Astm 482
Astm 482
Astm 482
1. Scope*
1.1 This test method specifies a procedure for the determination of the kinematic viscosity, ν, 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, η, can be obtained by multiplying the kinematic viscosity, ν, by the density, ρ, of the liquid.
iTeh Standards
NOTE 1—For the measurement of the kinematic viscosity and viscosity of bitumens, see also Test Methods D2170 and D2171.
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 mPa·s. For user reference, 1 mm2/s = 10-6 m2/s = 1 cSt
and 1 mPa·s = 1 cP = 0.001 Pa·s.
1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious
medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use Caution
when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional
information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national
law. Users must determine legality of sales in their location.
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1
This test method is under the jurisdiction of Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee D02.07
on Flow Properties.
Current edition approved Nov. 1, 2023April 1, 2024. Published November 2023April 2024. Originally approved in 1937. Last previous edition approved in 20212023 as
D445 – 21D445 – 23.ɛ2. DOI: 10.1520/D0445-23.10.1520/D0445-24.
1
D445 − 24
1.7 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.
2. Referenced Documents
iTeh Standards
D6617 Practice for Laboratory Bias Detection Using Single Test Result from Standard Material
D6708 Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purport
(https://standards.iteh.ai)
to Measure the Same Property of a Material
D8278 Specification for Digital Contact Thermometers for Test Methods Measuring Flow Properties of Fuels and Lubricants
E1 Specification for ASTM Liquid-in-Glass Thermometers
Document Preview
E77 Test Method for Inspection and Verification of Thermometers
E563 Practice for Preparation and Use of an Ice-Point Bath as a Reference Temperature
E1750 Guide for Use of Water Triple Point Cells
E2593 Guide for Accuracy Verification of IndustrialASTM
PlatinumD445-24
Resistance Thermometers
https://standards.iteh.ai/catalog/standards/astm/1b010020-1802-46c8-ac82-0e2024b174cd/astm-d445-24
2.2 ISO Standards:4
ISO 3104 Petroleum products—Transparent and opaque liquids—Determination 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 standards—Guidelines for selection and use
ISO 17025 General requirements for the competence of testing and calibration laboratories
2.3 NIST Standards:5
NIST Technical Note 1297 Guideline for Evaluating and Expressing the Uncertainty of NIST Measurement Results6
NIST GMP 11 Good Measurement Practice for Assignment and Adjustment of Calibration Intervals for Laboratory Standards7
NIST Special Publication 811 Guide for the Use of the International System of Units (SI)8
NIST Special Publication 1088 Maintenance and Validation of Liquid-in-Glass Thermometers9
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [email protected]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.
4
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
5
Available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460.
6
http://physics.nist.gov/cuu/Uncertainty/bibliography.html
7
http://ts.nist.gov/WeightsAndMeasures/upload/GMP_11_Mar_2003.pdf
8
http://www.nist.gov/pml/pubs/sp811/index.cfm
9
http://www.nist.gov/pml/pubs/sp1088/index.cfm
2
D445 − 24
3. Terminology
3.2.1 digital contact thermometer (DCT), n—an electronic device consisting of a digital display and associated temperature
sensing probe.
3.2.1.1 Discussion—
This 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.
3.2.1.2 Discussion—
The devices are often referred to as a “digital thermometers,” however the term includes devices that sense temperature by means
other than being in physical contact with the media.
3.2.1.3 Discussion—
PET is an acronym for portable electronic thermometers, a subset of digital contact thermometers (DCT).
3.3 Definitions of Terms Specific to This Standard:
3.3.1 automated viscometer, n—apparatus 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 Discussion—
Automated 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
iTeh Standards
those used in this test method are not considered to be Automated Viscometers.
(https://standards.iteh.ai)
3.3.2 density, n—the mass per unit volume of a substance at a given temperature.
Document Preview
3.3.3 dynamic viscosity, η, n—the ratio between the applied shear stress and rate of shear of a material.
3.3.3.1 Discussion—
It 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 material’s ability to transfer momentum in response to steady or time-dependent external
ASTM D445-24
shear forces. Dynamic viscosity has the dimension of mass divided by length and time and its SI unit is pascal times second (Pa·s).
https://standards.iteh.ai/catalog/standards/astm/1b010020-1802-46c8-ac82-0e2024b174cd/astm-d445-24
Among the transport properties for heat, mass, and momentum transfer, dynamic viscosity is the momentum conductivity.
