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Astm D445-17

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This test method specifies a procedure for determining the kinematic viscosity and dynamic viscosity of liquid petroleum products by measuring the time for a volume of liquid to flow under gravity through a calibrated glass capillary viscometer. The kinematic viscosity can then be used to calculate the dynamic viscosity by multiplying by the density of the liquid.

This test method specifies determining the kinematic viscosity of liquid petroleum products, both transparent and opaque. The result is dependent on Newtonian flow behavior, and is intended for liquids where shear stress and rate are proportional. If viscosity varies significantly with shear rate, different results may be obtained from viscometers of different diameters.

The range of kinematic viscosities covered by this test method is from 0.2 mm2/s to 300 000 mm2/s at all temperatures, as shown in Table A1.1.

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D445 − 17 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. Scope* 1.5 WARNING—Mercury has been designated by many


1.1 This test method specifies a procedure for the determi- regulatory agencies as a hazardous material that can cause
nation of the kinematic viscosity, ν, of liquid petroleum central nervous system, kidney and liver damage. Mercury, or
products, both transparent and opaque, by measuring the time its vapor, may be hazardous to health and corrosive to
for a volume of liquid to flow under gravity through a materials. Caution should be taken when handling mercury and
calibrated glass capillary viscometer. The dynamic viscosity, η, mercury containing products. See the applicable product Ma-
can be obtained by multiplying the kinematic viscosity, ν, by terial Safety Data Sheet (MSDS) for details and EPA’s
the density, ρ, of the liquid. website—http://www.epa.gov/mercury/faq.htm—for addi-
tional information. Users should be aware that selling mercury
NOTE 1—For the measurement of the kinematic viscosity and viscosity and/or mercury containing products into your state or country
of bitumens, see also Test Methods D2170 and D2171.
may be prohibited by law.
NOTE 2—ISO 3104 corresponds to Test Method D445 – 03.
1.6 This standard does not purport to address all of the
1.2 The result obtained from this test method is dependent
safety concerns, if any, associated with its use. It is the
upon the behavior of the sample and is intended for application
responsibility of the user of this standard to establish appro-
to liquids for which primarily the shear stress and shear rates
priate safety and health practices and determine the applica-
are proportional (Newtonian flow behavior). If, however, the
bility of regulatory limitations prior to use.
viscosity varies significantly with the rate of shear, different
results may be obtained from viscometers of different capillary 2. Referenced Documents
diameters. The procedure and precision values for residual fuel
oils, which under some conditions exhibit non-Newtonian 2.1 ASTM Standards:2
behavior, have been included. D396 Specification for Fuel Oils
D446 Specifications and Operating Instructions for Glass
1.3 The range of kinematic viscosities covered by this test Capillary Kinematic Viscometers
method is from 0.2 mm2/s to 300 000 mm2/s (see Table A1.1) D1193 Specification for Reagent Water
at all temperatures (see 6.3 and 6.4). The precision has only D1217 Test Method for Density and Relative Density (Spe-
been determined for those materials, kinematic viscosity cific Gravity) of Liquids by Bingham Pycnometer
ranges and temperatures as shown in the footnotes to the D1480 Test Method for Density and Relative Density (Spe-
precision section. cific Gravity) of Viscous Materials by Bingham Pycnom-
1.4 The values stated in SI units are to be regarded as eter
standard. The SI unit used in this test method for kinematic D1481 Test Method for Density and Relative Density (Spe-
viscosity is mm2/s, and the SI unit used in this test method for cific Gravity) of Viscous Materials by Lipkin Bicapillary
dynamic viscosity is mPa·s. For user reference, 1 mm2/s = Pycnometer
10-6 m2/s = 1 cSt and 1 mPa·s = 1 cP = 0.001 Pa·s. D2162 Practice for Basic Calibration of Master Viscometers
and Viscosity Oil Standards
1
This test method is under the jurisdiction of ASTM Committee D02 on D2170 Test Method for Kinematic Viscosity of Asphalts
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of (Bitumens)
Subcommittee D02.07 on Flow Properties.
Current edition approved Jan. 1, 2017. Published February 2017. Originally
2
approved in 1937. Last previous edition approved in 2016 as D445 – 16. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D0445-17. 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


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D445 − 17
D2171 Test Method for Viscosity of Asphalts by Vacuum NIST Special Publication 811 Guide for the Use of the
Capillary Viscometer International System of Units (SI) 7
D6071 Test Method for Low Level Sodium in High Purity NIST Special Publication 1088 Maintenance and Validation
Water by Graphite Furnace Atomic Absorption Spectros- of Liquid-in-Glass Thermometers8
copy
D6074 Guide for Characterizing Hydrocarbon Lubricant 3. Terminology
Base Oils 3.1 See also International Vocabulary of Metrology.9
D6299 Practice for Applying Statistical Quality Assurance 3.2 Definitions:
and Control Charting Techniques to Evaluate Analytical 3.2.1 digital contact thermometer (DCT), n—an electronic
Measurement System Performance device consisting of a digital display and associated tempera-
D6300 Practice for Determination of Precision and Bias ture sensing probe.
Data for Use in Test Methods for Petroleum Products and 3.2.1.1 Discussion—This device consists of a temperature
Lubricants sensor connected to a measuring instrument; this instrument
D6617 Practice for Laboratory Bias Detection Using Single measures the temperature-dependent quantity of the sensor,
Test Result from Standard Material computes the temperature from the measured quantity, and
D6708 Practice for Statistical Assessment and Improvement provides a digital output. This digital output goes to a digital
of Expected Agreement Between Two Test Methods that display and/or recording device that may be internal or external
Purport to Measure the Same Property of a Material to the device. These devices are sometimes referred to as a
E1 Specification for ASTM Liquid-in-Glass Thermometers “digital thermometer.”
E77 Test Method for Inspection and Verification of Ther- 3.2.1.2 Discussion—Portable electronic thermometers
mometers (PET) is an acronym sometimes used to refer to a subset of the
E563 Practice for Preparation and Use of an Ice-Point Bath devices covered by this definition.
as a Reference Temperature
E644 Test Methods for Testing Industrial Resistance Ther- 3.3 Definitions of Terms Specific to This Standard:
mometers 3.3.1 automated viscometer, n—apparatus which, in part or
E1137/E1137M Specification for Industrial Platinum Resis- in whole, has mechanized one or more of the procedural steps
tance Thermometers indicated in Section 11 or 12 without changing the principle or
E1750 Guide for Use of Water Triple Point Cells technique of the basic manual apparatus. The essential ele-
E2593 Guide for Accuracy Verification of Industrial Plati- ments of the apparatus in respect to dimensions, design, and
num Resistance Thermometers operational characteristics are the same as those of the manual
E2877 Guide for Digital Contact Thermometers method.
2.2 ISO Standards:3 3.3.1.1 Discussion—Automated viscometers have the capa-
ISO 3104 Petroleum Products—Transparent and Opaque bility to mimic some operation of the test method while
Liquids—Determination of Kinematic Viscosity and Cal- reducing or removing the need for manual intervention or
culation of Dynamic Viscosity interpretation. Apparatus which determine kinematic viscosity
ISO 3105 Glass Capillary Kinematic Viscometers— by physical techniques that are different than those used in this
Specification and Operating Instructions test method are not considered to be Automated Viscometers.
ISO 3696 Water for Analytical Laboratory Use— 3.3.2 density, n—the mass per unit volume of a substance at
Specification and Test Methods a given temperature.
ISO 5725 Accuracy (trueness and precision) of measurement 3.3.3 dynamic viscosity, η, n—the ratio between the applied
methods and results. shear stress and rate of shear of a material.
ISO 9000 Quality Management and Quality Assurance 3.3.3.1 Discussion—It is sometimes called the coefficient of
Standards—Guidelines for Selection and Use dynamic viscosity or absolute viscosity. Dynamic viscosity is a
ISO 17025 General Requirements for the Competence of measure of resistance to flow or deformation which constitutes
Testing and Calibration Laboratories a material’s ability to transfer momentum in response to steady
2.3 NIST Standards:4 or time-dependent external shear forces. Dynamic viscosity has
NIST Technical Note 1297 Guideline for Evaluating and the dimension of mass divided by length and time and its SI
Expressing the Uncertainty of NIST Measurement Re- unit is pascal times second (Pa·s). Among the transport
sults5 properties for heat, mass, and momentum transfer, dynamic
NIST GMP 11 Good Measurement Practice for Assignment viscosity is the momentum conductivity.
and Adjustment of Calibration Intervals for Laboratory 3.3.4 kinematic viscosity, ν, n—the ratio of the dynamic
Standards6 viscosity (η) to the density (ρ) of a material at the same
temperature and pressure.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
7
4th Floor, New York, NY 10036, http://www.ansi.org. http://www.nist.gov/pml/pubs/sp811/index.cfm
4 8
Available from National Institute of Standards and Technology (NIST), 100 http://www.nist.gov/pml/pubs/sp1088/index.cfm
9
Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460. International Vocabulary of Metrology — Basic and General Concepts and
5
http://physics.nist.gov/cuu/Uncertainty/bibliography.html Associated Terms (VIM), 3rd ed., 2008, http://www.bipm.org/en/publications/
6
http://ts.nist.gov/WeightsAndMeasures/upload/GMP_11_Mar_2003.pdf guides/vim.html.

