Astm D445 PDF

Download as pdf or txt
Download as pdf or txt
You are on page 1of 10

An American National Standard

Designation: D 445 – 04e2 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.

e1 NOTE—Repeatability information that was inadvertently duplicated in Section 17 was removed editorially in November
2004.
e2
Note—The footnote regarding viscosity oils was removed editorially in July 2005.

1. Scope* 1.5 This standard does not purport to address all of the
1.1 This test method specifies a procedure for the determi- safety concerns, if any, associated with its use. It is the
nation of the kinematic viscosity, n, of liquid petroleum responsibility of the user of this standard to establish appro-
products, both transparent and opaque, by measuring the time priate safety and health practices and determine the applica-
for a volume of liquid to flow under gravity through a bility of regulatory limitations prior to use.
calibrated glass capillary viscometer. The dynamic viscosity, h, 2. Referenced Documents
can be obtained by multiplying the kinematic viscosity, n, by
the density, r, of the liquid. 2.1 ASTM Standards: 2
D 446 Specifications and Operating Instructions for Glass
NOTE 1—For the measurement of the kinematic viscosity and viscosity Capillary Kinematic Viscometers
of bitumens, see also Test Methods D 2170 and D 2171.
D 1193 Specification for Reagent Water
1.2 The result obtained from this test method is dependent D 1217 Test Method for Density and Relative Density
upon the behavior of the sample and is intended for application (Specific Gravity) of Liquids by Bingham Pycnometer
to liquids for which primarily the shear stress and shear rates D 1480 Test Method for Density and Relative Density
are proportional (Newtonian flow behavior). If, however, the (Specific Gravity) of Viscous Materials by Bingham Pyc-
viscosity varies significantly with the rate of shear, different nometer
results may be obtained from viscometers of different capillary D 1481 Test Method for Density and Relative Density
diameters. The procedure and precision values for residual fuel (Specific Gravity) of Viscous Materials by Lipkin Bicap-
oils, which under some conditions exhibit non-Newtonian illary Pycnometer
behavior, have been included. D 2162 Test Method for Basic Calibration of Master Vis-
1.3 The range of kinematic viscosities covered by this test cometers and Viscosity Oil Standards
method is from 0.2 to 300 000 mm2/s (see Table A1.1) at all D 2170 Test Method for Kinematic Viscosity of Asphalts
temperatures (see 6.3 and 6.4). The precision has only been (Bitumens)
determined for those materials, kinematic viscosity ranges and D 2171 Test Method for Viscosity of Asphalts by Vacuum
temperatures as shown in the footnotes to the precision section. Capillary Viscometer
1.4 The values stated in SI units are to be regarded as the D 6074 Guide for Characterizing Hydrocarbon Lubricant
standard. Base Oils
D 6617 Practice for Laboratory Bias Detection Using
Single Test Result from Standard Material
1
This test method is under the jurisdiction of ASTM Committee D02 on
E 1 Specification for ASTM Liquid-in-Glass Thermometers
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
--```,,,,,,```,,`,,,,,``````,`-`-`,,`,,`,`,,`---

D02.07 on Flow Properties.


2
Current edition approved May 1, 2004. Published June 2004. Originally For referenced ASTM standards, visit the ASTM website, www.astm.org, or
approved in 1937. Last previous edition approved in 2003 as D 445–03. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
In the IP, this test method is under the jurisdiction of the Standardization Standards volume information, refer to the standard’s Document Summary page on
Committee. the ASTM website.

*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.

