube L (see Specifications D 446) held
Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460. vertical, vertical alignment shall be confirmed by using (1) a

2
D 445 – 03
holder ensured to hold Tube L vertical, or (2) a bubble level recognized carcinogen, highly corrosive, and potentially haz-
mounted on a rod designed to fit into Tube L, or (3) a plumb ardous in contact with organic materials. If used, wear a full
line suspended from the center of Tube L, or (4) other internal face-shield and full-length protective clothing including suit-
means of support provided in the constant temperature bath. able gloves. Avoid breathing vapor. Dispose of used chromic
6.3 Temperature-Controlled Bath—Use a transparent liquid acid carefully as it remains hazardous. Nonchromium-
bath of sufficient depth such, that at no time during the containing, strongly oxidizing acid cleaning solutions are also
measurement of flow time, any portion of the sample in the highly corrosive and potentially hazardous in contact with
viscometer is less than 20 mm below the surface of the bath organic materials, but do not contain chromium which has
liquid or less than 20 mm above the bottom of the bath. special disposal problems.)
6.3.1 Temperature Control—For each series of flow time 7.2 Sample Solvent, completely miscible with the sample.
measurements, the temperature control of the bath liquid shall Filter before use.
be such that within the range from 15 to 100°C, the tempera- 7.2.1 For most samples a volatile petroleum spirit or naph-
ture of the bath medium does not vary by more than 60.02°C tha is suitable. For residual fuels, a prewash with an aromatic
of the selected temperature over the length of the viscometer, solvent such as toluene or xylene may be necessary to remove
or between the position of each viscometer, or at the location of asphaltenic material.
the thermometer. For temperatures outside this range, the 7.3 Drying Solvent, a volatile solvent miscible with the
deviation from the desired temperature must not exceed sample solvent (see 7.2) and water (see 7.4). Filter before use.
60.05°C. 7.3.1 Acetone is suitable. (Warning—Extremely flam-
6.4 Temperature Measuring Device in the Range from 0 to mable.)
100°C—Use either calibrated liquid-in-glass thermometers 7.4 Water, deionized or distilled and conforming to Speci-
(Annex A2) of an accuracy after correction of 60.02°C or fication D 1193 or Grade 3 of ISO 3696. Filter before use.
better, or any other thermometric device of equal or better
accuracy. 8. Certified Viscosity Reference Standards
6.4.1 If calibrated liquid-in-glass thermometers are used, the 8.1 Certified viscosity reference standards shall be certified
use of two thermometers is recommended. The two thermom- by a laboratory that has been shown to meet the requirements
eters shall agree within 0.04°C. of ISO/IEC 17025 by independent assessment. Viscosity stan-
6.4.2 Outside the range from 0 to 100°C, use either cali- dards shall be traceable to master viscometer procedures
brated liquid-in-glass thermometers of an accuracy after cor- described in Test Method D 2162.
rection of 60.05°C or better, or any other thermometric device 8.2 The uncertainty of the certified viscosity reference
of equal or better accuracy. When two temperature measuring standard shall be stated for each certified value (k = 2, 95%
devices are used in the same bath, they shall agree within confidence). See ISO 5725 or NIST 1297.
60.1°C.
6.4.3 When using liquid-in-glass thermometers, such as 9. Calibration and Verification
those in Table A2.1, use a magnifying device to read the 9.1 Viscometers—Use only calibrated viscometers, ther-
thermometer to the nearest 1⁄5 division (for example, 0.01°C or mometers, and timers as described in Section 6.
0.02°F) to ensure that the required test temperature and 9.2 Certified Viscosity Reference Standards (Table A1.2)—
temperature control capabilities are met (see 10.1). It is These are for use as confirmatory checks on the procedure in
recommended that thermometer readings (and any corrections the laboratory.
supplied on the certificates of calibrations for the thermom- 9.2.1 If the determined kinematic viscosity does not agree
eters) be recorded on a periodic basis to demonstrate compli- within the acceptable tolerance band, as calculated from Annex
ance with the test method requirements. This information can A4, of the certified value, recheck each step in the procedure,
be quite useful, especially when investigating issues or causes including thermometer and viscometer calibration, to locate the
relating to testing accuracy and precision. source of error. Annex A1 gives details of standards available.
6.5 Timing Device—Use any timing device that is capable
NOTE 2—In previous issues of Test Method D 445, limits of 60.35% of
of taking readings with a discrimination of 0.1 s or better, and the certified value have been used. The data to support the limit of
has an accuracy within 60.07 % (see Annex A3) of the reading 60.35% cannot be verified. Annex A4 provides instructions on how to
when tested over intervals of $ 200 s. determine the tolerance band. The tolerance band combines both the
6.5.1 Electrical timing devices may be used if the current uncertainty of the certified viscosity reference standard as well as the
frequency is controlled to an accuracy of 0.05 % or better. uncertainty of the laboratory using the certified viscosity reference
Alternating currents, as provided by some public power sys- standard.
tems, are intermittently rather than continuously controlled. 9.2.1.1 As an alternative to the calculation in Annex A4, the
When used to actuate electrical timing devices, such control approximate tolerance bands in Table 1 may be used.10
can cause large errors in kinematic viscosity flow time mea- 9.2.2 The most common sources of error are caused by
surements. particles of dust lodged in the capillary bore and temperature
measurement errors. It must be appreciated that a correct result
7. Reagents and Materials
7.1 Chromic Acid Cleaning Solution, or a nonchromium-
containing, strongly oxidizing acid cleaning solution. 10
Supporting data have been filed at ASTM International Headquarters and may
(Warning—Chromic acid is a health hazard. It is toxic, a be obtained by requesting Research Report RR: D02–1490.