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D445 − 17
3.3.4.1 Discussion—Kinematic viscosity is the ratio be- a kinetic energy correction shall be applied in accordance with
tween momentum transport and momentum storage. Such Section 7 on Kinematic Viscosity Calculation of Specifications
ratios are called diffusivities with dimensions of length squared D446. The kinetic energy correction shall not exceed 3.0 % of
divided by time and the SI unit is metre squared divided by the measured viscosity. The automated apparatus shall be
second (m2/s). Among the transport properties for heat, mass, capable of determining kinematic viscosity of a certified
and momentum transfer, kinematic viscosity is the momentum viscosity reference standard within the limits stated in 9.2.1
diffusivity. and Section 17. The precision has been determined for auto-
3.3.4.2 Discussion—Formerly, kinematic viscosity was de- mated viscometers tested on the sample types listed in 17.3.1
fined specifically for viscometers covered by this test method and is no worse than the manual apparatus (that is, exhibits the
as the resistance to flow under gravity. More generally, it is the same or less variability).
ratio between momentum transport and momentum storage. NOTE 3—Precision and bias of kinematic viscosity measurements for
3.3.4.3 Discussion—For gravity-driven flow under a given flow times as low as 10 s has been determined for automated instruments
hydrostatic head, the pressure head of a liquid is proportional tested with the sample types listed in 17.3.1.
to its density, ρ, if the density of air is negligible compared to 6.2 Viscometer Holders—Use viscometer holders to enable
that of the liquid. For any particular viscometer covered by this all viscometers which have the upper meniscus directly above
test method, the time of flow of a fixed volume of liquid is the lower meniscus to be suspended vertically within 1° in all
directly proportional to its kinematic viscosity, ν, where directions. Those viscometers whose upper meniscus is offset
ν = η ⁄ρ, and η is the dynamic viscosity. from directly above the lower meniscus shall be suspended
vertically within 0.3° in all directions (see Specifications D446
4. Summary of Test Method and ISO 3105).
4.1 The time is measured for a fixed volume of liquid to 6.2.1 Viscometers shall be mounted in the constant tempera-
flow under gravity through the capillary of a calibrated ture bath in the same manner as when calibrated and stated on
viscometer under a reproducible driving head and at a closely the certificate of calibration. See Specifications D446, see
controlled and known temperature. The kinematic viscosity Operating Instructions in Annexes A1–A3. For those viscom-
(determined value) is the product of the measured flow time eters which have Tube L (see Specifications D446) held
and the calibration constant of the viscometer. Two such vertical, vertical alignment shall be confirmed by using (1) a
determinations are needed from which to calculate a kinematic holder ensured to hold Tube L vertical, or (2) a bubble level
viscosity result that is the average of two acceptable deter- mounted on a rod designed to fit into Tube L, or (3) a plumb
mined values. line suspended from the center of Tube L, or (4) other internal
means of support provided in the constant temperature bath.
5. Significance and Use
6.3 Temperature-Controlled Bath—Use a transparent liquid
5.1 Many petroleum products, and some non-petroleum bath of sufficient depth such, that at no time during the
materials, are used as lubricants, and the correct operation of measurement of flow time, any portion of the sample in the
the equipment depends upon the appropriate viscosity of the viscometer is less than 20 mm below the surface of the bath
liquid being used. In addition, the viscosity of many petroleum liquid or less than 20 mm above the bottom of the bath.
fuels is important for the estimation of optimum storage, 6.3.1 Temperature Control—For each series of flow time
handling, and operational conditions. Thus, the accurate deter- measurements, the temperature control of the bath liquid shall
mination of viscosity is essential to many product specifica- be such that within the range from 15 °C to 100 °C, the
tions. temperature of the bath medium does not vary by more than
60.02 °C of the selected temperature over the length of the
6. Apparatus viscometer, or between the position of each viscometer, or at
6.1 Viscometers—Use only calibrated viscometers of the the location of the thermometer. For temperatures outside this
glass capillary type, capable of being used to determine range, the deviation from the desired temperature must not
kinematic viscosity within the limits of the precision given in exceed 60.05 °C.
the precision section. 6.4 Temperature Measuring Device in the Range from 0 °C
6.1.1 Viscometers listed in Table A1.1, whose specifications to 100 °C—Use either calibrated liquid-in-glass thermometers
meet those given in Specifications D446 and in ISO 3105 meet (Annex A2) with an accuracy after correction of 60.02 °C or
these requirements. It is not intended to restrict this test method better, or a digital contact thermometer as described in 6.4.2
to the use of only those viscometers listed in Table A1.1. with equal or better accuracy.
Annex A1 gives further guidance. 6.4.1 If calibrated liquid-in-glass thermometers are used, the
6.1.2 Automated Viscometers—Automated apparatus may use of two thermometers is recommended. The two
be used as long as they mimic the physical conditions, thermometers, with corrections applied, shall agree within
operations or processes of the manual apparatus. Any 0.04 °C.
viscometer, temperature measuring device, temperature
control, temperature controlled bath or timing device incorpo-
rated in the automated apparatus shall conform to the specifi-
cation for these components as stated in Section 6 of this test
method. Flow times of less than 200 s are permitted, however,