3.3.4 kinematic viscosity, ν, n—the ratio of the dynamic viscosity (η) to the density (ρ) of a material at the same temperature and
pressure.
3.3.4.1 Discussion—
Kinematic viscosity is the ratio between momentum transport and momentum storage. Such 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 Discussion—
Formerly, 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 Discussion—
For gravity-driven flow under a given hydrostatic head, the pressure head of a liquid is proportional to its density, ρ, 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, ν, where ν = η ⁄ρ, and η is the dynamic viscosity.
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
10
International Vocabulary of Metrology — Basic and General Concepts and Associated Terms (VIM), 3rd ed., 2008, http://www.bipm.org/en/publications/guides/
vim.html.
3
D445 − 24
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.
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 Viscometers—Use 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 Viscometers—Automated 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 D446. The kinetic energy correction shall not
iTeh Standards
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 has been determined for automated
(https://standards.iteh.ai)
viscometers tested on the sample types listed in 17.3.1 and is no worse than the manual apparatus (that is, exhibits the same or
less variability).
Document Preview
NOTE 3—Precision and bias of kinematic viscosity measurements for flow times as low as 10 s have been determined for automated instruments tested
with the sample types listed in 17.3.1.
ASTM
6.2 Viscometer Holders—Use viscometer holders to enable allD445-24
viscometers which have the upper meniscus directly above the
https://standards.iteh.ai/catalog/standards/astm/1b010020-1802-46c8-ac82-0e2024b174cd/astm-d445-24
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 A1–A3. 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.
6.3 Temperature-Controlled Bath—Use 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 Control—For 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.
6.4.1 Liquid-in-glass Thermometers—Use calibrated thermometers noted in Annex A2. Devices with a nominal temperature range
from 0 °C to 100 °C will have an accuracy after correction of 60.02 °C or better. When the nominal temperature range is outside
the 0 °C to 100 °C range, they will have an accuracy after correction of 60.05 °C or better.
4
D445 − 24
6.4.1.1 If calibrated liquid-in-glass thermometers are used, the use of two thermometers is recommended. When the temperature
range is from 0 °C to 100 °C, the two thermometers, with corrections applied, shall agree within 0.04 °C. When the temperature
range is outside 0 °C to 100 °C, the two thermometers, with corrections applied, shall agree to within 0.1 °C.
6.4.2 Digital Contact Thermometer—Use the indicated DCT for the following nominal temperature ranges:
6.4.2.1 Verify the calibration at least annually. The probe shall be recalibrated when the check value differs by more than 0.02 °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 Practice E563 and Guides
E1750 and E2593 for more information regarding checking calibrations.
6.4.2.2 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 device of equal or better accuracy. When two temperature measuring devices are
used in the same bath, they shall agree within 60.1 °C.
6.4.5 When using liquid-in-glass thermometers, such as those in Table A2.1, use a magnifying device to read the thermometer to
the nearest 1⁄5 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.
6.5 Timing Device for Manual Viscometers—Use any timing device, mechanical (spring-wound or motor driven) 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 motors 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.
6.5.2 Timing devices employed in automated viscometers are an integral part of the apparatus and typically are digital (using a
precision crystal oscillator) with discriminations of 0.01 s or better. As such, the timing devices are included within the overall
system calibration of automated viscometers. Follow the manufacturer’s instructions for ensuring the automated viscometer is
properly calibrated using CRM’s such that it is capable of determining kinematic viscosity of a certified viscosity reference
standard within the limits stated in 9.2.1 and Section 17 (see 6.1.2).
6.6 Ultrasonic Bath, Unheated—(optional), with an operating frequency between 25 kHz to 60 kHz and a typical power output
5
D445 − 24
iTeh Standards
(https://standards.iteh.ai)
Document Preview
ASTM D445-24
https://standards.iteh.ai/catalog/standards/astm/1b010020-1802-46c8-ac82-0e2024b174cd/astm-d445-24
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.