3
D 445 – 03
TABLE 1 Approximate Tolerance Bands 10.2.2.1 The use of loosely packed drying tubes affixed to
NOTE—The tolerance bands were determined using Practice D 6617. the open ends of the viscometer is permitted, but not required.
The calculation is documented in Research Report D02–1490. If used, the drying tubes shall fit the design of the viscometer
Viscosity of Reference Material, mm2/s Tolerance Band and not restrict the flow of the sample by pressures created in
< 10 60.30%
the instrument.
10 to 100 60.32% 10.2.3 Viscometers used for silicone fluids, fluorocarbons,
100 to 1000 60.36% and other liquids which are difficult to remove by the use of a
1000 to 10 000 60.42%
10 000 to 100 000 60.54%
cleaning agent, shall be reserved for the exclusive use of those
> 100 000 60.73% fluids except during their calibration. Subject such viscometers
to calibration checks at frequent intervals. The solvent wash-
ings from these viscometers shall not be used for the cleaning
obtained on a standard oil does not preclude the possibility of of other viscometers.
a counterbalancing combination of the possible sources of
error. 11. Procedure for Transparent Liquids
9.3 The calibration constant, C, is dependent upon the 11.1 Charge the viscometer in the manner dictated by the
gravitational acceleration at the place of calibration and this design of the instrument, this operation being in conformity
must, therefore, be supplied by the standardization laboratory with that employed when the instrument was calibrated. If the
together with the instrument constant. Where the acceleration sample is thought or known to contain fibers or solid particles,
of gravity, g, differs by more that 0.1 %, correct the calibration filter through a 75 µm screen, either prior to or during charging
constant as follows: (see Specifications D 446).
C2 5 ~g2/g1! 3 C1 (1) NOTE 3—To minimize the potential of particles passing through the
where the subscripts 1 and 2 indicate, respectively, the filter from aggregating, it is recommended that the time lapse between
standardization laboratory and the testing laboratory. filtering and charging be kept to a minimum.
11.1.1 In general, the viscometers used for transparent
10. General Procedure for Kinematic Viscosity liquids are of the type listed in Table A1.1, A and B.
10.1 Adjust and maintain the viscometer bath at the required 11.1.2 With certain products which exhibit gel-like behav-
test temperature within the limits given in 6.3.1 taking account ior, exercise care that flow time measurements are made at
of the conditions given in Annex A2 and of the corrections sufficiently high temperatures for such materials to flow freely,
supplied on the certificates of calibration for the thermometers. so that similar kinematic viscosity results are obtained in
10.1.1 Thermometers shall be held in an upright position viscometers of different capillary diameters.
under the same conditions of immersion as when calibrated. 11.1.3 Allow the charged viscometer to remain in the bath
10.1.2 In order to obtain the most reliable temperature long enough to reach the test temperature. Where one bath is
measurement, it is recommended that two thermometers with used to accommodate several viscometers, never add or with-
valid calibration certificates be used (see 6.4). draw, or clean a viscometer while any other viscometer is in
10.1.3 They should be viewed with a lens assembly giving use for measuring a flow time.
approximately five times magnification and be arranged to
NOTE 4—This admonition is to avoid temperature control upsets during
eliminate parallax errors.
the measurement.
10.2 Select a clean, dry, calibrated viscometer having a
range covering the estimated kinematic viscosity (that is, a 11.1.4 Because this time will vary for different instruments,
wide capillary for a very viscous liquid and a narrower for different temperatures, and for different kinematic viscosi-
capillary for a more fluid liquid). The flow time shall not be ties, establish a safe equilibrium time by trial.
less than 200 s or the longer time noted in Specifications 11.1.4.1 Thirty minutes should be sufficient except for the
D 446. highest kinematic viscosities.
10.2.1 The specific details of operation vary for the different 11.1.5 Where the design of the viscometer requires it, adjust
types of viscometers listed in Table A1.1. The operating the volume of the sample to the mark after the sample has
instructions for the different types of viscometers are given in reached temperature equilibrium.
Specifications D 446. 11.2 Use suction (if the sample contains no volatile con-
10.2.2 When the test temperature is below the dew point, fill stituents) or pressure to adjust the head level of the test sample
the viscometer in the normal manner as required in 11.1. To to a position in the capillary arm of the instrument about 7 mm
ensure that moisture does not condense or freeze on the walls above the first timing mark, unless any other value is stated in
of the capillary, draw the test portion into the working capillary the operating instructions for the viscometer. With the sample
and timing bulb, place rubber stoppers into the tubes to hold flowing freely, measure, in seconds to within 0.1 s, the time
the test portion in place, and insert the viscometer into the bath. required for the meniscus to pass from the first to the second
After insertion, allow the viscometer to reach bath temperature, timing mark. If this flow time is less than the specified
and the remove the stoppers. When performing manual viscos- minimum (see 10.2), select a viscometer with a capillary of
ity determinations, do not use those viscometers which cannot smaller diameter and repeat the operation.
be removed from the constant temperature bath for charging 11.2.1 Repeat the procedure described in 11.2 to make a
the sample portion. second measurement of flow time. Record both measurements.