Copyright ASTM International 1Document provided by IHS Licensee=UTC P&W Canada/9999506005, 09/19/2005
Copyright by ASTM Int'l (all rights reserved);
Reproduced by IHS under license with ASTM 07:45:23 MDT Questions or comments about this message: please call the Document
Policy Group at 303-397-2295.
Reproduction authorized per License Agreement with Kathe Hooper (ASTMIHS Account); Mon Jul 25 12:15:51 EDT 2005
D 445 – 04e2
E 77 Test Method for Inspection and Verification of Ther- 3.1.4.1 Discussion—For gravity flow under a given hydro-
mometers static head, the pressure head of a liquid is proportional to its
2.2 ISO Standards:3 density, r. For any particular viscometer, the time of flow of a
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—
Specification 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
ISO 17025 General Requirements for the Competence of determinations are needed from which to calculate a kinematic
Testing and Calibration Laboratories viscosity result that is the average of two acceptable deter-
2.3 NIST Standards:4 mined values.
NIST Technical Note 1297, Guideline for Evaluating and
Expressing the Uncertainty of NIST Measurement Results 5. Significance and Use
NIST GMP 11
5.1 Many petroleum products, and some non-petroleum
NIST Special Publication 819
materials, are used as lubricants, and the correct operation of
3. Terminology the equipment depends upon the appropriate viscosity of the
3.1 Definitions of Terms Specific to This Standard: liquid being used. In addition, the viscosity of many petroleum
3.1.1 automated viscometer, n—apparatus which, in part or fuels is important for the estimation of optimum storage,
in whole, has mechanized one or more of the procedural steps handling, and operational conditions. Thus, the accurate deter-
indicated in 11 or 12 without changing the principle or mination of viscosity is essential to many product specifica-
technique of the basic manual apparatus. The essential ele- tions.
ments of the apparatus in respect to dimensions, design and
operational characteristics are not changed. The measured 6. Apparatus
result from the apparatus does not require correction to bring it 6.1 Viscometers—Use only calibrated viscometers of the
into correlation with the basic manual apparatus. The precision glass capillary type, capable of being used to determine
of the apparatus shall be of statistical equivalence to, or better kinematic viscosity within the limits of the precision given in
(has less variability) than the manual apparatus. the precision section.
3.1.1.1 Discussion—Automated viscometers have the capa- 6.1.1 Viscometers listed in Table A1.1, whose specifications
bility to mimic some operation of the test method while meet those given in Specifications D 446 and in ISO 3105 meet
reducing or removing the need for manual intervention or these requirements. It is not intended to restrict this test method
interpretation. Apparatus which determine kinematic viscosity to the use of only those viscometers listed in Table A1.1. Annex
by physical techniques that are different than those used in this A1 gives further guidance.
test method are not considered to be Automated Viscometers. 6.1.2 Automated Viscometers—Automated apparatus may
3.1.2 density, n—the mass per unit volume of a substance at be used as long as they mimic the physical conditions,
a given temperature. operations or processes of the manual apparatus they replace.
3.1.3 dynamic viscosity, n—the ratio between the applied Any viscometer, temperature measuring device, temperature
shear stress and rate of shear of a liquid. control, temperature controlled bath or timing device incorpo-
3.1.3.1 Discussion—It is sometimes called the coefficient of rated in the automated apparatus shall conform to the specifi-
dynamic viscosity or, simply, viscosity. Thus dynamic viscos- cation for these components as stated in 6 of this test method.
ity is a measure of the resistance to flow or deformation of a The automated apparatus shall be capable of determining
liquid. kinematic viscosity of a certified viscosity reference standard
3.1.3.2 Discussion—The term dynamic viscosity can also within the limits stated in 9.2.1 and Section 17.
be used in a different context to denote a frequency-dependent 6.2 Viscometer Holders—Use viscometer holders to enable
quantity in which shear stress and shear rate have a sinusodial all viscometers which have the upper meniscus directly above
time dependence. the lower meniscus to be suspended vertically within 1° in all
3.1.4 kinematic viscosity, n—the resistance to flow of a fluid directions. Those viscometers whose upper meniscus is offset
under gravity. from directly above the lower meniscus shall be suspended
vertically within 0.3° in all directions (see Specifications D 446
3
and ISO 3105).
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
6.2.1 Viscometers shall be mounted in the constant tempera-
4th Floor, New York, NY 10036.
4
Available from National Institute of Standards and Technology (NIST), 100 ture bath in the same manner as when calibrated and stated on
Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460. the certificate of calibration. See Specifications D 446, see
--```,,,,,,```,,`,,,,,``````,`-`-`,,`,,`,`,,`---

