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Designation: D445 14a

British Standard 2000: Part 71: Section 1: 1996

Designation: 71 Section 1/97

Standard Test Method for

Kinematic Viscosity of Transparent and Opaque Liquids


(and Calculation of Dynamic Viscosity)1
This standard is issued under the fixed designation D445; 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 () indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1.5 WARNINGMercury has been designated by many


regulatory agencies as a hazardous material that can cause
central nervous system, kidney and liver damage. Mercury, or
its vapor, may be hazardous to health and corrosive to
materials. Caution should be taken when handling mercury and
mercury containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPAs
websitehttp://www.epa.gov/mercury/faq.htmfor additional information. Users should be aware that selling mercury
and/or mercury containing products into your state or country
may be prohibited by law.
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

1. Scope*
1.1 This test method specifies a procedure for the determination of the kinematic viscosity, , of liquid petroleum
products, both transparent and opaque, by measuring the time
for a volume of liquid to flow under gravity through a
calibrated glass capillary viscometer. The dynamic viscosity, ,
can be obtained by multiplying the kinematic viscosity, , by
the density, , of the liquid.
NOTE 1For the measurement of the kinematic viscosity and viscosity
of bitumens, see also Test Methods D2170 and D2171.
NOTE 2ISO 3104 corresponds to Test Method D445 03.

1.2 The result obtained from this test method is dependent


upon the behavior of the sample and is intended for application
to liquids for which primarily the shear stress and shear rates
are proportional (Newtonian flow behavior). If, however, the
viscosity varies significantly with the rate of shear, different
results may be obtained from viscometers of different capillary
diameters. The procedure and precision values for residual fuel
oils, which under some conditions exhibit non-Newtonian
behavior, have been included.

2. Referenced Documents
2.1 ASTM Standards:2
D446 Specifications and Operating Instructions for Glass
Capillary Kinematic Viscometers
D1193 Specification for Reagent Water
D1217 Test Method for Density and Relative Density (Specific Gravity) of Liquids by Bingham Pycnometer
D1480 Test Method for Density and Relative Density (Specific Gravity) of Viscous Materials by Bingham Pycnometer
D1481 Test Method for Density and Relative Density (Specific Gravity) of Viscous Materials by Lipkin Bicapillary
Pycnometer
D2162 Practice for Basic Calibration of Master Viscometers
and Viscosity Oil Standards
D2170 Test Method for Kinematic Viscosity of Asphalts
(Bitumens)

1.3 The range of kinematic viscosities covered by this test


method is from 0.2 mm2/s to 300 000 mm2/s (see Table A1.1)
at all temperatures (see 6.3 and 6.4). The precision has only
been determined for those materials, kinematic viscosity
ranges and temperatures as shown in the footnotes to the
precision section.
1.4 The values stated in SI units are to be regarded as
standard. The SI unit used in this test method for kinematic
viscosity is mm2/s, and the SI unit used in this test method for
dynamic viscosity is mPas. For user reference, 1 mm2/s =
10-6 m2/s = 1 cSt and 1 mPas = 1 cP = 0.001 Pas.
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.07 on Flow Properties.
Current edition approved Dec. 15, 2014. Published February 2015. Originally
approved in 1937. Last previous edition approved in 2014 as D445 142. DOI:
10.1520/D0445-14a.
In the IP, this test method is under the jurisdiction of the Standardization
Committee.

2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standards Document Summary page on
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

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D445 14a
D2171 Test Method for Viscosity of Asphalts by Vacuum
Capillary Viscometer
D6071 Test Method for Low Level Sodium in High Purity
Water by Graphite Furnace Atomic Absorption Spectroscopy
D6074 Guide for Characterizing Hydrocarbon Lubricant
Base Oils
D6299 Practice for Applying Statistical Quality Assurance
and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
D6300 Practice for Determination of Precision and Bias
Data for Use in Test Methods for Petroleum Products and
Lubricants
D6617 Practice for Laboratory Bias Detection Using Single
Test Result from Standard Material
E1 Specification for ASTM Liquid-in-Glass Thermometers
E77 Test Method for Inspection and Verification of Thermometers
E563 Practice for Preparation and Use of an Ice-Point Bath
as a Reference Temperature
E644 Test Methods for Testing Industrial Resistance Thermometers
E1137/E1137M Specification for Industrial Platinum Resistance Thermometers
E1750 Guide for Use of Water Triple Point Cells
E2593 Guide for Accuracy Verification of Industrial Platinum Resistance Thermometers
E2877 Guide for Digital Contact Thermometers
2.2 ISO Standards:3
ISO 3104 Petroleum ProductsTransparent and Opaque
LiquidsDetermination of Kinematic Viscosity and Calculation of Dynamic Viscosity
ISO 3105 Glass Capillary Kinematic Viscometers
Specification and Operating Instructions
ISO 3696 Water for Analytical Laboratory Use
Specification and Test Methods
ISO 5725 Accuracy (trueness and precision) of measurement
methods and results.
ISO 9000 Quality Management and Quality Assurance
StandardsGuidelines for Selection and Use
ISO 17025 General Requirements for the Competence of
Testing and Calibration Laboratories
2.3 NIST Standards:4
NIST Technical Note 1297 Guideline for Evaluating and
Expressing the Uncertainty of NIST Measurement Results5
NIST GMP 11 Good Measurement Practice for Assignment
and Adjustment of Calibration Intervals for Laboratory
Standards6
NIST Special Publication 811 Guide for the Use of the
International System of Units (SI) 7