4
D 445 – 03
11.2.2 From the two measurements of flow time, calculate 12.3.2 After 10 min, adjust the volume of the sample (where
two determined values of kinematic viscosity. the design of the viscometer requires) to coincide with the
11.2.3 If the two determined values of kinematic viscosity filling marks as in the viscometer specifications (see Specifi-
calculated from the flow time measurements agree within the cations D 446).
stated determinability figure (see17.1.1) for the product, use 12.3.3 Allow the charged viscometers enough time to reach
the average of these determined values to calculate the kine- the test temperature (see 12.3.1). Where one bath is used to
matic viscosity result to be reported. Record the result. If not, accommodate several viscometers, never add or withdraw, or
repeat the measurements of flow times after a thorough clean a viscometer while any other viscometer is in use for
cleaning and drying of the viscometers and filtering (where measuring flow time.
required, see 11.1) of the sample until the calculated kinematic 12.4 With the sample flowing freely, measure in seconds to
viscosity determinations agree with the stated determinability. within 0.1 s, the time required for the advancing ring of contact
11.2.4 If the material or temperature, or both, is not listed in to pass from the first timing mark to the second. Record the
17.1.1, for temperatures between 15 and 100ºC, use as an measurement.
estimate of the determinability 0.20% and 0.35% for tempera- 12.4.1 In the case of samples requiring heat treatment
tures outside this range. described in 12.1 through 12.2.1, complete the measurements
of flow time within 1 h of completing 12.2.2. Record the
12. Procedure for Opaque Liquids measured flow times.
12.5 Calculate kinematic viscosity, n, in mm 2/s, from each
12.1 For steam-refined cylinder oils and black lubricating
measured flow time. Regard these as two determined values of
oils, proceed to 12.3 ensuring a thoroughly representative
kinematic viscosity.
sample is used. The kinematic viscosity of residual fuel oils
and similar waxy products can be affected by the previous 12.5.1 For residual fuel oils, if the two determined values of
thermal history and the following procedure described in kinematic viscosity agree within the stated determinability
12.1.1-12.2.2 shall be followed to minimize this. figure (see 17.1.1), use the average of these determined values
to calculate the kinematic viscosity result to be reported.
12.1.1 In general, the viscometers used for opaque liquids Record the result. If the calculated kinematic viscosities do not
are of the reverse-flow type listed in Table A1.1, C. agree, repeat the measurements of flow times after thorough
12.1.2 Heat in the original container, in an oven, at 60 6 cleaning and drying of the viscometers and filtering of the
2°C for 1 h. sample. If the material or temperature, or both, is not listed in
12.1.3 Thoroughly stir the sample with a suitable rod of 17.1.1, for temperatures between 15 and 100°C use as an
sufficient length to reach the bottom of the container. Continue estimate of the determinability 1.0 %, and 1.5 % for tempera-
stirring until there is no sludge or wax adhering to the rod. tures outside this range; it must be realized that these materials
12.1.4 Recap the container tightly and shake vigorously for can be non-Newtonian, and can contain solids which can come
1 min to complete the mixing. out of solution as the flow time is being measured.
12.1.4.1 With samples of a very waxy nature or oils of high
kinematic viscosity, it may be necessary to increase the heating 13. Cleaning of Viscometer
temperature above 60°C to achieve proper mixing. The sample 13.1 Between successive determinations of kinematic vis-
should be sufficiently fluid for ease of stirring and shaking. cosity, clean the viscometer thoroughly by several rinsings
12.2 Immediately after completing 12.1.4, pour sufficient with the sample solvent, followed by the drying solvent (see
sample to fill two viscometers into a 100-mL glass flask and 7.3). Dry the tube by passing a slow stream of filtered dry air
loosely stopper. through the viscometer for 2 min or until the last trace of
12.2.1 Immerse the flask in a bath of boiling water for 30 solvent is removed.
min. (Warning—Exercise care as vigorous boil-over can occur 13.2 Periodically clean the viscometer with the cleaning
when opaque liquids which contain high levels of water are solution (Warning—see 7.1), for several hours to remove
heated to high temperatures.) residual traces of organic deposits, rinse thoroughly with water
12.2.2 Remove the flask from the bath, stopper tightly, and (7.4) and drying solvent (see 7.3), and dry with filtered dry air
shake for 60 s. or a vacuum line. Remove any inorganic deposits by hydro-
chloric acid treatment before the use of cleaning acid, particu-
12.3 Charge two viscometers in the manner dictated by the
larly if the presence of barium salts is suspected. (Warning—It
design of the instrument. For example, for the cross-arm or the
is essential that alkaline cleaning solutions are not used as
BS U-tube viscometers for opaque liquids, filter the sample
changes in the viscometer calibration can occur.)
through a 75-µm filter into two viscometers previously placed
in the bath. For samples subjected to heat treatment, use a
14. Calculation
preheated filter to prevent the sample coagulating during the
filtration. 14.1 Calculate each of the determined kinematic viscosity
12.3.1 Viscometers which are charged before being inserted values, n1 and n2, from the measured flow times, t1 and t2, and
into the bath may need to be preheated in an oven prior to the viscometer constant, C, by means of the following equa-
charging the sample. This is to ensure that the sample will not tion:
be cooled below test temperature. n1,2 5 C · t1,2 (2)