Copyright ASTM International 2Document provided by IHS Licensee=UTC P&W Canada/9999506005, 09/19/2005
Copyright by ASTM Int'l (all rights reserved);
Reproduced by IHS under license with ASTM 07:45:23 MDT Questions or comments about this message: please call the Document
Policy Group at 303-397-2295.
Reproduction authorized per License Agreement with Kathe Hooper (ASTMIHS Account); Mon Jul 25 12:15:51 EDT 2005
D 445 – 04e2
Operating Instructions in Annexes A1–A3. For those viscom- 7. Reagents and Materials
eters which have Tube L (see Specifications D 446) held 7.1 Chromic Acid Cleaning Solution, or a nonchromium-
vertical, vertical alignment shall be confirmed by using (1) a containing, strongly oxidizing acid cleaning solution.
holder ensured to hold Tube L vertical, or (2) a bubble level (Warning—Chromic acid is a health hazard. It is toxic, a
mounted on a rod designed to fit into Tube L, or (3) a plumb recognized carcinogen, highly corrosive, and potentially haz-
line suspended from the center of Tube L, or (4) other internal ardous in contact with organic materials. If used, wear a full
means of support provided in the constant temperature bath. face-shield and full-length protective clothing including suit-
6.3 Temperature-Controlled Bath—Use a transparent liquid able gloves. Avoid breathing vapor. Dispose of used chromic
bath of sufficient depth such, that at no time during the acid carefully as it remains hazardous. Nonchromium-
measurement of flow time, any portion of the sample in the containing, strongly oxidizing acid cleaning solutions are also
viscometer is less than 20 mm below the surface of the bath highly corrosive and potentially hazardous in contact with
liquid or less than 20 mm above the bottom of the bath. organic materials, but do not contain chromium which has
6.3.1 Temperature Control—For each series of flow time special disposal problems.)
measurements, the temperature control of the bath liquid shall 7.2 Sample Solvent, completely miscible with the sample.
be such that within the range from 15 to 100°C, the tempera- Filter before use.
ture of the bath medium does not vary by more than 60.02°C 7.2.1 For most samples a volatile petroleum spirit or naph-
of the selected temperature over the length of the viscometer, tha is suitable. For residual fuels, a prewash with an aromatic
or between the position of each viscometer, or at the location of solvent such as toluene or xylene may be necessary to remove
the thermometer. For temperatures outside this range, the asphaltenic material.
deviation from the desired temperature must not exceed 7.3 Drying Solvent, a volatile solvent miscible with the
60.05°C. sample solvent (see 7.2) and water (see 7.4). Filter before use.

--```,,,,,,```,,`,,,,,``````,`-`-`,,`,,`,`,,`---
6.4 Temperature Measuring Device in the Range from 0 to 7.3.1 Acetone is suitable. (Warning—Extremely flam-
100°C—Use either calibrated liquid-in-glass thermometers mable.)
(Annex A2) of an accuracy after correction of 60.02°C or 7.4 Water, deionized or distilled and conforming to Speci-
better, or any other thermometric device of equal or better fication D 1193 or Grade 3 of ISO 3696. Filter before use.
accuracy.
8. Certified Viscosity Reference Standards
6.4.1 If calibrated liquid-in-glass thermometers are used, the
use of two thermometers is recommended. The two thermom- 8.1 Certified viscosity reference standards shall be certified
eters shall agree within 0.04°C. by a laboratory that has been shown to meet the requirements
of ISO 17025 by independent assessment. Viscosity standards
6.4.2 Outside the range from 0 to 100°C, use either cali-
shall be traceable to master viscometer procedures described in
brated liquid-in-glass thermometers of an accuracy after cor-
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 the minimum and maximum intervals of determine the tolerance band. The tolerance band combines both the
expected flow times. uncertainty of the certified viscosity reference standard as well as the
6.5.1 Electrical timing devices may be used if the current uncertainty of the laboratory using the certified viscosity reference
frequency is controlled to an accuracy of 0.05 % or better. standard.
Alternating currents, as provided by some public power sys- 9.2.1.1 As an alternative to the calculation in Annex A4, the
tems, are intermittently rather than continuously controlled. approximate tolerance bands in Table 1 may be used.
When used to actuate electrical timing devices, such control 9.2.2 The most common sources of error are caused by
can cause large errors in kinematic viscosity flow time mea- particles of dust lodged in the capillary bore and temperature
surements. measurement errors. It must be appreciated that a correct result

Copyright ASTM International 3Document provided by IHS Licensee=UTC P&W Canada/9999506005, 09/19/2005
Copyright by ASTM Int'l (all rights reserved);
Reproduced by IHS under license with ASTM 07:45:23 MDT Questions or comments about this message: please call the Document
Policy Group at 303-397-2295.
Reproduction authorized per License Agreement with Kathe Hooper (ASTMIHS Account); Mon Jul 25 12:15:51 EDT 2005
D 445 – 04e2
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.