NIST Special Publication 1088 Maintenance and Validation


of Liquid-in-Glass Thermometers8
3. Terminology
3.2 Definitions:
3.2.1 digital contact thermometer (DCT), nan electronic
device consisting of a digital display and associated temperature sensing probe.
3.2.1.1 DiscussionThis device consists of a temperature
sensor connected to a measuring instrument; this instrument
measures the temperature-dependent quantity of the sensor,
computes the temperature from the measured quantity, and
provides a digital output. This digital output goes to a digital
display and/or recording device that may be internal or external
to the device. These devices are sometimes referred to as a
digital thermometer.
3.2.1.2 DiscussionPortable electronic thermometers
(PET) is an acronym sometimes used to refer to a subset of the
devices covered by this definition.
3.3 Definitions of Terms Specific to This Standard:
3.3.1 automated viscometer, napparatus which, in part or
in whole, has mechanized one or more of the procedural steps
indicated in Section 11 or 12 without changing the principle or
technique of the basic manual apparatus. The essential elements of the apparatus in respect to dimensions, design, and
operational characteristics are the same as those of the manual
method.
3.3.1.1 DiscussionAutomated viscometers have the capability to mimic some operation of the test method while
reducing or removing the need for manual intervention or
interpretation. Apparatus which determine kinematic viscosity
by physical techniques that are different than those used in this
test method are not considered to be Automated Viscometers.
3.3.2 density, nthe mass per unit volume of a substance at
a given temperature.
3.3.3 dynamic viscosity, , nthe ratio between the applied
shear stress and rate of shear of a material.
3.3.3.1 DiscussionIt is sometimes called the coefficient of
dynamic viscosity or absolute viscosity. Dynamic viscosity is a
measure of resistance to flow or deformation which constitutes
a materials ability to transfer momentum in response to steady
or time-dependent external shear forces. Dynamic viscosity has
the dimension of mass divided by length and time and its SI
unit is pascal times second (Pas). Among the transport
properties for heat, mass, and momentum transfer, dynamic
viscosity is the momentum conductivity.
3.3.4 kinematic viscosity, , nthe ratio of the dynamic
viscosity () to the density () of a material at the same
temperature and pressure.
3.3.4.1 DiscussionKinematic viscosity is the ratio between momentum transport and momentum storage. Such

3
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org.
4
Available from National Institute of Standards and Technology (NIST), 100
Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460.
5
http://physics.nist.gov/cuu/Uncertainty/bibliography.html
6
http://ts.nist.gov/WeightsAndMeasures/upload/GMP_11_Mar_2003.pdf
7
http://www.nist.gov/pml/pubs/sp811/index.cfm

http://www.nist.gov/pml/pubs/sp1088/index.cfm
International Vocabulary of Metrology Basic and General Concepts and
Associated Terms (VIM), 3rd ed., 2008, http://www.bipm.org/en/publications/
guides/vim.html.
9

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3.1 See also International Vocabulary of Metrology.9

D445 14a
ratios are called diffusivities with dimensions of length squared
divided by time and the SI unit is metre squared divided by
second (m2/s). Among the transport properties for heat, mass,
and momentum transfer, kinematic viscosity is the momentum
diffusivity.
3.3.4.2 DiscussionFormerly, kinematic viscosity was defined specifically for viscometers covered by this test method
as the resistance to flow under gravity. More generally, it is the
ratio between momentum transport and momentum storage.
3.3.4.3 DiscussionFor gravity-driven flow under a given
hydrostatic head, the pressure head of a liquid is proportional
to its density, , if the density of air is negligible compared to
that of the liquid. For any particular viscometer covered by this
test method, the time of flow of a fixed volume of liquid is
directly proportional to its kinematic viscosity, , where
= , and is the dynamic viscosity.

D446. The kinetic energy correction shall not exceed 3.0 % of


the measured viscosity. The automated apparatus shall be
capable of determining kinematic viscosity of a certified
viscosity reference standard within the limits stated in 9.2.1
and Section 17. The precision shall be of statistical equivalence
to, or better (has less variability) than the manual apparatus.
NOTE 3Precision and bias of kinematic viscosity measurements for
flow times of less than 200 s has not been determined. The precision stated
in Section 17 is not know to be valid for kinematic viscosity measurements with flow times less than 200 s.

6.2 Viscometer HoldersUse viscometer holders to enable


all viscometers which have the upper meniscus directly above
the lower meniscus to be suspended vertically within 1 in all
directions. Those viscometers whose upper meniscus is offset
from directly above the lower meniscus shall be suspended
vertically within 0.3 in all directions (see Specifications D446
and ISO 3105).
6.2.1 Viscometers shall be mounted in the constant temperature bath in the same manner as when calibrated and stated on
the certificate of calibration. See Specifications D446, see
Operating Instructions in Annexes A1A3. For those viscometers which have Tube L (see Specifications D446) held
vertical, vertical alignment shall be confirmed by using (1) a
holder ensured to hold Tube L vertical, or (2) a bubble level
mounted on a rod designed to fit into Tube L, or (3) a plumb
line suspended from the center of Tube L, or (4) other internal
means of support provided in the constant temperature bath.

4. Summary of Test Method


4.1 The time is measured for a fixed volume of liquid to
flow under gravity through the capillary of a calibrated
viscometer under a reproducible driving head and at a closely
controlled and known temperature. The kinematic viscosity
(determined value) is the product of the measured flow time
and the calibration constant of the viscometer. Two such
determinations are needed from which to calculate a kinematic
viscosity result that is the average of two acceptable determined values.

6.3 Temperature-Controlled BathUse a transparent liquid


bath of sufficient depth such, that at no time during the
measurement of flow time, any portion of the sample in the
viscometer is less than 20 mm below the surface of the bath
liquid or less than 20 mm above the bottom of the bath.
6.3.1 Temperature ControlFor each series of flow time
measurements, the temperature control of the bath liquid shall
be such that within the range from 15 C to 100 C, the
temperature of the bath medium does not vary by more than
60.02 C of the selected temperature over the length of the
viscometer, or between the position of each viscometer, or at
the location of the thermometer. For temperatures outside this
range, the deviation from the desired temperature must not
exceed 60.05 C.

5. Significance and Use

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5.1 Many petroleum products, and some non-petroleum


materials, are used as lubricants, and the correct operation of
the equipment depends upon the appropriate viscosity of the
liquid being used. In addition, the viscosity of many petroleum
fuels is important for the estimation of optimum storage,
handling, and operational conditions. Thus, the accurate determination of viscosity is essential to many product specifications.
6. Apparatus
6.1 ViscometersUse only calibrated viscometers of the
glass capillary type, capable of being used to determine
kinematic viscosity within the limits of the precision given in
the precision section.
6.1.1 Viscometers listed in Table A1.1, whose specifications
meet those given in Specifications D446 and in ISO 3105 meet
these requirements. It is not intended to restrict this test method
to the use of only those viscometers listed in Table A1.1.
Annex A1 gives further guidance.
6.1.2 Automated ViscometersAutomated apparatus may
be used as long as they mimic the physical conditions,
operations or processes of the manual apparatus. Any
viscometer, temperature measuring device, temperature
control, temperature controlled bath or timing device incorporated in the automated apparatus shall conform to the specification for these components as stated in Section 6 of this test
method. Flow times of less than 200 s are permitted, however,
a kinetic energy correction shall be applied in accordance with
Section 7 on Kinematic Viscosity Calculation of Specifications

6.4 Temperature Measuring Device in the Range from 0 C


to 100 CUse either calibrated liquid-in-glass thermometers
(Annex A2) with an accuracy after correction of 60.02 C or
better, or a digital contact thermometer as described in 6.4.2
with equal or better accuracy.
6.4.1 If calibrated liquid-in-glass thermometers are used, the
use of two thermometers is recommended. The two thermometers shall agree within 0.04 C.