5
D 445 – 03

where: Base oils at 40 and 100°C11 0.0020 y (0.20 %)


n1,2 = determined kinematic viscosity values for n1 and n2, Formulated oils at 40 and 100°C12 0.0013 y (0.13 %)
Formulated oils at 150°C13 0.015 y (1.5 %)
respectively, mm2/s, Petroleum wax at 100°C14 0.0080 y (0.80 %)
C = calibration constant of the viscometer, mm2/s2, and Residual fuel oils at 80 and 100°C15 0.011 (y + 8)
t1,2 = measured flow times for t1 and t2, respectively, s. Residual fuel oils at 50°C15 0.017 y (1.7 %)
Additives at 100°C16 0.00106 y1.1
Calculate the kinematic viscosity result, n, as an average of n1 Gas oils at 40°C17 0.0013 (y+1)
and n2 (see 11.2.3 and 12.5.1). Jet fuels at –20°C18 0.0018 y (0.18 %)
14.2 Calculate the dynamic viscosity, h, from the calculated where: y is the average of determined values being com-
kinematic viscosity, n, and the density, r, by means of the pared.
following equation: 17.2 Comparison of Results:
h 5 n 3 r 3 10 23 (3) 17.2.1 Repeatability (r)—The difference between succes-
sive results obtained by the same operator in the same
where: laboratory with the same apparatus under constant operating
h = dynamic viscosity, mPa·s, conditions on identical test material would, in the long run, in
r = density, kg/m3, at the same temperature used for the
the normal and correct operation of this test method, exceed the
determination of the kinematic viscosity, and
values indicated only in one case in twenty:11,12,13,14,15,16,17,18
n = kinematic viscosity, mm2/s.
Base oils at 40 and 100°C11 0.0011 x (0.11 %)
14.2.1 The density of the sample can be determined at the Formulated oils at 40 and 100°C12 0.0026 x (0.26 %)
test temperature of the kinematic viscosity determination by an Formulated oils at 150°C13 0.0056 x (0.56 %)
appropriate method such as Test Methods D 1217, D 1480, or Petroleum wax at 100°C14 0.0141 x1.2
Residual fuel oils at 80 and 100°C15 0.013 (x + 8)
D 1481. Residual oils at 50°C15 0.015 x (1.5 %)
Additives at 100°C16 0.00192 x1.1
15. Expression of Results Gas oils at 40°C17 0.0043 (x+1)
Jet fuels at –20°C18 0.007 x (0.7 %)
15.1 Report the test results for the kinematic or dynamic
viscosity, or both, to four significant figures, together with the where: x is the average of results being compared.
test temperature. 17.2.2 Reproducibility (R)—The difference between two
single and independent results obtained by different operators
16. Report working in different laboratories on nominally identical test
16.1 Report the following information: material would, in the long run, in the normal and correct
16.1.1 Type and identification of the product tested, operation of this test method, exceed the values indicated
16.1.2 Reference to this test method or a corresponding below only in one case in twenty.11,12,13,14,15,16,17,18
international standard, Base oils at 40 and 100°C11 0.0065 x (0.65 %)
16.1.3 Result of the test (see Section 15), Formulated oils at 40 and 100°C12 0.0076 x (0.76 %)
Formulated oils at 150°C13 0.018 x (1.8 %)
16.1.4 Any deviation, by agreement or otherwise, from the Petroleum wax at 100°C14 0.0366 x1.2
procedure specified, Residual fuel oils at 80 and 100°C15 0.04 (x + 8)