10. General Procedure for Kinematic Viscosity 11.1.1 In general, the viscometers used for transparent
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
eliminate parallax errors. 11.1.4 Because this time will vary for different instruments,
10.2 Select a clean, dry, calibrated viscometer having a for different temperatures, and for different kinematic viscosi-
range covering the estimated kinematic viscosity (that is, a ties, establish a safe equilibrium time by trial.
wide capillary for a very viscous liquid and a narrower 11.1.4.1 Thirty minutes should be sufficient except for the
capillary for a more fluid liquid). The flow time shall not be highest kinematic viscosities.
less than 200 s or the longer time noted in Specifications 11.1.5 Where the design of the viscometer requires it, adjust
D 446. the volume of the sample to the mark after the sample has
10.2.1 The specific details of operation vary for the different reached temperature equilibrium.
types of viscometers listed in Table A1.1. The operating 11.2 Use suction (if the sample contains no volatile con-
instructions for the different types of viscometers are given in stituents) or pressure to adjust the head level of the test sample
Specifications D 446. to a position in the capillary arm of the instrument about 7 mm
10.2.2 When the test temperature is below the dew point, fill above the first timing mark, unless any other value is stated in
the viscometer in the normal manner as required in 11.1. To the operating instructions for the viscometer. With the sample
ensure that moisture does not condense or freeze on the walls flowing freely, measure, in seconds to within 0.1 s, the time
of the capillary, draw the test portion into the working capillary required for the meniscus to pass from the first to the second
and timing bulb, place rubber stoppers into the tubes to hold timing mark. If this flow time is less than the specified
--```,,,,,,```,,`,,,,,``````,`-`-`,,`,,`,`,,`---

the test portion in place, and insert the viscometer into the bath. minimum (see 10.2), select a viscometer with a capillary of
After insertion, allow the viscometer to reach bath temperature, smaller diameter and repeat the operation.
and the remove the stoppers. When performing manual viscos- 11.2.1 Repeat the procedure described in 11.2 to make a
ity determinations, do not use those viscometers which cannot second measurement of flow time. Record both measurements.
be removed from the constant temperature bath for charging 11.2.2 From the two measurements of flow time, calculate
the sample portion. two determined values of kinematic viscosity.

Copyright ASTM International 4Document provided by IHS Licensee=UTC P&W Canada/9999506005, 09/19/2005
Copyright by ASTM Int'l (all rights reserved);
Reproduced by IHS under license with ASTM 07:45:23 MDT Questions or comments about this message: please call the Document
Policy Group at 303-397-2295.
Reproduction authorized per License Agreement with Kathe Hooper (ASTMIHS Account); Mon Jul 25 12:15:51 EDT 2005
D 445 – 04e2
11.2.3 If the two determined values of kinematic viscosity charging the sample. This is to ensure that the sample will not
calculated from the flow time measurements agree within the be cooled below test temperature.
stated determinability figure (see 17.1.1) for the product, use 12.3.2 After 10 min, adjust the volume of the sample (where
the average of these determined values to calculate the kine- the design of the viscometer requires) to coincide with the
matic viscosity result to be reported. Record the result. If not, filling marks as in the viscometer specifications (see Specifi-
repeat the measurements of flow times after a thorough cations D 446).
cleaning and drying of the viscometers and filtering (where 12.3.3 Allow the charged viscometers enough time to reach
required, see 11.1) of the sample until the calculated kinematic the test temperature (see 12.3.1). Where one bath is used to
viscosity determinations agree with the stated determinability. accommodate several viscometers, never add or withdraw, or
11.2.4 If the material or temperature, or both, is not listed in clean a viscometer while any other viscometer is in use for
17.1.1, for temperatures between 15 and 100ºC, use as an measuring flow time.
estimate of the determinability 0.20% and 0.35% for tempera- 12.4 With the sample flowing freely, measure in seconds to
tures outside this range. within 0.1 s, the time required for the advancing ring of contact
to pass from the first timing mark to the second. Record the
12. Procedure for Opaque Liquids measurement.
12.1 For steam-refined cylinder oils and black lubricating 12.4.1 In the case of samples requiring heat treatment
oils, proceed to 12.3 ensuring a thoroughly representative described in 12.1 through 12.2.1, complete the measurements
sample is used. The kinematic viscosity of residual fuel oils of flow time within 1 h of completing 12.2.2. Record the
and similar waxy products can be affected by the previous measured flow times.
thermal history and the following procedure described in 12.5 Calculate kinematic viscosity, n, in mm2/s, from each
12.1.1-12.2.2 shall be followed to minimize this. measured flow time. Regard these as two determined values of
12.1.1 In general, the viscometers used for opaque liquids kinematic viscosity.
are of the reverse-flow type listed in Table A1.1, C. 12.5.1 For residual fuel oils, if the two determined values of
kinematic viscosity agree within the stated determinability
12.1.2 Heat in the original container, in an oven, at 60 6
figure (see 17.1.1), use the average of these determined values
2°C for 1 h.
to calculate the kinematic viscosity result to be reported.
12.1.3 Thoroughly stir the sample with a suitable rod of
Record the result. If the calculated kinematic viscosities do not
sufficient length to reach the bottom of the container. Continue
agree, repeat the measurements of flow times after thorough
stirring until there is no sludge or wax adhering to the rod.
cleaning and drying of the viscometers and filtering of the
--```,,,,,,```,,`,,,,,``````,`-`-`,,`,,`,`,,`---