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D445 14a
device of equal or better accuracy. When two temperature
measuring devices are used in the same bath, they shall agree
within 60.1 C.
6.4.4 When using liquid-in-glass thermometers, such as
those in Table A2.1, use a magnifying device to read the
thermometer to the nearest 15 division (for example, 0.01 C or
0.02 F) to ensure that the required test temperature and
temperature control capabilities are met (see 10.1). It is
recommended that thermometer readings (and any corrections
supplied on the certificates of calibrations for the thermometers) be recorded on a periodic basis to demonstrate compliance with the test method requirements. This information can
be quite useful, especially when investigating issues or causes
relating to testing accuracy and precision.

6.4.2 Digital contact thermometer meeting the following


requirements:
Criteria

Minimum Requirements

DCT
Display resolution
Display accuracy

E2877 Class A
0.01 C, recommended 0.001 C
20 mK (0.02 C) for combined probe and sensor
RTD, such as a PRT or thermistor
less than 10 mK (0.01 C) per year
less than or equal to 6 s as defined in Specification E1137/E1137M
10 mK over range of intended use
The DCT shall have a report of temperature calibration traceable to a national calibration or metrology standards body issued by a competent
calibration laboratory with demonstrated competency in temperature calibration. An ISO 17025
accredited laboratory with temperature calibration
in its accreditation scope would meet this requirement.
The calibration report shall include at least 3 calibration temperatures at least 5 C apart which
are appropriate for its intended use.

Sensor type
Drift
Response time
Linearity
Calibration Report

Calibration Data

6.5 Timing DeviceUse any timing device, spring-wound


or digital, that is capable of taking readings with a discrimination of 0.1 s or better and has an accuracy within 60.07 %
(see Annex A3) of the reading when tested over the minimum
and maximum intervals of expected flow times.
6.5.1 Timing devices powered by alternating electric current
may be used if the current frequency is controlled to an
accuracy of 0.05 % or better. Alternating currents, as provided
by some public power systems, are intermittently rather than
continuously controlled. When used to actuate electrical timing
devices, such control can cause large errors in kinematic
viscosity flow time measurements.

6.4.2.1 The DCT probe is to be immersed by more than its


minimum immersion depth in a constant temperature bath so
that the center of the probes sensing region is at the same level
as the lower half of the working capillary provided the probes
minimum immersion depth is met and is no less than indicated
on calibration certificate. See Fig. 1. The end of the probe
sheath shall not extend past the bottom of the viscometer. It is
preferable for the center of the sensing element to be located at
the same level as the lower half of the working capillary as
long as the minimum immersion requirements are met.

6.6 Ultrasonic Bath, Unheated(optional), with an operating frequency between 25 kHz to 60 kHz and a typical power
output of 100 W, of suitable dimensions to hold container(s)
placed inside of bath, for use in effectively dissipating and
removing air or gas bubbles that can be entrained in viscous
sample types prior to analysis. It is permissible to use ultrasonic baths with operating frequencies and power outputs
outside this range, however it is the responsibility of the
laboratory to conduct a data comparison study to confirm that
results determined with and without the use of such ultrasonic
baths does not materially impact results.

NOTE 4With respect to DCT probe immersion depth, a procedure is


available in Test Method E644, Section 7, for determining the minimum
depth. With respect to an ice bath, Test Method E563 provides guidance
on the preparation of an ice bath however variance from the specific steps
is permitted provided preparation is consistent as it is being used to track
change in calibration.

6.4.2.2 Verify the calibration at least annually. The probe


shall be recalibrated, when the check value differs by more
than 0.01 C from the last probe calibration. Verification can be
accomplished with the use of a water triple point cell, an ice
bath or other suitable constant temperature device which has a
known temperature value of suitable precision. See Test
Methods E563, E1750, and E2593 for more information
regarding checking calibrations.
6.4.2.3 In the case of constant temperature baths used in
instruments for automatic viscosity determinations, the user is
to contact the instrument manufacturer for the correct DCT that
has performance equivalence to that described here.
6.4.3 Outside the range from 0 C to 100 C, use either
calibrated liquid-in-glass thermometers of an accuracy after
correction of 60.05 C or better, or any other thermometric

7. Reagents and Materials


7.1 Chromic Acid Cleaning Solution, or a nonchromiumcontaining, strongly oxidizing acid cleaning solution.
(WarningChromic acid is a health hazard. It is toxic, a
recognized carcinogen, highly corrosive, and potentially hazardous in contact with organic materials. If used, wear a full
face-shield and full-length protective clothing including suitable gloves. Avoid breathing vapor. Dispose of used chromic
acid carefully as it remains hazardous. Nonchromiumcontaining, strongly oxidizing acid cleaning solutions are also
highly corrosive and potentially hazardous in contact with

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D445 14a

FIG. 1 Temperature Probe Immersion in Constant Temperature Bath

8. Certified Viscosity Reference Standards

organic materials, but do not contain chromium which has


special disposal problems.)

8.1 Certified viscosity reference standards shall be certified


by a laboratory that has been shown to meet the requirements
of ISO 17025 by independent assessment. Viscosity standards
shall be traceable to master viscometer procedures described in
Test Method D2162.

7.2 Sample Solvent, completely miscible with the sample.


Filter before use.
7.2.1 For most samples a volatile petroleum spirit or naphtha is suitable. For residual fuels, a prewash with an aromatic
solvent such as toluene or xylene may be necessary to remove
asphaltenic material.

8.2 The uncertainty of the certified viscosity reference


standard shall be stated for each certified value (k = 2, 95 %
confidence). See ISO 5725 or NIST 1297.

7.3 Drying Solvent, a volatile solvent miscible with the


sample solvent (see 7.2) and water (see 7.4). Filter before use.
7.3.1 Acetone is suitable. (WarningExtremely flammable.)