16.1.5 Date of the test, and Residual oils at 50°C15 0.074 x (7.4 %)
Additives at 100°C16 0.00862 x1.1
16.1.6 Name and address of the test laboratory. Gas oils at 40°C17 0.0082 (x+1)
Jet fuels at –20°C18 0.019 x (1.9 %)
17. Precision
where: x is the average of results being compared.
17.1 Comparison of Determined Values: 17.3 The precision for used oils has not been determined but
17.1.1 Determinability (d)—The difference between succes- is expected to be poorer than that for formulated oils. Because
sive determined values obtained by the same operator in the
same laboratory using the same apparatus for a series of
operations leading to a single result, would in the long run, in 14
These precision values were obtained by statistical examination of interlabo-
the normal and correct operation of this test method, exceed the ratory results from five petroleum waxes in the range from 3 to 16 mm2/s at 100°C,
and were first published in 1988. Precision data available from ASTM Headquarters.
values indicated only in one case in twenty:11,12,13,14,15,16,17,18
Request RR:D02-1334.
15
These precision values were obtained by statistical examination of interlabo-
ratory results from fourteen residual fuel oils in the range from 30 to 1300 mm 2/s
11
These precision values were obtained by statistical examination of interlabo- at 50°C and from 5 to 170 mm2/s at 80 and 100°C, and were first published in 1984.
ratory results from six mineral oils (base oils without additive package) in the range Precision data available from ASTM Headquarters. Request RR:D02-1198.
16
from 8 to 1005 mm2/s at 40°C and from 2 to 43 mm2/s at 100°C, and were first These precision values were obtained by statistical examination of interlabo-
published in 1989. Precision data available from ASTM Headquarters. Request ratory results from eight additives in the range from 145 to 1500 mm2/s at 100°C
RR:D02-1331 and RR:D02-1132. See Guide D 6074. and were first available in 1997. Precision data available from ASTM Headquarters.
12
These precision values were obtained by statistical examination of interlabo- Request RR:D02-1421.
17
ratory results from seven fully formulated engine oils in the range from 36 to 340 These precision values were obtained by statistical examination of interlabo-
mm /s at 40°C and from 6 to 25 mm 2/s at 100°C, and were first published in 1991.
2
ratory results from eight gas oils in the range from 1 to 13 mm2/s at 40°C and were
Precision data available from ASTM Headquarters. Request RR:D02-1332. See first available in 1997. Precision data available from ASTM Headquarters. Request
Guide D 6074. RR:D02-1422.
13 18
These precision values were obtained by statistical examination of interlabo- These precision values were obtained by statistical examination of interlabo-
ratory results for eight fully formulated engine oils in the range from 7 to 19 mm 2/s ratory results from nine jet fuels in the range from 4.3 to 5.6 mm 2/s at– 20°C and
at 150°C, and first published in 1991. Precision data available from ASTM were first available in 1997. Precision data available from ASTM Headquarters.
Headquarters. Request RR:D02-1333. See Guide D 6074. Request RR:D02-1420.