12.1.4 Recap the container tightly and shake vigorously for


sample. If the material or temperature, or both, is not listed in
1 min to complete the mixing.
17.1.1, for temperatures between 15 and 100°C use as an
12.1.4.1 With samples of a very waxy nature or oils of high estimate of the determinability 1.0 %, and 1.5 % for tempera-
kinematic viscosity, it may be necessary to increase the heating tures outside this range; it must be realized that these materials
temperature above 60°C to achieve proper mixing. The sample can be non-Newtonian, and can contain solids which can come
should be sufficiently fluid for ease of stirring and shaking. out of solution as the flow time is being measured.
12.2 Immediately after completing 12.1.4, pour sufficient
sample to fill two viscometers into a 100-mL glass flask and 13. Cleaning of Viscometer
loosely stopper. 13.1 Between successive determinations of kinematic vis-
12.2.1 Immerse the flask in a bath of boiling water for 30 cosity, clean the viscometer thoroughly by several rinsings
min. (Warning—Exercise care as vigorous boil-over can occur with the sample solvent, followed by the drying solvent (see
when opaque liquids which contain high levels of water are 7.3). Dry the tube by passing a slow stream of filtered dry air
heated to high temperatures.) through the viscometer for 2 min or until the last trace of
12.2.2 Remove the flask from the bath, stopper tightly, and solvent is removed.
shake for 60 s. 13.2 Periodically clean the viscometer with the cleaning
12.3 Two determinations of the kinematic viscosity of the solution (Warning—see 7.1), for several hours to remove
test material are required. For those viscometers that require a residual traces of organic deposits, rinse thoroughly with water
complete cleaning after each flow time measurement, two (7.4) and drying solvent (see 7.3), and dry with filtered dry air
viscometers may be used. A single viscometer in which an or a vacuum line. Remove any inorganic deposits by hydro-
immediate, repeat flow time measurement can be made without chloric acid treatment before the use of cleaning acid, particu-
cleaning may also be used for the two measurements of flow larly if the presence of barium salts is suspected. (Warning—It
time and calculation of kinematic viscosity. Charge two vis- is essential that alkaline cleaning solutions are not used as
cometers in the manner dictated by the design of the instru- changes in the viscometer calibration can occur.)
ment. For example, for the cross-arm or the BS U-tube
14. Calculation
viscometers for opaque liquids, filter the sample through a
75-µm filter into two viscometers previously placed in the bath. 14.1 Calculate each of the determined kinematic viscosity
For samples subjected to heat treatment, use a preheated filter values, n1 and n2, from the measured flow times, t1 and t2, and
to prevent the sample coagulating during the filtration. the viscometer constant, C, by means of the following equa-
12.3.1 Viscometers which are charged before being inserted tion:
into the bath may need to be preheated in an oven prior to n1,2 5 C · t1,2 (2)