9. Calibration and Verification


9.1 ViscometersUse only calibrated viscometers,
thermometers, and timers as described in Section 6.

7.4 Water, deionized or distilled and conforming to Specification D1193 or Grade 3 of ISO 3696. Filter before use.
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D445 14a

10.2 Select a clean, dry, calibrated viscometer having a


range covering the estimated kinematic viscosity (that is, a
wide capillary for a very viscous liquid and a narrower
capillary for a more fluid liquid). The flow time for manual
viscometers shall not be less than 200 s or the longer time
noted in Specifications D446. Flow times of less than 200 s are
permitted for automated viscometers, provided they meet the
requirements of 6.1.2.
10.2.1 The specific details of operation vary for the different
types of viscometers listed in Table A1.1. The operating
instructions for the different types of viscometers are given in
Specifications D446.
10.2.2 When the test temperature is below the dew point, fill
the viscometer in the normal manner as required in 11.1. To
ensure that moisture does not condense or freeze on the walls
of the capillary, draw the test portion into the working capillary
and timing bulb, place rubber stoppers into the tubes to hold
the test portion in place, and insert the viscometer into the bath.
After insertion, allow the viscometer to reach bath temperature,
and the remove the stoppers. When performing manual viscosity determinations, do not use those viscometers which cannot
be removed from the constant temperature bath for charging
the sample portion.
10.2.2.1 The use of loosely packed drying tubes affixed to
the open ends of the viscometer is permitted, but not required.
If used, the drying tubes shall fit the design of the viscometer
and not restrict the flow of the sample by pressures created in
the instrument.
10.2.3 Viscometers used for silicone fluids, fluorocarbons,
and other liquids which are difficult to remove by the use of a
cleaning agent, shall be reserved for the exclusive use of those
fluids except during their calibration. Subject such viscometers
to calibration checks at frequent intervals. The solvent washings from these viscometers shall not be used for the cleaning
of other viscometers.

NOTE 5In previous issues of Test Method D445, limits of 60.35 % of


the certified value have been used. The data to support the limit of
60.35 % cannot be verified. Annex A4 provides instructions on how to
determine the tolerance band. The tolerance band combines both the
uncertainty of the certified viscosity reference standard as well as the
uncertainty of the laboratory using the certified viscosity reference
standard.

9.2.1.1 As an alternative to the calculation in Annex A4, the


approximate tolerance bands in Table 1 may be used.
9.2.2 The most common sources of error are caused by
particles of dust lodged in the capillary bore and temperature
measurement errors. It must be appreciated that a correct result
obtained on a standard oil does not preclude the possibility of
a counterbalancing combination of the possible sources of
error.
9.3 The calibration constant, C, is dependent upon the
gravitational acceleration at the place of calibration and this
must, therefore, be supplied by the standardization laboratory
together with the instrument constant. Where the acceleration
of gravity, g, differs by more that 0.1 %, correct the calibration
constant as follows:
C 2 5 ~ g 2 /g 1 ! 3 C 1

(1)

where the subscripts 1 and 2 indicate, respectively, the


standardization laboratory and the testing laboratory.
10. General Procedure for Kinematic Viscosity
10.1 Adjust and maintain the viscometer bath at the required
test temperature within the limits given in 6.3.1 taking account
of the conditions given in Annex A2 and of the corrections
supplied on the certificates of calibration for the thermometers.
10.1.1 Thermometers shall be held in an upright position
under the same conditions of immersion as when calibrated.
10.1.2 In order to obtain the most reliable temperature
measurement, it is recommended that two thermometers with
valid calibration certificates be used (see 6.4).

11. Procedure for Transparent Liquids


11.1 Although not mandatory, for some transparent liquid
sample types such as viscous oils that are prone to having
entrained air or gas bubbles present in the sample, the use of an
ultrasonic bath (see 6.6) without the heater turned on (if so
equipped) has been found effective in homogenizing and
dissipating bubbles typically within 5 min prior to taking a test
specimen for analysis, with no material impact on results.
Charge the viscometer in the manner dictated by the design of
the instrument, this operation being in conformity with that
employed when the instrument was calibrated. If the sample is
thought or known to contain fibers or solid particles, filter
through a 75 m screen, either prior to or during charging (see
Specifications D446).

TABLE 1 Approximate Tolerance Bands

NOTE 1The tolerance bands were determined using Practice D6617.


The calculation is documented in Research Report RR:D02-1498.A
Viscosity of Reference Material,
mm2/s

Tolerance Band

< 10
10 to 100
100 to 1000
1000 to 10 000
10 000 to 100 000
> 100 000

0.30 %
0.32 %
0.36 %
0.42 %
0.54 %
0.73 %

NOTE 6To minimize the potential of particles passing through the


filter from aggregating, it is recommended that the time lapse between
filtering and charging be kept to a minimum.

A
Supporting data have been filed at ASTM International Headquarters and may be
obtained by requesting Research Report RR:D02-1498.

11.1.1 In general, the viscometers used for transparent


liquids are of the type listed in Table A1.1, A and B.
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10.1.3 They should be viewed with a lens assembly giving


approximately five times magnification and be arranged to
eliminate parallax errors.

9.2 Certified Viscosity Reference Standards (Table A1.2)


These are for use as confirmatory checks on the procedure in
the laboratory.
9.2.1 If the determined kinematic viscosity does not agree
within the acceptable tolerance band, as calculated from Annex
A4, of the certified value, recheck each step in the procedure,
including thermometer and viscometer calibration, to locate the
source of error. Annex A1 gives details of standards available.

D445 14a
12.1.4 Recap the container tightly and shake vigorously for
1 min to complete the mixing.
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
temperature above 60 C to achieve proper mixing. The sample
should be sufficiently fluid for ease of stirring and shaking.

11.1.2 With certain products which exhibit gel-like


behavior, exercise care that flow time measurements are made
at sufficiently high temperatures for such materials to flow
freely, so that similar kinematic viscosity results are obtained
in viscometers of different capillary diameters.
11.1.3 Allow the charged viscometer to remain in the bath
long enough to reach the test temperature. Where one bath is
used to accommodate several viscometers, never add or
withdraw, or clean a viscometer while any other viscometer is
in use for measuring a flow time.
11.1.4 Because this time will vary for different instruments,
for different temperatures, and for different kinematic
viscosities, establish a safe equilibrium time by trial.
11.1.4.1 Thirty minutes should be sufficient except for the
highest kinematic viscosities.
11.1.5 Where the design of the viscometer requires it, adjust
the volume of the sample to the mark after the sample has
reached temperature equilibrium.