7. Reagents and Materials
7.1 Chromic Acid Cleaning Solution, or a nonchromium-containing, strongly oxidizing acid cleaning solution. (Warning—
Chromic 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. Nonchromium-containing, strongly oxidizing acid cleaning
solutions are also highly corrosive and potentially hazardous in contact with organic materials, but do not contain chromium which
has special disposal problems.)
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.
6
D445 − 24
7.3 Drying Solvent, a volatile solvent miscible with the sample solvent (see 7.2) and water (see 7.4). Filter before use.
7.4 Water, deionized or distilled and conforming to Specification D1193 or Grade 3 of ISO 3696. Filter before use.
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 Practice
D2162.
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.
9.1 Viscometers—Use only calibrated viscometers, thermometers, and timers as described in Section 6.
9.2 Certified Viscosity Reference Standards (Table A1.2)—These are for use as confirmatory checks on the procedure in the
laboratory.
iTeh Standards
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
(https://standards.iteh.ai)
error. Annex A1 gives details of standards available.
Document Preview
NOTE 4—In 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.
ASTM
9.2.1.1 As an alternative to the calculation in Annex A4, D445-24 tolerance bands in Table 1 may be used.
the approximate
https://standards.iteh.ai/catalog/standards/astm/1b010020-1802-46c8-ac82-0e2024b174cd/astm-d445-24
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 than 0.1 %, correct the calibration constant as follows:
C 2 5 ~g 2/g 1! ×C 1 (1)
where the subscripts 1 and 2 indicate, respectively, the standardization laboratory and the testing laboratory.
7
D445 − 24
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).
10.1.3 They should be viewed with a lens assembly giving approximately five times magnification and be arranged to eliminate
parallax errors.
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 ambient dew point, the use of loosely-packed drying tubes affixed to the open ends
of the viscometer is permitted but not mandatory. These are designed to prevent water condensation. It is essential that they do
iTeh Standards
not set up a pressure differential and affect the rate of flow. Before the first use of drying tubes, it is recommended that a certified
viscosity reference standard is used to verify the correct use of the viscometer with and without drying tubes in order to ensure
that there is no restriction in the flow. When the test temperature is below the dew point, fill the viscometer in the normal manner
(https://standards.iteh.ai)
as required in 11.1. It is recommended to charge the viscometer outside the bath. 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
Document Preview
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 then 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.
ASTM D445-24
10.2.3 Viscometers used for silicone fluids, fluorocarbons, and other liquids which are difficult to remove by the use of a cleaning
https://standards.iteh.ai/catalog/standards/astm/1b010020-1802-46c8-ac82-0e2024b174cd/astm-d445-24
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.
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 µm screen, either prior to or during charging (see Specifications D446).
NOTE 5—To 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.
11.1.1 In general, the viscometers used for transparent liquids are of the type listed in Table A1.1; however, for the manual
measurement of kinematic viscosity of jet fuels at –20 °C only suspended-level type viscometers as noted in Table A1.1 shall be
used. The suspended level type viscometer types used for jet fuel do not require a correction to the calibration constant for the test
temperature being used.
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.
8
D445 − 24
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, however a minimum of 30 min is
specifically required for manual analysis of jet fuels at −20 °C.
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.
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.
iTeh Standards
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
(https://standards.iteh.ai)
result to be reported. Record the result. If not, repeat the measurements of flow times (11.2 to 11.2.2) after a thorough cleaning
and drying of the viscometers and filtering (where required, see 11.1) of the sample until the calculated kinematic viscosity
Document Preview
determinations agree with the stated determinability.
NOTE 6—Poor determinability can be the result of several factors including: air bubbles trapped in the sample within the viscometer, poor temperature
stability of the constant temperature bath, particulate contamination in the viscometer, or specimen heterogeneity. Additional sample-specific issues may
be conformational changes related to time and thermal historyASTM D445-24
(incomplete reaction of blended chemistries, re-alignment of polymeric chains, or
https://standards.iteh.ai/catalog/standards/astm/1b010020-1802-46c8-ac82-0e2024b174cd/astm-d445-24
outgassing of un-reacted
portion of the sample).
components) or the sample is a binary mixture of mixed phases (i.e., there may be precipitated solids such as waxes in the liquid
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.