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D445 − 17
6.4.2 Digital contact thermometer meeting the following device of equal or better accuracy. When two temperature
requirements: measuring devices are used in the same bath, they shall agree
Criteria Minimum Requirements within 60.1 °C.
6.4.4 When using liquid-in-glass thermometers, such as
DCT E2877 Class A
Display resolution 0.01 °C, recommended 0.001 °C
those in Table A2.1, use a magnifying device to read the
Display accuracy ±20 mK (±0.02 °C) for combined probe and sen- thermometer to the nearest 1⁄5 division (for example, 0.01 °C or
sor 0.02 °F) to ensure that the required test temperature and
Sensor type RTD, such as a PRT or thermistor
Drift less than 10 mK (0.01 °C) per year
temperature control capabilities are met (see 10.1). It is
Response time less than or equal to 6 s as defined in Specifica- recommended that thermometer readings (and any corrections
tion E1137/E1137M supplied on the certificates of calibrations for the thermom-
Linearity 10 mK over range of intended use
Calibration Report The DCT shall have a report of temperature cali-
eters) be recorded on a periodic basis to demonstrate compli-
bration traceable to a national calibration or me- ance with the test method requirements. This information can
trology standards body issued by a competent be quite useful, especially when investigating issues or causes
calibration laboratory with demonstrated compe-
tency in temperature calibration. An ISO 17025
relating to testing accuracy and precision.
accredited laboratory with temperature calibration 6.5 Timing Device—Use any timing device, spring-wound
in its accreditation scope would meet this require-
ment. or digital, that is capable of taking readings with a discrimi-
Calibration Data The calibration report shall include at least 3 cali- nation of 0.1 s or better and has an accuracy within 60.07 %
bration temperatures at least 5 °C apart which
are appropriate for its intended use.
(see Annex A3) of the reading when tested over the minimum
and maximum intervals of expected flow times.
6.4.2.1 The DCT probe is to be immersed by more than its 6.5.1 Timing devices powered by alternating electric current
minimum immersion depth in a constant temperature bath so may be used if the current frequency is controlled to an
that the center of the probe’s sensing region is at the same level accuracy of 0.05 % or better. Alternating currents, as provided
as the lower half of the working capillary provided the probes by some public power systems, are intermittently rather than
minimum immersion depth is met and is no less than indicated continuously controlled. When used to actuate electrical timing
on calibration certificate. See Fig. 1. The end of the probe devices, such control can cause large errors in kinematic
sheath shall not extend past the bottom of the viscometer. It is viscosity flow time measurements.
preferable for the center of the sensing element to be located at
the same level as the lower half of the working capillary as 6.6 Ultrasonic Bath, Unheated—(optional), with an operat-
long as the minimum immersion requirements are met. ing frequency between 25 kHz to 60 kHz and a typical power
output of ≤100 W, of suitable dimensions to hold container(s)
NOTE 4—With respect to DCT probe immersion depth, a procedure is placed inside of bath, for use in effectively dissipating and
available in Test Method E644, Section 7, for determining the minimum
depth. With respect to an ice bath, Test Method E563 provides guidance removing air or gas bubbles that can be entrained in viscous
on the preparation of an ice bath however variance from the specific steps sample types prior to analysis. It is permissible to use ultra-
is permitted provided preparation is consistent as it is being used to track sonic baths with operating frequencies and power outputs
change in calibration. outside this range, however it is the responsibility of the
6.4.2.2 Verify the calibration at least annually. The probe laboratory to conduct a data comparison study to confirm that
shall be recalibrated, when the check value differs by more results determined with and without the use of such ultrasonic
than 0.01 °C from the last probe calibration. Verification can be baths does not materially impact results.
accomplished with the use of a water triple point cell, an ice
bath or other suitable constant temperature device which has a 7. Reagents and Materials
known temperature value of suitable precision. See Test 7.1 Chromic Acid Cleaning Solution, or a nonchromium-
Methods E563, E1750, and E2593 for more information containing, strongly oxidizing acid cleaning solution.
regarding checking calibrations. (Warning—Chromic acid is a health hazard. It is toxic, a
6.4.2.3 In the case of constant temperature baths used in recognized carcinogen, highly corrosive, and potentially haz-
instruments for automatic viscosity determinations, the user is ardous in contact with organic materials. If used, wear a full
to contact the instrument manufacturer for the correct DCT that face-shield and full-length protective clothing including suit-
has performance equivalence to that described here. able gloves. Avoid breathing vapor. Dispose of used chromic
6.4.3 Outside the range from 0 °C to 100 °C, use either acid carefully as it remains hazardous. Nonchromium-
calibrated liquid-in-glass thermometers of an accuracy after containing, strongly oxidizing acid cleaning solutions are also
correction of 60.05 °C or better, or any other thermometric highly corrosive and potentially hazardous in contact with

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D445 − 17

FIG. 1 Temperature Probe Immersion in Constant Temperature Bath

organic materials, but do not contain chromium which has 8. Certified Viscosity Reference Standards
special disposal problems.)
8.1 Certified viscosity reference standards shall be certified
7.2 Sample Solvent, completely miscible with the sample. by a laboratory that has been shown to meet the requirements
Filter before use. of ISO 17025 by independent assessment. Viscosity standards
7.2.1 For most samples a volatile petroleum spirit or naph- shall be traceable to master viscometer procedures described in
tha is suitable. For residual fuels, a prewash with an aromatic Test Method D2162.
solvent such as toluene or xylene may be necessary to remove
asphaltenic material. 8.2 The uncertainty of the certified viscosity reference
7.3 Drying Solvent, a volatile solvent miscible with the standard shall be stated for each certified value (k = 2, 95 %
sample solvent (see 7.2) and water (see 7.4). Filter before use. confidence). See ISO 5725 or NIST 1297.
7.3.1 Acetone is suitable. (Warning—Extremely flam-
mable.) 9. Calibration and Verification
7.4 Water, deionized or distilled and conforming to Speci- 9.1 Viscometers—Use only calibrated viscometers,
fication D1193 or Grade 3 of ISO 3696. Filter before use. thermometers, and timers as described in Section 6.