12.2 Immediately after completing 12.1.4, pour sufficient


sample to fill two viscometers into a 100 mL glass flask and
loosely stopper.
12.2.1 Immerse the flask in a bath of boiling water for
30 min. (WarningExercise care as vigorous boil-over can
occur when opaque liquids which contain high levels of water
are heated to high temperatures.)
12.2.2 Remove the flask from the bath, stopper tightly, and
shake for 60 s.
12.3 Two determinations of the kinematic viscosity of the
test material are required. For those viscometers that require a
complete cleaning after each flow time measurement, two
viscometers may be used. A single viscometer in which an
immediate, repeat flow time measurement can be made without
cleaning may also be used for the two measurements of flow
time and calculation of kinematic viscosity. Charge two viscometers in the manner dictated by the design of the instrument. For example, for the cross-arm or the BS U-tube
viscometers for opaque liquids, filter the sample through a
75 m filter into two viscometers previously placed in the bath.
For samples subjected to heat treatment, use a preheated filter
to prevent the sample coagulating during the filtration.
12.3.1 Viscometers which are charged before being inserted
into the bath may need to be preheated in an oven prior to
charging the sample. This is to ensure that the sample will not
be cooled below test temperature.
12.3.2 After 10 min, adjust the volume of the sample (where
the design of the viscometer requires) to coincide with the
filling marks as in the viscometer specifications (see Specifications D446).
12.3.3 Allow the charged viscometers enough time to reach
the test temperature (see 12.3.1). Where one bath is used to
accommodate several viscometers, never add or withdraw, or
clean a viscometer while any other viscometer is in use for
measuring flow time.

11.2 Use suction (if the sample contains no volatile constituents) or pressure to adjust the head level of the test sample
to a position in the capillary arm of the instrument about 7 mm
above the first timing mark, unless any other value is stated in
the operating instructions for the viscometer. With the sample
flowing freely, measure, in seconds to within 0.1 s, the time
required for the meniscus to pass from the first to the second
timing mark. If this flow time is less than the specified
minimum (see 10.2), select a viscometer with a capillary of
smaller diameter and repeat the operation.
11.2.1 Repeat the procedure described in 11.2 to make a
second measurement of flow time. Record both measurements.
11.2.2 From the two measurements of flow time, calculate
two determined values of kinematic viscosity.
11.2.3 If the two determined values of kinematic viscosity
calculated from the flow time measurements agree within the
stated determinability figure (see 17.1.1) for the product, use
the average of these determined values to calculate the kinematic viscosity result to be reported. Record the result. If not,
repeat the measurements of flow times after a thorough
cleaning and drying of the viscometers and filtering (where
required, see 11.1) of the sample until the calculated kinematic
viscosity determinations agree with the stated determinability.
11.2.4 If the material or temperature, or both, is not listed in
17.1.1, use 1.5 % as an estimate of the determinability.

12.4 With the sample flowing freely, measure in seconds to


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
measurement.
12.4.1 In the case of samples requiring heat treatment
described in 12.1 through 12.2.1, complete the measurements
of flow time within 1 h of completing 12.2.2. Record the
measured flow times.

12. Procedure for Opaque Liquids


12.1 For steam-refined cylinder oils and black lubricating
oils, proceed to 12.3 ensuring a thoroughly representative
sample is used. The kinematic viscosity of residual fuel oils
and similar waxy products can be affected by the previous
thermal history and the following procedure described in
12.1.1 12.2.2 shall be followed to minimize this.
12.1.1 In general, the viscometers used for opaque liquids
are of the reverse-flow type listed in Table A1.1, C.
12.1.2 Heat in the original container, in an oven, at 60 C 6
2 C for 1 h.
12.1.3 Thoroughly stir the sample with a suitable rod of
sufficient length to reach the bottom of the container. Continue
stirring until there is no sludge or wax adhering to the rod.

12.5 Calculate kinematic viscosity, , in millimetres squared


per second, from each measured flow time. Regard these as two
determined values of kinematic viscosity.
12.5.1 For residual fuel oils, if the two determined values of
kinematic viscosity agree within the stated determinability
figure (see 17.1.1), use the average of these determined values
to calculate the kinematic viscosity result to be reported.
Record the result. If the calculated kinematic viscosities do not

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

7
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D445 14a
15. Expression of Results

agree, repeat the measurements of flow times after thorough


cleaning and drying of the viscometers and filtering of the
sample. If the material or temperature, or both, is not listed in
17.1.1, for temperatures between 15 C and 100 C use as an
estimate of the determinability 1.0 %, and 1.5 % for temperatures outside this range; it must be realized that these materials
can be non-Newtonian, and can contain solids which can come
out of solution as the flow time is being measured.

15.1 Report the test results for the kinematic or dynamic


viscosity, or both, to four significant figures, together with the
test temperature.
16. Report
16.1 Report the following information:
16.1.1 Type and identification of the product tested,
16.1.2 Reference to this test method or a corresponding
international standard,
16.1.3 Result of the test (see Section 15),
16.1.4 Any deviation, by agreement or otherwise, from the
procedure specified,
16.1.5 Date of the test, and
16.1.6 Name and address of the test laboratory.

13. Cleaning of Viscometer


13.1 Between successive determinations of kinematic
viscosity, clean the viscometer thoroughly by several rinsings
with the sample solvent, followed by the drying solvent (see
7.3). Dry the tube by passing a slow stream of filtered dry air
through the viscometer for 2 min or until the last trace of
solvent is removed.
13.2 Periodically clean the viscometer with the cleaning
solution (Warningsee 7.1), for several hours to remove
residual traces of organic deposits, rinse thoroughly with water
(7.4) and drying solvent (see 7.3), and dry with filtered dry air
or a vacuum line. Remove any inorganic deposits by hydrochloric acid treatment before the use of cleaning acid, particularly if the presence of barium salts is suspected. (WarningIt
is essential that alkaline cleaning solutions are not used as
changes in the viscometer calibration can occur.)