11.2.5 In automated apparatuses, it is permissible to continue running successive determinations after the initial two
determinations up to a maximum of four, without the need to clean and dry the viscometer tube in between determinations. Choose
from any two successive determinations (i.e., 1-2, 2-3, 3-4) which meet the corresponding determinability precision statement for
the material type being measured. If two successive determinations that meet the determinability precision cannot be found for a
sample, suspend execution of this test method for that sample. See Note 6 for further guidance.
12.1 For steam-refined cylinder oils and black lubricating oils, proceed to 12.2 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 to 12.1.8 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 the sample in the original container at a temperature between 60 °C and 65 °C for 1 h.
12.1.3 Place the BS/IP/RF U-tube reverse-flow, or Zeitfuchs Cross-arm, or Lantz-Zeitfuchs type reverse-flow viscometer for the
samples to be tested in the viscometer bath(s) at the required test temperature. If the viscometers are to be charged prior to insertion
in the viscometer bath, for example, Cannon Fenske Opaque, see 12.2.1.
9
D445 − 24
12.1.4 Upon completion of step 12.1.2, vigorously stir each sample for approximately 20 s with a glass or steel rod of sufficient
length to reach the bottom of the container. For samples of a very waxy nature or oils of high kinematic viscosity, it may be
necessary to increase the heating temperature above 65 °C to achieve proper mixing. The sample should be sufficiently fluid for
ease of stirring and shaking.
12.1.5 Remove the stirring rod and inspect for sludge or wax adhering to the rod. Continue stirring until there is no sludge or wax
adhering to the rod.
12.1.6 Recap the container tightly and shake vigorously for 1 min to complete the mixing. To protect the integrity of the sample
should a repeat analysis be required, pour sufficient sample to fill two flasks and loosely stopper. (Each flask should hold sufficient
sample to fill two viscometers in order to obtain two determinations. The second flask is required to carry out a repeat analysis.)
If a repeat analysis is not a consideration the next steps can be performed using the original container, loosely capped.
12.1.7 Heat the first sample flask or sample container between 100 °C and 105 °C for 30 min.
12.1.8 Remove the first sample flask or sample container from the heat, close tightly, and shake vigorously for 60 s.
12.2 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 must be used. These two determinations are used to calculate one
result. Charge two viscometers in the manner dictated by the design of the instrument. For example, for the Lantz-Zeitfuchs
Cross-arm or the BS/IP/RF U-tube reverse-flow viscometers for opaque liquids, filter the sample through a 75 µm 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.
iTeh Standards
12.2.1 Viscometers which are charged before being inserted into the bath may need to be preheated in an oven prior to charging
(https://standards.iteh.ai)
the sample. This is to ensure that the sample will not be cooled below test temperature.
12.2.2 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 specificationsDocument
(see Specifications D446).Preview
12.2.3 Allow the charged viscometers enough time to reach the test temperature (see 12.2.1). Where one bath is used to
ASTM
accommodate several viscometers, never add or withdraw, D445-24
or clean a viscometer while any other viscometer is in use for measuring
flow time.
https://standards.iteh.ai/catalog/standards/astm/1b010020-1802-46c8-ac82-0e2024b174cd/astm-d445-24
12.3 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.
12.3.1 In the case of samples requiring heat treatment described in 12.1 through 12.1.8, complete the measurements of flow time
within 1 h of completing 12.1.8. Record the measured flow times.
12.4 Calculate kinematic viscosity, ν, in millimetres squared per second, from each measured flow time. Regard these as two
determined values of kinematic viscosity.
12.4.1 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. This constitutes one
analysis. Record the result. If a second value (repeat) is required, then repeat the analysis after thorough cleaning and drying of
the viscometers starting from sample 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, then this is not suitable for a repeat analysis. If the calculated kinematic viscosities do not 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.
NOTE 7—Poor determinability can be the result of several factors including: air bubbles trapped in the sample within the viscometer, poor temperature
stability of the constant temperature bath, particulate contamination in the viscometer, or specimen heterogeneity. Additional sample-specific issues may
be conformational changes related to time and thermal history (incomplete reaction of blended chemistries, re-alignment of polymeric chains, or
10