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D445 − 17
9.2 Certified Viscosity Reference Standards (Table A1.2)— 10.1.3 They should be viewed with a lens assembly giving
These are for use as confirmatory checks on the procedure in approximately five times magnification and be arranged to
the laboratory. eliminate parallax errors.
9.2.1 If the determined kinematic viscosity does not agree 10.2 Select a clean, dry, calibrated viscometer having a
within the acceptable tolerance band, as calculated from Annex range covering the estimated kinematic viscosity (that is, a
A4, of the certified value, recheck each step in the procedure, wide capillary for a very viscous liquid and a narrower
including thermometer and viscometer calibration, to locate the capillary for a more fluid liquid). The flow time for manual
source of error. Annex A1 gives details of standards available. viscometers shall not be less than 200 s or the longer time
NOTE 5—In previous issues of Test Method D445, limits of 60.35 % of noted in Specifications D446. Flow times of less than 200 s are
the certified value have been used. The data to support the limit of permitted for automated viscometers, provided they meet the
60.35 % cannot be verified. Annex A4 provides instructions on how to requirements of 6.1.2.
determine the tolerance band. The tolerance band combines both the
uncertainty of the certified viscosity reference standard as well as the
10.2.1 The specific details of operation vary for the different
uncertainty of the laboratory using the certified viscosity reference types of viscometers listed in Table A1.1. The operating
standard. instructions for the different types of viscometers are given in
9.2.1.1 As an alternative to the calculation in Annex A4, the Specifications D446.
approximate tolerance bands in Table 1 may be used. 10.2.2 When the test temperature is below the dew point, fill
9.2.2 The most common sources of error are caused by the viscometer in the normal manner as required in 11.1. To
particles of dust lodged in the capillary bore and temperature ensure that moisture does not condense or freeze on the walls
measurement errors. It must be appreciated that a correct result of the capillary, draw the test portion into the working capillary
obtained on a standard oil does not preclude the possibility of and timing bulb, place rubber stoppers into the tubes to hold
a counterbalancing combination of the possible sources of the test portion in place, and insert the viscometer into the bath.
error. After insertion, allow the viscometer to reach bath temperature,
and the remove the stoppers. When performing manual viscos-
9.3 The calibration constant, C, is dependent upon the ity determinations, do not use those viscometers which cannot
gravitational acceleration at the place of calibration and this be removed from the constant temperature bath for charging
must, therefore, be supplied by the standardization laboratory the sample portion.
together with the instrument constant. Where the acceleration 10.2.2.1 The use of loosely packed drying tubes affixed to
of gravity, g, differs by more that 0.1 %, correct the calibration the open ends of the viscometer is permitted, but not required.
constant as follows: If used, the drying tubes shall fit the design of the viscometer
C 2 5 ~ g 2 /g 1 ! 3 C 1 (1) and not restrict the flow of the sample by pressures created in
the instrument.
where the subscripts 1 and 2 indicate, respectively, the
10.2.3 Viscometers used for silicone fluids, fluorocarbons,
standardization laboratory and the testing laboratory.
and other liquids which are difficult to remove by the use of a
10. General Procedure for Kinematic Viscosity cleaning agent, shall be reserved for the exclusive use of those
fluids except during their calibration. Subject such viscometers
10.1 Adjust and maintain the viscometer bath at the required to calibration checks at frequent intervals. The solvent wash-
test temperature within the limits given in 6.3.1 taking account ings from these viscometers shall not be used for the cleaning
of the conditions given in Annex A2 and of the corrections of other viscometers.
supplied on the certificates of calibration for the thermometers.
10.1.1 Thermometers shall be held in an upright position 11. Procedure for Transparent Liquids
under the same conditions of immersion as when calibrated. 11.1 Although not mandatory, for some transparent liquid
10.1.2 In order to obtain the most reliable temperature sample types such as viscous oils that are prone to having
measurement, it is recommended that two thermometers with entrained air or gas bubbles present in the sample, the use of an
valid calibration certificates be used (see 6.4). 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
TABLE 1 Approximate Tolerance Bands specimen for analysis, with no material impact on results.
Charge the viscometer in the manner dictated by the design of
NOTE 1—The tolerance bands were determined using Practice D6617.
The calculation is documented in Research Report RR:D02-1498.A the instrument, this operation being in conformity with that
Viscosity of Reference Material, Tolerance Band employed when the instrument was calibrated. If the sample is
mm2/s thought or known to contain fibers or solid particles, filter
< 10 ±0.30 % through a 75 µm screen, either prior to or during charging (see
10 to 100 ±0.32 % Specifications D446).
100 to 1000 ±0.36 %
1000 to 10 000 ±0.42 % NOTE 6—To minimize the potential of particles passing through the
10 000 to 100 000 ±0.54 % filter from aggregating, it is recommended that the time lapse between
> 100 000 ±0.73 %
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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D445 − 17
11.1.2 With certain products which exhibit gel-like for the samples to be tested in the viscometer bath(s) at the
behavior, exercise care that flow time measurements are made required test temperature. If the viscometers are to be charged
at sufficiently high temperatures for such materials to flow prior to insertion in the viscometer bath, for example, Cannon
freely, so that similar kinematic viscosity results are obtained Fenske Opaque, see 12.2.1.
in viscometers of different capillary diameters. 12.1.4 Upon completion of step 12.1.2, vigorously stir each
11.1.3 Allow the charged viscometer to remain in the bath sample for approximately 20 s with a glass or steel rod of
long enough to reach the test temperature. Where one bath is sufficient length to reach the bottom of the container. For
used to accommodate several viscometers, never add or samples of a very waxy nature or oils of high kinematic
withdraw, or clean a viscometer while any other viscometer is viscosity, it may be necessary to increase the heating tempera-
in use for measuring a flow time. ture above 65 °C to achieve proper mixing. The sample should
11.1.4 Because this time will vary for different instruments,
be sufficiently fluid for ease of stirring and shaking.
for different temperatures, and for different kinematic
viscosities, establish a safe equilibrium time by trial. 12.1.5 Remove the stirring rod and inspect for sludge or
11.1.4.1 Thirty minutes should be sufficient except for the wax adhering to the rod. Continue stirring until there is no
highest kinematic viscosities. sludge or wax adhering to the rod.
11.1.5 Where the design of the viscometer requires it, adjust 12.1.6 Recap the container tightly and shake vigorously for
the volume of the sample to the mark after the sample has 1 min to complete the mixing. To protect the integrity of the
reached temperature equilibrium. sample should a repeat analysis be required, pour sufficient
11.2 Use suction (if the sample contains no volatile con- sample to fill two flasks and loosely stopper. (Each flask should
stituents) or pressure to adjust the head level of the test sample hold sufficient sample to fill two viscometers order to obtain
to a position in the capillary arm of the instrument about 7 mm two determinations. The second flask is required to carry out a
above the first timing mark, unless any other value is stated in repeat analysis.) If a repeat analysis is not a consideration the
the operating instructions for the viscometer. With the sample next steps can be performed using the original container,
flowing freely, measure, in seconds to within 0.1 s, the time loosely capped.
required for the meniscus to pass from the first to the second 12.1.7 Heat the first sample flask or sample container
timing mark. If this flow time is less than the specified between 100 ºC and 105 °C for 30 min.
minimum (see 10.2), select a viscometer with a capillary of 12.1.8 Remove the first sample flask or sample container
smaller diameter and repeat the operation. from the heat, close tightly, and shake vigorously for 60 s.
11.2.1 Repeat the procedure described in 11.2 to make a
second measurement of flow time. Record both measurements. 12.2 Two determinations of the kinematic viscosity of the
11.2.2 From the two measurements of flow time, calculate test material are required. For those viscometers that require a
two determined values of kinematic viscosity. complete cleaning after each flow time measurement, two
11.2.3 If the two determined values of kinematic viscosity viscometers must be used. These two determinations are used
calculated from the flow time measurements agree within the to calculate one result. Charge two viscometers in the manner
stated determinability figure (see 17.1.1) for the product, use dictated by the design of the instrument. For example, for the
the average of these determined values to calculate the kine- Lantz-Zeitfuchs Cross-arm or the BS/IP/RF U-tube reverse-
matic viscosity result to be reported. Record the result. If not, flow viscometers for opaque liquids, filter the sample through
repeat the measurements of flow times after a thorough a 75 µm filter into two viscometers previously placed in the
cleaning and drying of the viscometers and filtering (where bath. For samples subjected to heat treatment, use a preheated
required, see 11.1) of the sample until the calculated kinematic filter to prevent the sample coagulating during the filtration.
viscosity determinations agree with the stated determinability. 12.2.1 Viscometers which are charged before being inserted
11.2.4 If the material or temperature, or both, is not listed in into the bath may need to be preheated in an oven prior to
17.1.1, use 1.5 % as an estimate of the determinability. charging the sample. This is to ensure that the sample will not
be cooled below test temperature.
12. Procedure for Residual Fuel Oils and Opaque 12.2.2 After 10 min, adjust the volume of the sample (where
Liquids the design of the viscometer requires) to coincide with the
12.1 For steam-refined cylinder oils and black lubricating filling marks as in the viscometer specifications (see Specifi-
oils, proceed to 12.2 ensuring a thoroughly representative cations D446).
sample is used. The kinematic viscosity of residual fuel oils 12.2.3 Allow the charged viscometers enough time to reach
and similar waxy products can be affected by the previous the test temperature (see 12.2.1). Where one bath is used to
thermal history and the following procedure described in accommodate several viscometers, never add or withdraw, or
12.1.1 to 12.1.8 shall be followed to minimize this. clean a viscometer while any other viscometer is in use for
12.1.1 In general, the viscometers used for opaque liquids measuring flow time.
are of the reverse-flow type listed in Table A1.1, C.
12.1.2 Heat the sample in the original container at a 12.3 With the sample flowing freely, measure in seconds to
temperature between 60 °C and 65 °C for 1 h. within 0.1 s, the time required for the advancing ring of contact
12.1.3 Place the BS/IP/RF U-tube reverse-flow, or Zeitfuchs to pass from the first timing mark to the second. Record the
Cross-arm, or Lantz-Zeitfuchs type reverse-flow viscometer measurement.