17. Precision and Bias

Base oils at 40 C and 100 C10


Formulated oils at 40 C and
100 C11
Formulated oils at 150 C12
Petroleum wax at 100 C13
Residual fuel oils at 80 C and
100 C14
Residual fuel oils at 50 C14

14. Calculation
14.1 Calculate each of the determined kinematic viscosity
values, 1 and 2, from the measured flow times, t1 and t2, and
the viscometer constant, C, by means of the following equation:
1,2 5 Ct 1,2

0.015 y
0.0080 y
0.011 (y + 8)

(1.5 %)
(0.80 %)

0.017 y

(1.7 %)

23

10
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Reports RR:D02-1331 and RR:D02-1132.
These precision values were obtained by statistical examination of interlaboratory
results from six mineral oils (base oils without additive package) in the range from
8 mm2/s to 1005 mm2/s at 40 C and from 2 mm2/s to 43 mm2/s at 100 C, and were
first published in 1989. See Guide D6074.
11
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1332. These precision values
were obtained by statistical examination of interlaboratory results from seven fully
formulated engine oils in the range from 36 mm2/s to 340 mm2/s at 40 C and from
6 mm2/s to 25 mm2/s at 100 C, and were first published in 1991. See Guide D6071.
12
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1333. These precision values
were obtained by statistical examination of interlaboratory results for eight fully
formulated engine oils in the range from 7 mm2/s to 19 mm2/s at 150 C, and first
published in 1991. See Guide D6074.
13
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1334. These precision values
were obtained by statistical examination of interlaboratory results from five
petroleum waxes in the range from 3 mm2/s to 16 mm2/s at 100 C, and were first
published in 1988.
14
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1198. These precision values
were obtained by statistical examination of interlaboratory results from fourteen
residual fuel oils in the range from 30 mm2/s to 1300 mm2/s at 50 C and from
5 mm2/s to 170 mm2/s at 80 C and 100 C, and were first published in 1984.

(3)

where:

= dynamic viscosity, mPas,

= density, kg/m3, at the same temperature used for the


determination of the kinematic viscosity, and

= kinematic viscosity, mm2/s.


14.2.1 The density of the sample can be determined at the
test temperature of the kinematic viscosity determination by an
appropriate method such as Test Methods D1217, D1480, or
D1481.

8
Copyright ASTM International

(0.20 %)
(0.13 %)

(2)

where:
1,2 = determined kinematic viscosity values for 1 and 2,
respectively, mm2/s,
C
= calibration constant of the viscometer, mm2/s2, and
t1,2 = measured flow times for t1 and t2, respectively, s.
Calculate the kinematic viscosity result, , as an average of
1 and 2 (see 11.2.3 and 12.5.1).
14.2 Calculate the dynamic viscosity, , from the calculated
kinematic viscosity, , and the density, , by means of the
following equation:
5 3 3 10

0.0020 y
0.0013 y

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

17.1 Comparison of Determined Values:


17.1.1 Determinability (d)The difference between successive 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
the normal and correct operation of this test method, exceed the
values indicated only in one case in twenty:

D445 14a
Additives at 100 C15
Gas oils at 40 C16
Jet fuels at 20 C17
Kerosine, diesel fuels, biodiesel
fuels, and biodiesel fuel blends at
40 C18

0.00106 y1.1
0.0013 (y+1)
0.0018 y
0.0037 y

and biodiesel fuel blends at 40 C round robin study are 16.


Since the minimum requirement of 30 (in accordance with
Practice D6300) is not met, users are cautioned that the actual
repeatability may be significantly different than these estimates.
17.2.2 Reproducibility (R)The difference between two
single and independent results obtained by different operators
working in different laboratories on nominally identical test
material would, in the long run, in the normal and correct
operation of this test method, exceed the values indicated
below only in one case in twenty.

(0.18 %)
(0.37 %)

where: y is the average of determined values being compared.


17.2 Comparison of Results:
17.2.1 Repeatability (r)The difference between successive
results obtained by the same operator in the same laboratory
with the same apparatus under constant operating conditions on
identical test material would, in the long run, in the normal and
correct operation of this test method, exceed the values
indicated only in one case in twenty:
Base oils at 40 C and 100 C10
Formulated oils at 40 C and 100 C11
Formulated oils at 150 C12
Petroleum wax at 100 C13
Residual fuel oils at 80 C and 100 C14
Residual oils at 50 C14
Additives at 100 C15
Gas oils at 40 C16
Jet fuels at 20 C17
Kerosine, diesel fuels, biodiesel fuels,
and biodiesel fuel blends at 40 C18

0.0011 x
0.0026 x
0.0056 x
0.0141 x1.2
0.013 (x + 8)
0.015 x
0.00192 x1.1
0.0043 (x+1)
0.007 x
0.0056 x

Base oils at 40 C and 100 C10


Formulated oils at 40 C and 100 C11
Formulated oils at 150 C12
Petroleum wax at 100 C13
Residual fuel oils at 80 C and 100 C14
Residual oils at 50 C14
Additives at 100 C15
Gas oils at 40 C16
Jet fuels at 20 C17
Kerosine, diesel fuels, biodiesel fuels,
and biodiesel fuel blends at 40 C18

(0.11 %)
(0.26 %)
(0.56 %)

(1.5 %)

(0.65 %)
(0.76 %)
(1.8 %)

(7.4 %)

(1.9 %)
(2.24 %)

where: x is the average of results being compared.


17.2.2.1 The degrees of freedom associated with the reproducibility estimate for the kerosine, diesel fuels, biodiesel
fuels, and biodiesel fuel blends at 40 C round robin study are
19. Since the minimum requirement of 30 (in accordance with
Practice D6300) is not met, users are cautioned that the actual
reproducibility may be significantly different than these estimates.

(0.7 %)
(0.56 %)

where: x is the average of results being compared.


17.2.1.1 The degrees of freedom associated with the repeatability estimate for the kerosine, diesel fuels, biodiesel fuels,
15
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1421. These precision values
were obtained by statistical examination of interlaboratory results from eight
additives in the range from 145 mm2/s to 1500 mm2/s at 100 C and were first
available in 1997.
16
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1422. These precision values
were obtained by statistical examination of interlaboratory results from eight gas
oils in the range from 1 mm2/s to 13 mm2/s at 40 C and were first available in 1997.
Kerosine and diesel fuel samples, which can be considered as gas oils, were
included in a dataset to determine the precision for kerosine, diesel fuels, biodiesel
fuels, and biodiesel fuel blends at 40 C (RR:D02-1780). The precision stated in
RR:D02-1780 was developed in a more recent interlaboratory study than the
precision stated in RR RR:D02-1422. Therefore, the gas oil precision statements do
not apply to kerosine and diesel fuels and a user should refer to the precision
statements for kerosine, diesel fuels, biodiesel fuels, and biodiesel fuel blends at
40 C.
17
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1420. These precision values
were obtained by statistical examination of interlaboratory results from nine jet fuels
in the range from 4.3 mm2/s to 5.6 mm2/s at 20 C and were first available in 1997.
18
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1780. These precision values
were obtained by statistical examination of interlaboratory results from seven
samples including kerosine, diesel fuels, biodiesel fuels, and biodiesel fuel blends
(RR:D02-1780) in the range from 2.06 mm2/s to 4.50 mm2/s at 40 C. These
precision statements only refer to measurement of viscosity using manual viscometers.