6
D 445 – 03
of the extreme variability of such used oils, it is not anticipated cometer data. It is also shown that there is no bias of the
that the precision of used oils will be determined. automated data in comparison to the manual data.19
17.4 The precision for specific automated viscometers has 18. Keywords
not been determined. However, an analysis has been made of a
18.1 dynamic viscosity; kinematic viscosity; viscometer;
large data set including both automated and manual viscom-
viscosity
eters over the temperature range of 40 to 100°C. The repro-
ducibility of automated viscometer data is not statistically
significantly different than the reproducibility of manual vis- 19
Precision data available from ASTM Headquarters. Request RR: D02–1498.

ANNEXES

(Mandatory Information)

A1. VISCOMETER TYPES AND CERTIFIED VISCOSITY REFERENCE STANDARDS

A1.1 Viscometer Types TABLE A1.1 Viscometer Types


Viscometer Identification Kinematic Viscosity Range,A mm2/s
A1.1.1 Table A1.1 lists capillary viscometers commonly in
A. Ostwald Types for Transparent Liquids
use for viscosity determinations on petroleum products. For
specifications, operating instructions, and calibration, refer to Cannon-Fenske routineB 0.5 to 20 000
Zeitfuchs 0.6 to 3 000
Specifications D 446. BS/U-tubeB 0.9 to 10 000
BS/U/M miniature 0.2 to 100
A1.1.2 Table A1.2 lists certified viscosity reference stan-
SILB 0.6 to 10 000
dards. Cannon-Manning semi-micro 0.4 to 20 000
PinkevitchB 0.6 to 17 000
B. Suspended-level Types for Transparent Liquids
BS/IP/SLB 3.5 to 100 000
BS/IP/SL(S)B 1.05 to 10 000
BS/IP/MSL 0.6 to 3 000
UbbelohdeB 0.3 to 100 000
FitzSimons 0.6 to 1 200
AtlanticB 0.75 to 5 000
Cannon-Ubbelohde(A), Cannon 0.5 to 100 000
Ubbelohde dilutionB(B)
Cannon-Ubbelohde semi-micro 0.4 to 20 000
C. Reverse-flow Types for Transparent and Opaque Liquids
Cannon-Fenske opaque 0.4 to 20 000
Zeitfuchs cross-arm 0.6 to 100 000
BS/IP/RF U-tube reverse-flow 0.6 to 300 000
Lantz-Zeitfuchs type reverse-flow 60 to 100 000
A
Each range quoted requires a series of viscometers. To avoid the necessity of
making a kinetic energy correction, these viscometers are designed for a flow time
in excess of 200 s except where noted in Specifications D 446.
B
In each of these series, the minimum flow time for the viscometers with lowest
constants exceeds 200 s.

7
D 445 – 03
TABLE A1.2 Certified Viscosity Reference Standards
Approximate Kinematic Viscosity, mm2/s
Designation
20°C 25°C 40°C 50°C 80 °C 100°C
S3 4.6 4.0 2.9 ... ... 1.2
S6 11 8.9 5.7 ... ... 1.8
S20 44 34 18 ... ... 3.9
S60 170 120 54 ... ... 7.2
S200 640 450 180 ... ... 17
S600 2400 1600 520 280 67 32
S2000 8700 5600 1700 ... ... 75
S8000 37 000 23 000 6700 ... ... ...
S30000 ... 81 000 23 000 11 000 ... ...