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D445 − 17
12.3.1 In the case of samples requiring heat treatment 14. Calculation
described in 12.1 through 12.1.8, complete the measurements 14.1 Calculate each of the determined kinematic viscosity
of flow time within 1 h of completing 12.1.8. Record the values, ν1 and ν2, from the measured flow times, t1 and t2, and
measured flow times. the viscometer constant, C, by means of the following equa-
12.4 Calculate kinematic viscosity, ν, in millimetres squared tion:
per second, from each measured flow time. Regard these as two ν 1,2 5 C·t 1,2 (2)
determined values of kinematic viscosity.
12.4.1 For residual fuel oils, if the two determined values of where:
kinematic viscosity agree within the stated determinability ν1,2 = determined kinematic viscosity values for ν1 and ν2,
figure (see 17.1.1), use the average of these determined values respectively, mm2/s,
to calculate the kinematic viscosity result to be reported. This C = calibration constant of the viscometer, mm2/s2, and
constitutes one analysis. Record the result. If a second value t1,2 = measured flow times for t1 and t2, respectively, s.
(repeat) is required, then repeat the analysis after thorough Calculate the kinematic viscosity result, ν, as an average of
cleaning and drying of the viscometers starting from sample ν1 and ν2 (see 11.2.3 and 12.4.1).
preparation steps 12.1.6 using the second flask. If the original
container has been conditioned using steps 12.1.2 to 12.1.8, 14.2 Calculate the dynamic viscosity, η, from the calculated
then this is not suitable for a repeat analysis. If the calculated kinematic viscosity, ν, and the density, ρ, by means of the
kinematic viscosities do not agree, repeat the measurements of following equation:
flow times after thorough cleaning and drying of the viscom- η 5 ν 3 ρ 3 1023 (3)
eters and filtering of the sample. If the material or temperature,
where:
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 η = dynamic viscosity, mPa·s,
1.5 % for temperatures outside this range; it must be realized ρ = density, kg/m3, at the same temperature used for the
that these materials can be non-Newtonian, and can contain determination of the kinematic viscosity, and
ν = kinematic viscosity, mm2/s.
solids which can come out of solution as the flow time is being
measured. 14.2.1 The density of the sample can be determined at the
test temperature of the kinematic viscosity determination by an
13. Cleaning of Viscometer appropriate method such as Test Methods D1217, D1480, or
13.1 Between successive determinations of kinematic D1481.
viscosity, clean the viscometer thoroughly by several rinsings
with the sample solvent, followed by the drying solvent (see 15. Expression of Results
7.3). Dry the tube by passing a slow stream of filtered dry air
15.1 Report the test results for the kinematic or dynamic
through the viscometer for 2 min or until the last trace of
viscosity, or both, to four significant figures, together with the
solvent is removed.
test temperature.
13.2 If periodic verification of the viscometer calibration
using certified viscosity reference standards (see 9.2) is outside 16. Report
of the acceptable tolerance band, the viscometer may need to
be cleaned. Clean the viscometer with the cleaning solution 16.1 Report the following information:
(Warning—see 7.1), for several hours to remove residual 16.1.1 Type and identification of the product tested,
traces of organic deposits, rinse thoroughly with water (7.4) 16.1.2 Reference to this test method or a corresponding
and drying solvent (see 7.3), and dry with filtered dry air or a international standard,
vacuum line. Remove any inorganic deposits by hydrochloric 16.1.3 Result of the test (see Section 15),
acid treatment before the use of cleaning acid, particularly if 16.1.4 Any deviation, by agreement or otherwise, from the
the presence of barium salts is suspected. (Warning—It is procedure specified,
essential that alkaline cleaning solutions are not used as 16.1.5 Date of the test, and
changes in the viscometer calibration can occur.) 16.1.6 Name and address of the test laboratory.