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
not been determined. However, an analysis has been made of a
large data set including both automated and manual viscometers over the temperature range of 40 C to 100 C. The
reproducibility of automated viscometer data is not statistically
significantly different than the reproducibility of manual viscometer data. It is also shown that there is no bias of the
automated data in comparison to the manual data.19
18. Keywords
18.1 dynamic viscosity; kinematic viscosity; viscometer;
viscosity

19
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1498.

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9
Copyright ASTM International

0.0065 x
0.0076 x
0.018 x
0.0366 x1.2
0.04 (x + 8)
0.074 x
0.00862 x1.1
0.0082 (x+1)
0.019 x
0.0224 x

D445 14a
ANNEXES
(Mandatory Information)
A1. VISCOMETER TYPES AND CERTIFIED VISCOSITY REFERENCE STANDARDS
TABLE A1.1 Viscometer Types

A1.1 Viscometer Types

Kinematic Viscosity Range,A mm2/s

Viscometer Identification

A1.1.1 Table A1.1 lists capillary viscometers commonly in


use for viscosity determinations on petroleum products. For
specifications, operating instructions, and calibration, refer to
specifications in Specifications D446.

A. Ostwald Types for Transparent Liquids


Cannon-Fenske routineB
0.5 to 20 000
Zeitfuchs
0.6 to 3 000
0.9 to 10 000
BS/U-tubeB
BS/U/M miniature
0.2 to
100
SILB
0.6 to 10 000
Cannon-Manning semi-micro
0.4 to 20 000
PinkevitchB
0.6 to 17 000
B. Suspended-level Types for Transparent Liquids
3.5 to 100 000
BS/IP/SLB
BS/IP/SL(S)B
1.05 to 10 000
BS/IP/MSL
0.6 to 3 000
0.3 to 100 000
UbbelohdeB
FitzSimons
0.6 to 1 200
0.75 to 5 000
AtlanticB
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

A1.1.2 Table A1.2 lists certified viscosity reference standards.

TABLE A1.2 Certified Viscosity Reference Standards


Designation
S3
S6
S20
S60
S200
S600
S2000
S8000
S30 000

Approximate Kinematic Viscosity, mm2/s


20 C

25 C

40 C

50 C

80 C

100 C

4.6
11
44
170
640
2400
8700
37 000
...

4.0
8.9
34
120
450
1600
5600
23 000
81 000

2.9
5.7
18
54
180
520
1700
6700
23 000

...
...
...
...
...
280
...
...
11 000

...
...
...
...
...
67
...
...
...

1.2
1.8
3.9
7.2
17
32
75
...
...

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

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 D446.
B
In each of these series, the minimum flow time for the viscometers with lowest
constants exceeds 200 s.

A2. KINEMATIC VISCOSITY TEST THERMOMETERS

A2.1 Short-Range Specialized Liquid-in-Glass Thermometer

A2.1. As an alternative, use a Digital Contact Thermometer


(DCT) as defined in 6.4.2.

A2.1.1 Use a short-range specialized Liquid-in-Glass thermometer conforming to the generic specification given in Table
A2.1 and Table A2.2 and to one of the designs shown in Fig.

A2.1.2 The difference in the designs of the liquid-in-glass


thermometers rests mainly in the position of the ice point scale.
In Design A, the ice point is within the scale range, in Design

10
Copyright ASTM International

D445 14a
TABLE A2.1 General Specification for Thermometers

NOTE 1Table A2.2 gives a range of ASTM, IP, and ASTM/IP


thermometers that comply with the specification in Table A2.1, together
with their designated test temperatures. See Specification E1 and Test
Method E77.
Immersion

Total

Scale marks:
Subdivisions
C
Long lines at each
C
Numbers at each
C
Maximum line width
mm
Scale error at test temperature, max C
Expansion chamber:
Permit heating to
C

Total length
Stem outside diameter
Bulb length
Bulb outside diameter
Length of scale range

0.05
0.1 and 0.5
1
0.10
0.1
105 up to 90, 120 between 90 and 95
130 between 95 and 105, 170 above
105
300 to 310
6.0 to 8.0
45 to 55
no greater than stem
40 to 90

mm
mm
mm
mm
mm

TABLE A2.2 Complying Thermometers


Thermometer No.

Test
Temperature
C

ASTM 132C, IP 102C


ASTM 110C, F/IP 93C
ASTM 121C/IP 32C
ASTM 129C, F/IP 36C
ASTM 48C, F/IP 90C
IP 100C
ASTM 47C, F/IP 35C
ASTM 29C, F/IP 34C
ASTM 46C F/IP 66C
ASTM 120C/IP 92C
ASTM 28C, F/IP 31C
ASTM 118C, F
ASTM 45C, F/IP 30C
ASTM 44C, F/IP 29C

150
135
98.9,
100
93.3
82.2
80
60
54.4
50
40
37.8
30
25
20

Thermometer No.

F
275
210,
212
200
180

C
ASTM
ASTM
ASTM
ASTM
ASTM
ASTM

128C, F/IP 33C


72C, F/IP 67C
127C/IP 99C
126C, F/IP 71C
73C, F/IP 68C
74C, F/IP 69C

0
32
17.8 0
20
4
26.1 20
40 40
53.9 65

140
130
122
100
86
77
68

to continue to meet the expanded measurement uncertainty


requirements of this section. NIST Special Publication 1088,
Section 7.9 on determining uncertainty of correction, may be
helpful to the user in making this decision. If in-house ice point
verification brings the expanded measurement uncertainty out
of the requirements of A2.2.1, complete recalibration at a
laboratory meeting the requirements of A2.2.1 is required.
A2.2.2.1 For liquid-in-glass thermometers, the interval for
ice-point verification shall be no longer than six months (see
NIST GMP 11). For new thermometers, monthly checking for
the first six months is recommended. A change of one or more
scale divisions in the ice point means that the thermometer may
have been overheated or damaged, and it may be out of
calibration. Such thermometers shall be removed from service
until inspected, or recalibrated, or both.
A2.2.2.2 Keep records of all recalibration.