Copyright ASTM International 5Document provided by IHS Licensee=UTC P&W Canada/9999506005, 09/19/2005
Reproduced by IHS under license with ASTM Copyright by ASTM Int'l (all rights reserved); 07:45:23 MDT Questions or comments about this message: please call the Document
Policy Group at 303-397-2295.
Reproduction authorized per License Agreement with Kathe Hooper (ASTMIHS Account); Mon Jul 25 12:15:51 EDT 2005
D 445 – 04e2

where: Jet fuels at –20°C12 0.0018 y (0.18 %)


n1,2 = determined kinematic viscosity values for n1 and n2, where: y is the average of determined values being com-
respectively, mm2/s, pared.
C = calibration constant of the viscometer, mm2/s2, and 17.2 Comparison of Results:
t1,2 = measured flow times for t1 and t2, respectively, s.
17.2.1 Repeatability (r)—The difference between succes-
Calculate the kinematic viscosity result, n, as an average of n1
sive results obtained by the same operator in the same
and n2 (see 11.2.3 and 12.5.1).
laboratory with the same apparatus under constant operating
14.2 Calculate the dynamic viscosity, h, from the calculated
conditions on identical test material would, in the long run, in
kinematic viscosity, n, and the density, r, by means of the
the normal and correct operation of this test method, exceed the
following equation:
values indicated only in one case in twenty:
h 5 n 3 r 3 1023 (3) Base oils at 40 and 100°C5 0.0011 x (0.11 %)
Formulated oils at 40 and 100°C6 0.0026 x (0.26 %)
where: Formulated oils at 150°C7 0.0056 x (0.56 %)
h = dynamic viscosity, mPa·s, Petroleum wax at 100°C8 0.0141 x1.2
Residual fuel oils at 80 and 100°C9 0.013 (x + 8)
r = density, kg/m3, at the same temperature used for the Residual oils at 50°C9 0.015 x (1.5 %)
determination of the kinematic viscosity, and Additives at 100°C10 0.00192 x1.1
n = kinematic viscosity, mm2/s. Gas oils at 40°C11 0.0043 (x+1)
Jet fuels at –20°C12 0.007 x (0.7 %)
14.2.1 The density of the sample can be determined at the
test temperature of the kinematic viscosity determination by an where: x is the average of results being compared.
appropriate method such as Test Methods D 1217, D 1480, or 17.2.2 Reproducibility (R)—The difference between two
D 1481. single and independent results obtained by different operators
working in different laboratories on nominally identical test
15. Expression of Results material would, in the long run, in the normal and correct
15.1 Report the test results for the kinematic or dynamic
viscosity, or both, to four significant figures, together with the
test temperature. 5
These precision values were obtained by statistical examination of interlabo-
16. Report ratory results from six mineral oils (base oils without additive package) in the range
from 8 to 1005 mm2/s at 40°C and from 2 to 43 mm2/s at 100°C, and were first
16.1 Report the following information: published in 1989. Precision data available from ASTM Headquarters. Request
16.1.1 Type and identification of the product tested, RR:D02-1331 and RR:D02-1132. See Guide D 6074.
6
These precision values were obtained by statistical examination of interlabo-
16.1.2 Reference to this test method or a corresponding ratory results from seven fully formulated engine oils in the range from 36 to 340
international standard, mm2/s at 40°C and from 6 to 25 mm2/s at 100°C, and were first published in 1991.
16.1.3 Result of the test (see Section 15), Precision data available from ASTM Headquarters. Request RR:D02-1332. See
16.1.4 Any deviation, by agreement or otherwise, from the Guide D 6071.
7
These precision values were obtained by statistical examination of interlabo-
procedure specified, ratory results for eight fully formulated engine oils in the range from 7 to 19 mm2/s
16.1.5 Date of the test, and at 150°C, and first published in 1991. Precision data available from ASTM
16.1.6 Name and address of the test laboratory. Headquarters. Request RR:D02-1333. See Guide D 6074.
8
These precision values were obtained by statistical examination of interlabo-
17. Precision 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.
17.1 Comparison of Determined Values: Request RR:D02-1334.
9
17.1.1 Determinability (d)—The difference between succes- These precision values were obtained by statistical examination of interlabo-
ratory results from fourteen residual fuel oils in the range from 30 to 1300 mm2/s
sive determined values obtained by the same operator in the at 50°C and from 5 to 170 mm2/s at 80 and 100°C, and were first published in 1984.
same laboratory using the same apparatus for a series of Precision data available from ASTM Headquarters. Request RR:D02-1198.
operations leading to a single result, would in the long run, in 10
These precision values were obtained by statistical examination of interlabo-
the normal and correct operation of this test method, exceed the ratory results from eight additives in the range from 145 to 1500 mm2/s at 100°C
and were first available in 1997. Precision data available from ASTM Headquarters.
values indicated only in one case in twenty: Request RR:D02-1421.
11
Base oils at 40 and 100°C5 0.0020 y (0.20 %) These precision values were obtained by statistical examination of interlabo-
Formulated oils at 40 and 100°C6 0.0013 y (0.13 %) ratory results from eight gas oils in the range from 1 to 13 mm2/s at 40°C and were
Formulated oils at 150°C7 0.015 y (1.5 %) first available in 1997. Precision data available from ASTM Headquarters. Request
Petroleum wax at 100°C8 0.0080 y (0.80 %) RR:D02-1422.
Residual fuel oils at 80 and 100°C9 0.011 (y + 8) 12
These precision values were obtained by statistical examination of interlabo-
Residual fuel oils at 50°C9 0.017 y (1.7 %) ratory results from nine jet fuels in the range from 4.3 to 5.6 mm2/s at– 20°C and
Additives at 100°C10 0.00106 y1.1 were first available in 1997. Precision data available from ASTM Headquarters.
Gas oils at 40°C11 0.0013 (y+1) Request RR:D02-1420.