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D445 − 17
17. Precision and Bias Additives at 100 °C14 0.00106 y1.1
Gas oils at 40 °C15 0.0013 (y+1)
17.1 Comparison of Determined Values: Jet fuels at –20 °C16 0.0018 y (0.18 %)
17.1.1 Determinability (d)—The difference between succes- Kerosine, diesel fuels, 0.0037 y (0.37 %)
sive determined values obtained by the same operator in the biodiesel fuels, and biodiesel
fuel blends at 40 °C17
same laboratory using the same apparatus for a series of
where: y is the average of determined values being com-
operations leading to a single result, would in the long run, in
pared.
the normal and correct operation of this test method, exceed the
17.1.2 The determinability for used (in-service) formulated
values indicated only in one case in twenty:
oils has not been determined, however use a limit of 1.0 % (see
Base oils at 40 °C10 0.0037 y (0.37 %)
Base oils at 100 °C10 0.0036 y (0.36 %)
12.4.1) for temperatures between 15 °C and 100 °C.18
Formulated oils at 40 °C10 0.0037 y (0.37 %)
Formulated oils at 100 °C10 0.0036 y (0.36 %) 14
Supporting data have been filed at ASTM International Headquarters and may
Formulated oils at 150 °C11 0.015 y (1.5 %) be obtained by requesting Research Report RR:D02-1421. These precision values
Petroleum wax at 100 °C12 0.0080 y (0.80 %) were obtained by statistical examination of interlaboratory results from eight
Residual fuel oils at 50 °C13 0.0244 y (2.44 %) additives in the range from 145 mm2/s to 1500 mm2/s at 100 °C and were first
Residual fuel oils at 100 °C13 0.03 y (3 %) available in 1997.
15
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
10
Supporting data has been filed at ASTM International Headquarters and may oils in the range from 1 mm2/s to 13 mm2/s at 40 °C and were first available in 1997.
be obtained by requesting Research Report RR:D02-1788. These precision values Kerosine and diesel fuel samples, which can be considered as gas oils, were
were obtained by statistical examination of interlaboratory results for the following included in a dataset to determine the precision for kerosine, diesel fuels, biodiesel
samples: Base Oils with viscosities between (12.0 and 476.0) mm2/s at 40 °C tested fuels, and biodiesel fuel blends at 40 °C (RR:D02-1780). The precision stated in
in seven laboratories; Formulated Oils with viscosities between (28.0 and 472.0) RR:D02-1780 was developed in a more recent interlaboratory study than the
mm2/s at 40 °C tested in seven laboratories; Base Oils with viscosities between (2.90 precision stated in RR RR:D02-1422. Therefore, the gas oil precision statements do
and 32.0) mm2/s at 100 °C tested in eight laboratories; Formulated Oils with not apply to kerosine and diesel fuels and a user should refer to the precision
viscosities between (6.50 and 107.0) mm2/s at 100 °C tested in eight laboratories. statements for kerosine, diesel fuels, biodiesel fuels, and biodiesel fuel blends at
Formulated Oils include automatic transmission fluids, hydraulic fluids, motor oils, 40 °C.
16
gear oils, polymers in base oil and additives in base oil. The determinability, Supporting data have been filed at ASTM International Headquarters and may
repeatability, and reproducibility results are for tests performed with manual be obtained by requesting Research Report RR:D02-1420. These precision values
viscometers. Determinability, repeatability, and reproducibility for automated/ were obtained by statistical examination of interlaboratory results from nine jet fuels
automatic instruments are no worse than that for the manual instruments. For the in the range from 4.3 mm2/s to 5.6 mm2/s at– 20 °C and were first available in 1997.
17
precision of specific automated/automatic instruments see Research Report Supporting data have been filed at ASTM International Headquarters and may
RR:D02-1820. be obtained by requesting Research Report RR:D02-1780. These precision values
11
Supporting data have been filed at ASTM International Headquarters and may were obtained by statistical examination of interlaboratory results from seven
be obtained by requesting Research Report RR:D02-1333. These precision values samples including kerosine, diesel fuels, biodiesel fuels, and biodiesel fuel blends
were obtained by statistical examination of interlaboratory results for eight fully (RR:D02-1780) in the range from 2.06 mm2/s to 4.50 mm2/s at 40 °C. The
formulated engine oils in the range from 7 mm2/s to 19 mm2/s at 150 °C, and first determinability, repeatability, and reproducibility results are for tests performed with
published in 1991. See Guide D6074. manual viscometers. Determinability, repeatability, and reproducibility for
12
Supporting data have been filed at ASTM International Headquarters and may automated/automatic instruments are no worse than that for the manual instruments.
be obtained by requesting Research Report RR:D02-1334. These precision values For the precision of specific automated/automatic instruments see Research Report
were obtained by statistical examination of interlaboratory results from five RR:D02-1820.
petroleum waxes in the range from 3 mm2/s to 16 mm2/s at 100 °C, and were first 18
Supporting data have been filed at ASTM International Headquarters and may
published in 1988. be obtained by requesting Research Report RR:D02-1852. The precision values
13
Supporting data have been filed at ASTM International Headquarters and may were obtained by statistical examination of interlaboratory results from 10 used
be obtained by requesting Research Report RR:D02-1837. These precision values (in-service) formulated oil samples. These consisted of steam turbine, gas turbine,
were obtained by statistical examination of interlaboratory results from eleven diesel engine, hydraulic, and gasoline engine oil samples which were analyzed by 10
laboratories on residual fuel oil samples conforming to D396Grades 5 or 6 and/or laboratories using both manual and automated apparatuses. The kinematic viscosi-
ISO8217 RMG and RMK at 50 °C and 10 at 100 °C in the range from 27.34 mm2/s ties of these samples ranged from 25 mm2/s to 125 mm2/s at 40 °C, and from 6
to 2395 mm2/s at 50 °C. and 6.36 mm2/s to 120.8 mm2/s at 100 °C These precision mm2/s to 16 mm2/s at 100 °C. The statistical output is based on 10 laboratories and
statements only refer to measurement of viscosity using manual viscometers. 8 samples at 40 °C and 10 laboratories and 10 samples at 100 °C.