B, the ice point is below the scale range, and in Design C, the
ice point is above the scale range.
A2.2 Calibration
A2.2.1 When using a liquid-in-glass thermometer, it shall
have a report of temperature calibration traceable to a national
calibration or metrology standards body issued by a competent
calibration laboratory with demonstrated competency in temperature calibration. An ISO 17025 accredited laboratory with
temperature calibration in its accreditation scope would meet
this requirement. The calibration report shall include data for a
series of temperatures which are appropriate for its intended
use.
A2.2.2 The scale correction of liquid-in-glass thermometers
can change during storage and use. Therefore, regular in-house
ice point verifications are required, and can be achieved within
the working laboratory, using an ice melting bath. However,
these checks may not be an adequate means of recalibration as
the use of a single-point recalibration at the ice point adds an
additional uncertainty to the updated thermometer calibration
result at every temperature but the ice point. The user must
determine if the thermometer requires complete re-calibration

A2.2.3 Procedure for Ice-point Verification of Liquid-inGlass Thermometers.


A2.2.3.1 Unless otherwise listed on the certificate of
calibration, the recalibration of calibrated kinematic viscosity
thermometers requires that the ice-point reading shall be taken
within 60 min after being at test temperature for not less than
11

Copyright ASTM International

Test
Temperature

D445 14a

FIG. A2.1 Thermometer Designs

A2.2.3.4 Record the ice-point readings and determine the


thermometer correction at this temperature from the mean
reading. If the correction is found to be higher or lower than
that corresponding to a previous calibration, change the correction at all other temperatures by the same value. See A2.2.1
for discussion on expanded measurement uncertainty changes
when changing correction values from ice point verifications.
A2.2.3.5 During the procedure, apply the following conditions:
(1) The thermometer shall be supported vertically.
(2) View the thermometer with an optical aid that gives a
magnification of approximately five and also eliminates parallax.
(3) Express the ice-point reading to the nearest 0.01 C.

3 min. NIST Special Publication 1088 from the NIST website


describes an effective procedure for ice point verification,
including all formulae necessary for calculations of change of
correction and measurement uncertainty. Alternatively use Test
Method E563 or those in A2.2.3.2 through A2.2.3.5.
A2.2.3.2 Select clear pieces of ice, preferably made from
distilled or pure water. Discard any cloudy or unsound portions. Rinse the ice with distilled water and shave or crush into
small pieces, avoiding direct contact with the hands or any
chemically unclean objects. Fill the Dewar vessel with the
crushed ice and add sufficient water to form a slush, but not
enough to float the ice. As the ice melts, drain off some of the
water and add more crushed ice. Insert the thermometer, and
pack the ice gently about the stem, to a depth approximately
one scale division below the 0 C graduation.
A2.2.3.3 After at least 3 min have elapsed, tap the thermometer gently and repeatedly at right angles to its axis while
making observations. Successive readings taken at least 1 min
apart shall agree within 0.005 C.

A2.2.4 When in use, immerse the thermometric device to


the same depth as when it was fully calibrated. For example, if
a liquid-in-glass thermometer was calibrated at the normal total
immersion condition, it shall be immersed to the top of the

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12
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D445 14a
mercury column with the remainder of the stem and the
expansion volume at the uppermost end exposed to room
temperature and pressure. In practice, this means that the top of
the mercury column shall be within a length equivalent to four
scale divisions of the surface of the medium whose temperature
is being measured.

A2.2.4.1 If this condition cannot be met, then an extra


correction may be necessary.

A3. TIMER ACCURACY

A3.1 Regularly check timers for accuracy and maintain


records of such checks.

WWV
WWVH
CHU

A3.1.1 Time signals as broadcast by the National Institute


of Standards and Technology are a convenient and primary
standard reference for calibrating timing devices. The following can be used to an accuracy of 0.1 s:

Fort Collins, CO
Kauai, HI
Ottawa, Canada

(2.5, 5, 10, 15, 20) MHz


(2.5, 5, 10, 15) MHz
(3.33, 7.335, 14.67) MHz

A3.1.2 Radio broadcast of voice and audio on a telephone


line at phone 303-499-7111. Additional time services are
available from the National Institute of Standards and
Technology.

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

A4.4 Construct the acceptable tolerance zone:

NOTE A4.1These calculations are based on Practice D6617.

A4.1 Determine the standard deviation for site uncertainty,


site, from a laboratory quality control program. (See Practice
D6299.)

2
2
TZ 5 61.44 = site
1SEARV

A4.5 Worked out example for kinematic viscosity zone


(band):

A4.1.1 If the standard deviation for site uncertainty, site, is


not known, use the value 0.19 %.

site 5 0.19 % ~ default value from A4.1.1!

A4.2 Determine the combined extended uncertainty (CEU)


of the accepted reference value (ARV) of the certified reference
material (CRM) from the suppliers label or included documentation. In this test method, the CRM is the Certified
Viscosity Reference Standard (CVRS) as defined in 9.2.

(A4.3)

CEUARV 5 0.22 % ~ from the CVRS label or documentation!


k 5 2 ~ from the CVRS label or documentation!
SEARV 5

NOTE A4.2Combined Extended Uncertainty (CEU) is equivalent to


Expanded Uncertainty (U). See NIST Technical Note 1297.

0.22
5 0.11
2

TZ 5 61.44=0.192 10.112 5 61.44=0.036110.0121 5 60.32 %

A4.3 Calculate the standard error of the accepted reference


value (SEARV) by dividing the CEU by the coverage factor, k,
listed on the suppliers label or included documentation.

A4.5.1 In this example, the tolerance zone will be 60.32 %


of the certified viscosity reference standard value on the report
of test or bottle label. If this site uses a CVRS (for example)
with a kinematic viscosity of 33.98 mm2/s, the TZ =
33.87 mm2/s to 34.09 mm2/s, with 95 % certainty. Viscosity
measurements made with this CVRS at that site should fall
within that tolerance zone (band) 19 out of 20 times.

CEUARV
(A4.1)
k
NOTE A4.3Standard Error (SEARV) is equivalent to Combined Standard Uncertainty (UC). See NIST Technical Note 1297.
SEARV 5

A4.3.1 If the coverage factor, k, is not known, use the value


2.

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13
Copyright ASTM International

(A4.2)

D445 14a

SUMMARY OF CHANGES
Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D445 142) that may impact the use of this standard. (Approved Dec. 15, 2014.)
(3) Reformatted and revised DCT requirements in 6.4.
(4) Revised wording in 6.5 regarding timing devices.
(5) Revised A2.2 regarding liquid-in-glass thermometer calibration.

(1) Revised Referenced Documents, adding additional Committee E20 and NIST references.
(2) Revised definition of DCT and renumbered subsequent
notes.

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D445 12) that may impact the use of this standard. (Approved July 1, 2014.)
(3) Updated Section 17.

(1) Added 6.6.


(2) Updated 11.1.

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