--```,,,,,,```,,`,,,,,``````,`-`-`,,`,,`,`,,`---

Copyright ASTM International 6Document provided by IHS Licensee=UTC P&W Canada/9999506005, 09/19/2005
Copyright by ASTM Int'l (all rights reserved);
Reproduced by IHS under license with ASTM 07:45:23 MDT Questions or comments about this message: please call the Document
Policy Group at 303-397-2295.
Reproduction authorized per License Agreement with Kathe Hooper (ASTMIHS Account); Mon Jul 25 12:15:51 EDT 2005
D 445 – 04e2
operation of this test method, exceed the values indicated large data set including both automated and manual viscom-
below only in one case in twenty. eters over the temperature range of 40 to 100°C. The repro-
Base oils at 40 and 100°C5 0.0065 x (0.65 %) ducibility of automated viscometer data is not statistically
Formulated oils at 40 and 100°C6 0.0076 x (0.76 %) significantly different than the reproducibility of manual vis-
Formulated oils at 150°C7 0.018 x (1.8 %)
Petroleum wax at 100°C8 0.0366 x1.2 cometer data. It is also shown that there is no bias of the
Residual fuel oils at 80 and 100°C9 0.04 (x + 8) automated data in comparison to the manual data.13
Residual oils at 50°C9 0.074 x (7.4 %)
Additives at 100°C10 0.00862 x1.1
Gas oils at 40°C11 0.0082 (x+1) 18. Keywords
Jet fuels at –20°C12 0.019 x (1.9 %)
18.1 dynamic viscosity; kinematic viscosity; viscometer;
where: x is the average of results being compared. viscosity
17.3 The precision for used oils has not been determined but
is expected to be poorer than that for formulated oils. Because
of the extreme variability of such used oils, it is not anticipated
that the precision of used oils will be determined.
17.4 The precision for specific automated viscometers has 13
Supporting data have been filed at ASTM International Headquarters and may
not been determined. However, an analysis has been made of a be obtained by requesting Research Report 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 in 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.

Copyright ASTM International 7Document provided by IHS Licensee=UTC P&W Canada/9999506005, 09/19/2005
Copyright by ASTM Int'l (all rights reserved);
Reproduced by IHS under license with ASTM 07:45:23 MDT Questions or comments about this message: please call the Document
Policy Group at 303-397-2295.
Reproduction authorized per License Agreement with Kathe Hooper (ASTMIHS Account); Mon Jul 25 12:15:51 EDT 2005
D 445 – 04e2
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 ... ... ...
S30 000 ... 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 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. A2.2.2.1 The interval for ice-point recalibration shall be no
A2.2.2 The scale correction of liquid-in-glass thermometers longer than six months (see NIST GMP 11). For new thermom-
can change during storage and use, and therefore regular
--```,,,,,,```,,`,,,,,``````,`-`-`,,`,,`,`,,`---