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D445 − 17
17.2 Comparison of Results: 17.3 The precision for specific automated and automatic
17.2.1 Repeatability (r)—The difference between successive viscometers has been determined for sample types and tem-
results obtained by the same operator in the same laboratory peratures listed in 17.3.1. An analysis has been made of a large
with the same apparatus under constant operating conditions on dataset including both automated/automatic and manual vis-
identical test material would, in the long run, in the normal and cometers over the temperature range of 40 °C to 100 °C for the
correct operation of this test method, exceed the values sample types listed in 17.3.1. The determinability, repeatability,
indicated only in one case in twenty: and reproducibility of automated/automatic viscometer data are
Base oils at 40 °C 10 0.0101 x (1.01 %)
no worse than the determinability, repeatability, and reproduc-
Base oils at 100 °C10 0.0085 x (0.85 %) ibility for the manual instruments. It is also shown in the
Formulated oils at 40 °C10 0.0074 x (0.74 %) research reports that no statistically significant bias was ob-
Formulated oils at 100 °C10 0.0084 x (0.84 %)
Formulated oils at 150 °C11 0.0056 x (0.56 %)
served between the automated/automatic data in comparison to
Petroleum wax at 100 °C12 0.0141 x1.2 the manual data.19 For the precision of specific automated/
Residual fuel oils at 80 °C13 0.013 (x + 8) automatic instruments, see RR:D02-1820.20
Residual fuel oils at 100 °C13 0.08088 x (8.08 %)
Residual oils at 50 °C13 0.07885 x (7.88 %)
17.3.1 The determinability, repeatability, and reproducibil-
Additives at 100 °C14 0.00192 x1.1 ity have been determined for automated/automatic viscometers
Gas oils at 40 °C15 0.0043 (x+1) for the following sample types and temperatures:
Jet fuels at –20 °C16 0.007 x (0.7 %)
Kerosine, diesel fuels, biodiesel 0.0056 x (0.56 %)
Distillates, fatty acid methyl esters, and distillates contain-
fuels, and biodiesel fuel blends at ing fatty acid methyl esters at 40 °C
40 °C17 Base oils at 40 °C and 100 °C
Used (in-service) formulated oils at 0.000233 x1.722
40 °C18
Formulated oils at 40 °C and 100 °C
Used (in-service) formulated oils at 0.001005 x1.4633 For these sample types, determinability, repeatability, and
100 °C18 reproducibility for automated/automatic instruments are no
where: x is the average of results being compared. worse than that for the manual instruments. For the precision of
17.2.1.1 The degrees of freedom associated with the repeat- specific automated/automatic instruments see Research Report
ability estimate for the kerosine, diesel fuels, biodiesel fuels, RR:D02-1820.
and biodiesel fuel blends at 40 °C round robin study are 16. The precision has been determined for automated viscom-
Since the minimum requirement of 30 (in accordance with eters and the range of r and R values for automated instruments
Practice D6300) is not met, users are cautioned that the actual is shown in RR:D02-1820. For the samples listed in RR:D02-
repeatability may be significantly different than these esti- 1820, precision for automated instruments is no worse than that
mates. for the manual instruments.21
17.3.1.1 Degree of Agreement between Results by Manual
17.2.2 Reproducibility (R)—The difference between two
and Automated Instruments in Test Method D445—Results for
single and independent results obtained by different operators
the sample types listed in RR:D02-1820 produced by Manual
working in different laboratories on nominally identical test
and Automated Instruments in this test method have been
material would, in the long run, in the normal and correct
assessed in accordance with procedures outlined in Practice
operation of this test method, exceed the values indicated
D6708.
below only in one case in twenty.
17.3.1.2 The findings are: Results from Manual and Auto-
Base oils at 40 °C10 0.0136 x (1.36 %) mated Instruments in Test Method D445 may be considered to
Base oils at 100 °C10 0.0190 x (1.90 %)
Formulated oils at 40 °C10 0.0122 x (1.22 %) be practically equivalent, for sample types listed in RR:D02-
Formulated oils at 100 °C10 0.0138 x (1.38 %) 1820. No sample-specific bias, as defined in Practice D6708,
Formulated oils at 150 °C11 0.018 x (1.8 %) was observed for the materials studied. Differences between
Petroleum wax at 100 °C12 0.0366 x1.2
Residual fuel oils at 80 °C13 0.04 (x + 8) results from Manual and Automated Instruments in Test
Residual fuel oils at 100 °C13 0.1206 (12.06 %) Method D445, for the samples listed in RR:D02-1820, are
Residual oils at 50 °C13 0.08461 x (8.46 %)
expected to exceed the following between methods reproduc-
Additives at 100 °C14 0.00862 x1.1
Gas oils at 40 °C15 0.0082 (x+1) ibility; 1.91 % for distillates, fatty acid methyl esters, and
Jet fuels at –20 °C16 0.019 x (1.9 %) distillates containing fatty acid methyl esters at 40 °C; 1.27 %
Kerosine, diesel fuels, biodiesel fuels, 0.0224 x (2.24 %)
and biodiesel fuel blends at 40 °C17
for base oils at 40 °C; 1.23 % for formulated oils at 40 °C,
Used (in-service) formulated oils at 0.000594 x1.722
40 °C18
Used (in-service) formulated oils at 0.003361 x1.4633
19
100 °C18 Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1498.
where: x is the average of results being compared. 20
Supporting data have been filed at ASTM International Headquarters and may
17.2.2.1 The degrees of freedom associated with the repro- be obtained by requesting Research Report RR:D02-1820. Contact ASTM Customer
Service at service@astm.org.
ducibility estimate for the kerosine, diesel fuels, biodiesel 21
Supporting data have been filed at ASTM International Headquarters and may
fuels, and biodiesel fuel blends at 40 °C round robin study are be obtained by requesting Research Report RR:D02-1787. These precision values
19. Since the minimum requirement of 30 (in accordance with were obtained by statistical examination of interlaboratory results from seven
samples including distillates, fatty acid methyl esters, and distillates containing fatty
Practice D6300) is not met, users are cautioned that the actual
acid methyl esters (RR:D02-1790) in the range from (2.06 to 4.50) mm2/s at 40 °C.
reproducibility may be significantly different than these esti- These seven samples were tested in 21 different Cannon and Herzog instruments to
mates. obtain the precision values shown.

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D445 − 17
1.70 % for base oils at 100 °C; 1.21 % for formulated oils at 18. Keywords
100 °C, as defined in Practice D6708, about 5 % of the time. 18.1 dynamic viscosity; kinematic viscosity; viscometer;
These percent differences are based upon the highest calculated viscosity
combined method reproducibilities (Rxy in Practice D6708).22

22
Supporting data has been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1787. These precision values
were obtained by statistical examination of interlaboratory results for the following
samples: Base Oils with viscosities between (12.0 and 476.0) mm2/s at 40 °C tested
in 22 laboratories; Formulated Oils with viscosities between (28.0 and 472.0) mm2/s
at 40 °C tested in 22 laboratories; Base Oils with viscosities between (2.90 and 32.0)
mm2/s at 100 °C tested in 21 laboratories; Formulated Oils with viscosities between
(6.50 and 107.0) mm2/s at 100 °C tested in 21 laboratories. Formulated Oils include
automatic transmission fluids, hydraulic fluids, motor oils, gear oils, polymers in
base oil, and additives in base oil.

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 Cannon-Fenske routineB 0.5 to 20 000
specifications, operating instructions, and calibration, refer to Zeitfuchs
B
0.6 to 3 000
BS/U-tube 0.9 to 10 000
specifications in Specifications D446. BS/U/M miniature 0.2 to 100
SILB 0.6 to 10 000
A1.1.2 Table A1.2 lists certified viscosity reference stan- Cannon-Manning semi-micro 0.4 to 20 000
dards. PinkevitchB 0.6 to 17 000
B. Suspended-level Types for Transparent Liquids
BS/IP/SLB 3.5 to 100 000
B
BS/IP/SL(S) 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 D446.
B
In each of these series, the minimum flow time for the viscometers with lowest
constants exceeds 200 s.

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D445 − 17
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 Liquid-in-Glass Thermom- this requirement. The calibration report shall include data for a
eter series of temperatures which are appropriate for its intended
A2.1.1 Use a short-range specialized Liquid-in-Glass ther- use.
mometer conforming to the generic specification given in Table A2.2.2 The scale correction of liquid-in-glass thermometers
A2.1 and Table A2.2 and to one of the designs shown in Fig. can change during storage and use. Therefore, regular in-house
A2.1. As an alternative, use a Digital Contact Thermometer ice point verifications are required, and can be achieved within
(DCT) as defined in 6.4.2. the working laboratory, using an ice melting bath. However,
A2.1.2 The difference in the designs of the liquid-in-glass these checks may not be an adequate means of recalibration as
thermometers rests mainly in the position of the ice point scale. the use of a single-point recalibration at the ice point adds an
In Design A, the ice point is within the scale range, in Design additional uncertainty to the updated thermometer calibration
B, the ice point is below the scale range, and in Design C, the result at every temperature but the ice point. The user must
ice point is above the scale range. determine if the thermometer requires complete re-calibration
A2.2 Calibration to continue to meet the expanded measurement uncertainty
requirements of this section. NIST Special Publication 1088,
A2.2.1 When using a liquid-in-glass thermometer, it shall Section 7.9 on determining uncertainty of correction, may be
have a report of temperature calibration traceable to a national helpful to the user in making this decision. If in-house ice point
calibration or metrology standards body issued by a competent
verification brings the expanded measurement uncertainty out
calibration laboratory with demonstrated competency in tem-
of the requirements of A2.2.1, complete recalibration at a
perature calibration. An ISO 17025 accredited laboratory with
laboratory meeting the requirements of A2.2.1 is required.
temperature calibration in its accreditation scope would meet