A2. KINEMATIC VISCOSITY TEST THERMOMETERS

A2.1 Short-Range Specialized Thermometer TABLE A2.2 Complying Thermometers

A2.1.1 Use a short-range specialized thermometer conform- Test Test


Thermometer No. Temperature Thermometer No. Temperature
ing to the generic specification given in Table A2.1 and Table
°C °F °C °F
A2.2 and to one of the designs shown in Fig. A2.1.
A2.1.2 The difference in the designs rests mainly in the ASTM 132C, IP 102C 150 ASTM 128C, F/IP 33C 0 32
ASTM 110C, F/IP 93C 135 275 ASTM 72C, F/IP 67C −17.8 0
position of the ice point scale. In Design A, the ice point is ASTM 121C/IP 32C 98.9, 210, ASTM 127C/IP 99C −20 −4
within the scale range, in Design B, the ice point is below the 100 212 ASTM 126C, F/IP 71C −26.1 −20
scale range, and in Design C, the ice point is above the scale ASTM 129C, F/IP 36C 93.3 200 ASTM 73C, F/IP 68C −40 −40
ASTM 48C, F/IP 90C 82.2 180 ASTM 74C, F/IP 69C −53.9 −65
range. IP 100C 80
ASTM 47C, F/IP 35C 60 140
A2.2 Calibration ASTM 29C, F/IP 34C 54.4 130
ASTM 46C F/IP 66C 50 122
A2.2.1 Use liquid-in-glass thermometers with an accuracy ASTM 120C/IP 92C 40
after correction of 0.02°C or better, calibrated by a laboratory ASTM 28C, F/IP 31C 37.8 100
ASTM 118C, F 30 86
meeting the requirements of ISO 9000 or ISO/IEC 17025, and ASTM 45C, F/IP 30C 25 77
carrying certificates confirming that the calibration is traceable ASTM 44C, F/IP 29C 20 68
to a national standard. As an alternative, use thermometric
devices such as platinum resistance thermometers, of equal or
better accuracy, with the same certification requirements.
A2.2.2 The scale correction of liquid-in-glass thermometers A2.2.2.1 It is recommended that the interval for ice-point
can change during storage and use, and therefore regular checking be not greater than six months, but for new thermom-
re-calibration is required. This is most conveniently achieved eters, monthly checking for the first six months is recom-
in a working laboratory by means of a re-calibration of the ice mended. A complete new re-calibration of the thermometer,
point, and all of the main scale corrections altered for the while permitted, is not necessary in order to meet the accuracy
change seen in the ice point. ascribed to this design thermometer until the ice-point change
from the last full calibration amounts to one scale division, or
more than five years have elapsed since the last full calibration.
TABLE A2.1 General Specification for Thermometers
A2.2.2.2 Other thermometric devices, if used, will also
NOTE—Table A2.2 gives a range of ASTM, IP, and ASTM/IP thermom- require periodic recalibration. Keep records of all recalibration.
eters that comply with the specification in Table A2.1, together with their A2.2.3 Procedure for Ice-point Recalibration of Liquid-in-
designated test temperatures. See Specification E 1 and Test Method E 77.
glass Thermometers.
Immersion Total A2.2.3.1 Unless otherwise listed on the certificate of cali-
Scale marks: bration, the recalibration of calibrated kinematic viscosity
Subdivisions °C 0.05
Long lines at each °C 0.1 and 0.5
thermometers requires that the ice-point reading shall be taken
Numbers at each °C 1 within 60 min after being at test temperature for not less than
Maximum line width mm 0.10 3 min.
Scale error at test temperature, max °C 0.1
Expansion chamber: A2.2.3.2 Select clear pieces of ice, preferably made from
Permit heating to °C 105 up to 90, 120 between 90 and 95 distilled or pure water. Discard any cloudy or unsound por-
130 between 95 and 105, 170 above tions. Rinse the ice with distilled water and shave or crush into
105
Total length mm 300 to 310 small pieces, avoiding direct contact with the hands or any
Stem outside diameter mm 6.0 to 8.0 chemically unclean objects. Fill the Dewar vessel with the
Bulb length mm 45 to 55 crushed ice and add sufficient water to form a slush, but not
Bulb outside diameter mm no greater than stem
Length of scale range mm 40 to 90 enough to float the ice. As the ice melts, drain off some of the
water and add more crushed ice. Insert the thermometer, and