eters, monthly checking for the first six months is recom-


re-calibration is required. This is most conveniently achieved mended. A change of one or more scale divisions in the ice
in a working laboratory by means of a re-calibration of the ice point means that the thermometer may have been overheated or
point, and all of the main scale corrections altered for the damaged, and it may be out of calibration. Such thermometers
change seen in the ice point. shall be removed from service until inspected, or recalibrated,
or both. A complete recalibration of the thermometer, while
TABLE A2.1 General Specification for Thermometers
permitted, is not necessary in order to meet the accuracy
ascribed to this design thermometer (see NIST Special Publi-
NOTE—Table A2.2 gives a range of ASTM, IP, and ASTM/IP thermom- cation 819). Any change in ice-point correction shall be added
eters that comply with the specification in Table A2.1, together with their to the other corrections of the original Report of Calibration.
designated test temperatures. See Specification E 1 and Test Method E 77.
A2.2.2.2 Other thermometric devices, if used, will also
Immersion Total
require periodic recalibration. Keep records of all recalibration.
Scale marks: A2.2.3 Procedure for Ice-point Recalibration of Liquid-in-
Subdivisions °C 0.05
Long lines at each °C 0.1 and 0.5 glass Thermometers.
Numbers at each °C 1 A2.2.3.1 Unless otherwise listed on the certificate of cali-
Maximum line width mm 0.10 bration, the recalibration of calibrated kinematic viscosity
Scale error at test temperature, max °C 0.1
Expansion chamber: thermometers requires that the ice-point reading shall be taken
Permit heating to °C 105 up to 90, 120 between 90 and 95 within 60 min after being at test temperature for not less than
130 between 95 and 105, 170 above 3 min.
105
Total length mm 300 to 310 A2.2.3.2 Select clear pieces of ice, preferably made from
Stem outside diameter mm 6.0 to 8.0 distilled or pure water. Discard any cloudy or unsound por-
Bulb length mm 45 to 55 tions. Rinse the ice with distilled water and shave or crush into
Bulb outside diameter mm no greater than stem
Length of scale range mm 40 to 90 small pieces, avoiding direct contact with the hands or any
chemically unclean objects. Fill the Dewar vessel with the

Copyright ASTM International 8Document provided by IHS Licensee=UTC P&W Canada/9999506005, 09/19/2005
Reproduced by IHS under license with ASTM Copyright by ASTM Int'l (all rights reserved); 07:45:23 MDT Questions or comments about this message: please call the Document
Policy Group at 303-397-2295.
Reproduction authorized per License Agreement with Kathe Hooper (ASTMIHS Account); Mon Jul 25 12:15:51 EDT 2005
D 445 – 04e2

FIG. A2.1 Thermometer Designs

crushed ice and add sufficient water to form a slush, but not (2) View the thermometer with an optical aid that gives a
enough to float the ice. As the ice melts, drain off some of the magnification of approximately five and also eliminates paral-
water and add more crushed ice. Insert the thermometer, and lax.
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
apart shall agree within 0.005°C. immersion condition, it shall be immersed to the top of the
A2.2.3.4 Record the ice-point readings and determine the mercury column with the remainder of the stem and the
thermometer correction at this temperature from the mean expansion volume at the uppermost end exposed to room
reading. If the correction is found to be higher or lower than temperature and pressure. In practice, this means that the top of
that corresponding to a previous calibration, change the cor- the mercury column shall be within a length equivalent to four
rection at all other temperatures by the same value. scale divisions of the surface of the medium whose temperature
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.

--```,,,,,,```,,`,,,,,``````,`-`-`,,`,,`,`,,`---

Copyright ASTM International 9Document provided by IHS Licensee=UTC P&W Canada/9999506005, 09/19/2005
Copyright by ASTM Int'l (all rights reserved);
Reproduced by IHS under license with ASTM 07:45:23 MDT Questions or comments about this message: please call the Document
Policy Group at 303-397-2295.
Reproduction authorized per License Agreement with Kathe Hooper (ASTMIHS Account); Mon Jul 25 12:15:51 EDT 2005
D 445 – 04e2

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 MATERIAL

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

SUMMARY OF CHANGES

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D 445–03) that may impact the use of this standard.

(1) Replaced A2.2.2.1. (3) Added text to 6.5.


(2) Added text to 12.3.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
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.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org).

--```,,,,,,```,,`,,,,,``````,`-`-`,,`,,`,`,,`---

Copyright ASTM International 10Document provided by IHS Licensee=UTC P&W Canada/9999506005, 09/19/2005
Copyright by ASTM Int'l (all rights reserved);
Reproduced by IHS under license with ASTM 07:45:23 MDT Questions or comments about this message: please call the Document
Policy Group at 303-397-2295.
Reproduction authorized per License Agreement with Kathe Hooper (ASTMIHS Account); Mon Jul 25 12:15:51 EDT 2005

You might also like