TABLE A2.1 General Specification for Thermometers


NOTE 1—Table 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 0.05
Long lines at each °C 0.1 and 0.5
Numbers at each °C 1
Maximum line width mm 0.10
Scale error at test temperature, max °C 0.1
Expansion chamber:
Permit heating to °C 105 up to 90, 120 between 90 and 95
130 between 95 and 105, 170 above
105
Total length mm 300 to 310
Stem outside diameter mm 6.0 to 8.0
Bulb length mm 45 to 55
Bulb outside diameter mm no greater than stem
Length of scale range mm 40 to 90

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D445 − 17
TABLE A2.2 Complying Thermometers
Test Test
Thermometer No. Temperature Thermometer No. Temperature
°C °F °C °F
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
ASTM 121C/IP 32C 98.9, 210, ASTM 127C/IP 99C −20 −4
100 212 ASTM 126C, F/IP 71C −26.1 −20
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
IP 100C 80
ASTM 47C, F/IP 35C 60 140
ASTM 29C, F/IP 34C 54.4 130
ASTM 46C F/IP 66C 50 122
ASTM 120C/IP 92C 40
ASTM 28C, F/IP 31C 37.8 100
ASTM 118C, F 30 86
ASTM 45C, F/IP 30C 25 77
ASTM 44C, F/IP 29C 20 68

FIG. A2.1 Thermometer Designs

A2.2.2.1 For liquid-in-glass thermometers, the interval for the first six months is recommended. A change of one or more
ice-point verification shall be no longer than six months (see scale divisions in the ice point means that the thermometer may
NIST GMP 11). For new thermometers, monthly checking for have been overheated or damaged, and it may be out of

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D445 − 17
calibration. Such thermometers shall be removed from service A2.2.3.4 Record the ice-point readings and determine the
until inspected, or recalibrated, or both. thermometer correction at this temperature from the mean
A2.2.2.2 Keep records of all recalibration. reading. If the correction is found to be higher or lower than
A2.2.3 Procedure for Ice-point Verification of Liquid-in- that corresponding to a previous calibration, change the cor-
Glass Thermometers. rection at all other temperatures by the same value. See A2.2.1
A2.2.3.1 Unless otherwise listed on the certificate of for discussion on expanded measurement uncertainty changes
calibration, the recalibration of calibrated kinematic viscosity when changing correction values from ice point verifications.
thermometers requires that the ice-point reading shall be taken A2.2.3.5 During the procedure, apply the following condi-
within 60 min after being at test temperature for not less than tions:
3 min. NIST Special Publication 1088 from the NIST website (1) The thermometer shall be supported vertically.
describes an effective procedure for ice point verification, (2) View the thermometer with an optical aid that gives a
including all formulae necessary for calculations of change of magnification of approximately five and also eliminates paral-
correction and measurement uncertainty. Alternatively use Test lax.
Method E563 or those in A2.2.3.2 through A2.2.3.5. (3) Express the ice-point reading to the nearest 0.01 °C.
A2.2.3.2 Select clear pieces of ice, preferably made from
distilled or pure water. Discard any cloudy or unsound por- A2.2.4 When in use, immerse the thermometric device to
tions. Rinse the ice with distilled water and shave or crush into the same depth as when it was fully calibrated. For example, if
small pieces, avoiding direct contact with the hands or any a liquid-in-glass thermometer was calibrated at the normal total
chemically unclean objects. Fill the Dewar vessel with the immersion condition, it shall be immersed to the top of the
crushed ice and add sufficient water to form a slush, but not mercury column with the remainder of the stem and the
enough to float the ice. As the ice melts, drain off some of the expansion volume at the uppermost end exposed to room
water and add more crushed ice. Insert the thermometer, and temperature and pressure. In practice, this means that the top of
pack the ice gently about the stem, to a depth approximately the mercury column shall be within a length equivalent to four
one scale division below the 0 °C graduation. scale divisions of the surface of the medium whose temperature
A2.2.3.3 After at least 3 min have elapsed, tap the thermom- is being measured.
eter gently and repeatedly at right angles to its axis while
A2.2.4.1 If this condition cannot be met, then an extra
making observations. Successive readings taken at least 1 min
apart shall agree within 0.005 °C. correction may be necessary.

A3. TIMER ACCURACY

A3.1 Regularly check timers for accuracy and maintain WWV Fort Collins, CO (2.5, 5, 10, 15, 20) MHz
records of such checks. WWVH Kauai, HI (2.5, 5, 10, 15) MHz
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.

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

NOTE A4.1—These calculations are based on Practice D6617. A4.2 Determine the combined extended uncertainty (CEU)
of the accepted reference value (ARV) of the certified reference
A4.1 Determine the standard deviation for site uncertainty,
material (CRM) from the supplier’s label or included docu-
σsite, from a laboratory quality control program. (See Practice
mentation. In this test method, the CRM is the Certified
D6299.)
Viscosity Reference Standard (CVRS) as defined in 9.2.
A4.1.1 If the standard deviation for site uncertainty, σsite, is NOTE A4.2—Combined Extended Uncertainty (CEU) is equivalent to
not known, use the value 0.19 %. Expanded Uncertainty (U). See NIST Technical Note 1297.

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D445 − 17
A4.3 Calculate the standard error of the accepted reference k 5 2 ~ from the CVRS label or documentation!
value (SEARV) by dividing the CEU by the coverage factor, k,
listed on the supplier’s label or included documentation. 0.22
SEARV 5 5 0.11
2
CEUARV
SEARV 5 (A4.1)
k TZ 5 61.44=0.192 10.112 5 61.44=0.036110.0121 5 60.32 %
NOTE A4.3—Standard Error (SEARV) is equivalent to Combined Stan-
dard Uncertainty (UC). See NIST Technical Note 1297. A4.5.1 In this example, the tolerance zone will be 60.32 %
A4.3.1 If the coverage factor, k, is not known, use the value of the certified viscosity reference standard value on the report
2. of test or bottle label. If this site uses a CVRS (for example)
with a kinematic viscosity of 33.98 mm2/s, the TZ =
A4.4 Construct the acceptable tolerance zone:
33.87 mm2/s to 34.09 mm2/s, with 95 % certainty. Viscosity
TZ 5 61.44 =σ site
2 2
1SEARV (A4.2) measurements made with this CVRS at that site should fall
within that tolerance zone (band) 19 out of 20 times.
A4.5 Worked out example for kinematic viscosity zone
(band):
σ site 5 0.19 % ~ default value from A4.1.1! (A4.3)

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

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SUMMARY OF CHANGES

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D445 – 16) that may impact the use of this standard. (Approved Jan. 1, 2017.)

(1) Added precision estimates for used (in-service) formulated (3) Deleted former subsection 17.3.
oils in 17.2.1 and 17.2.2.
(2) Added new footnote 18 describing the ILS conducted for
the above addition.

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D445 – 15a) that may impact the use of this standard. (Approved Dec. 15, 2016.)

(1) Revised subsection 13.2. (3) Updated subsections 17.1.1, 17.2.1, and 17.2.2 on
(2) Revised Section 12 on sample preparation of residual fuel determinability, repeatability, and reproducibility of residual
oils. fuel oils at 50 °C and 100 °C; updated footnote (13) with
information on residual fuel oil interlaboratory study.

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