8
D 445 – 03

FIG. A2.1 Thermometer Designs

pack the ice gently about the stem, to a depth approximately (3) Express the ice-point reading to the nearest 0.005°C.
one scale division below the 0°C graduation. A2.2.4 When in use, immerse the thermometric device to
A2.2.3.3 After at least 3 min have elapsed, tap the thermom- the same depth as when it was fully calibrated. For example, if
eter gently and repeatedly at right angles to its axis while a liquid-in-glass thermometer was calibrated at the normal total
making observations. Successive readings taken at least 1 min immersion condition, it shall be immersed to the top of the
apart shall agree within 0.005°C. mercury column with the remainder of the stem and the
A2.2.3.4 Record the ice-point readings and determine the expansion volume at the uppermost end exposed to room
thermometer correction at this temperature from the mean
temperature and pressure. In practice, this means that the top of
reading. If the correction is found to be higher or lower than
the mercury column shall be within a length equivalent to four
that corresponding to a previous calibration, change the cor-
scale divisions of the surface of the medium whose temperature
rection at all other temperatures by the same value.
A2.2.3.5 During the procedure, apply the following condi- is being measured.
tions: A2.2.4.1 If this condition cannot be met, then an extra
(1) The thermometer shall be supported vertically. correction may be necessary.
(2) View the thermometer with an optical aid that gives a
magnification of approximately five and also eliminates paral-
lax.

9
D 445 – 03

A3. TIMER ACCURACY

A3.1 Regularly check timers for accuracy and maintain WWVH Kauai, HI 2.5, 5, 10, 15, MHz
records of such checks. CHU Ottawa, Canada 3.33, 7.335, 14.67 MHz

A3.1.1 Time signals as broadcast by the National Institute A3.1.2 Radio broadcast of voice and audio on a telephone
of Standards and Technology are a convenient and primary line at phone 303-499-7111. Additional time services are
standard reference for calibrating timing devices. The follow- available from the National Institute of Standards and
ing can be used to an accuracy of 0.1 s: Technology.
WWV Fort Collins, CO 2.5, 5, 10, 15, 20 MHz

A4. CALCULATION OF ACCEPTABLE TOLERANCE ZONE (BAND) TO DETERMINE CONFORMANCE WITH A


CERTIFIED REFERENCE MATERIAL10,20

A4.1 Determine the standard deviation for site uncertainty, material (CRM) from the supplier’s label or included docu-
ssite, from a laboratory quality control program. mentation.
A4.1.1 If the standard deviation for site uncertainty, ssite, is A4.3 Calculate the standard error of the accepted reference
not known, use the value 0.19%. value (SEARV) by dividing the CEU by the coverage factor, k,
listed on the supplier’s label or included documentation.
A4.2 Determine the combined extended uncertainty (CEU)
A4.3.1 If the coverage factor, k, is not known, use the value
of the accepted reference value (ARV) of the certified reference
2.
A4.4 Construct the acceptable tolerance zone:
20
These calculations are based on Practice D 6617. TZ 5 61.44 =ssite
2
1 SE2ARV

SUMMARY OF CHANGES

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D 445–01) that may impact the use of this standard.

(1) Added “and” to title. viscosity reference standard throughout.


(2) Included reference to Test Method D 2162 in Referenced (8) Added new Annex A4.
Documents and 8.1. (9) Listed reference to the use and calculation of the tolerance
(3) Deleted ISO 25. Added ISO/IEC 17025 and 5725 to band when using certified viscosity reference standards as
Referenced Documents, 8.1, 8.2, and A2.2. confirmatory checks on the procedure in the laboratory.
(4) Added NIST 1297 to Referenced Documents and 8.2.
(10) Added to 11.1.3 and 12.3.3 that viscometers should not be
(5) Modified throughout to clarify the difference between a
cleaned in the bath while the flow time is being measured with
determination and a result and the use of two determinations to
other viscometers in the bath.
calculate a single result.
(6) Added new Section 8, Certified Viscosity Reference Stan- (11) Deleted A1.2 and A1.3.
dards. (12) Updated Annex A1.1.
(7) Clarified requirements for agreement with a certified (13) Added 80°C data and updated title in Table A1.2.

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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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10

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