INTERNATIONAL ISO

STANDARD 3104

Fourth edition
2023-11

Petroleum products — Transparent

and opaque liquids — Determination
of kinematic viscosity and calculation
of dynamic viscosity
Produits pétroliers — Liquides opaques et transparents —
Détermination de la viscosité cinématique et calcul de la viscosité
dynamique

Reference number
ISO 3104:2023(E)

© ISO 2023
ISO 3104:2023(E)

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© ISO 2023
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Published in Switzerland

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 ISO 3104:2023(E)

Contents Page

Foreword......................................................................................................................................................................................................................................... iv
Introduction..................................................................................................................................................................................................................................v
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references...................................................................................................................................................................................... 1
3 Terms and definitions..................................................................................................................................................................................... 1
4 Principle......................................................................................................................................................................................................................... 2
5 Reagents and materials................................................................................................................................................................................. 2
6 Apparatus..................................................................................................................................................................................................................... 3
7 ​ erification................................................................................................................................................................................................................. 6
V
7.1 Viscometer................................................................................................................................................................................................... 6
7.2 Liquid-in-glass thermometer...................................................................................................................................................... 7
7.3 Digital contact thermometer...................................................................................................................................................... 7
7.4 Timer................................................................................................................................................................................................................ 7
8 Re-calibration.......................................................................................................................................................................................................... 7
9 Quality control........................................................................................................................................................................................................ 7
10 Sample preparation........................................................................................................................................................................................... 8
10.1 Pre-analysis sample conditioning.......................................................................................................................................... 8
10.2 Visual inspection and filtering.................................................................................................................................................. 8
11 Procedure A — Manual equipment (referee test method)....................................................................................... 8
12 Procedure B — Automated equipment...................................................................................................................................... 10
13 Cleaning of the viscometer tube........................................................................................................................................................ 11
14 Calculation................................................................................................................................................................................................................12
14.1 Procedure A — Manual viscometers................................................................................................................................ 12
14.2 Procedure B — Automated viscometers....................................................................................................................... 13
15 Expression of results.....................................................................................................................................................................................13
16 Precision..................................................................................................................................................................................................................... 13
16.1 Determinability, d.............................................................................................................................................................................. 13
16.2 Repeatability, r..................................................................................................................................................................................... 14
16.3 Reproducibility, R............................................................................................................................................................................... 14
16.4 Procedure A — Manual viscometers................................................................................................................................ 14
16.5 Procedure B — Automated viscometers....................................................................................................................... 14
17 Test report................................................................................................................................................................................................................ 15
Annex A (normative) Viscometer types, calibration and verification.......................................................................... 16
Annex B (normative) Thermometers for kinematic viscosity test................................................................................... 17
Annex C (normative) Conditioning of samples prior to manual or automated analysis........................... 21
Annex D (normative) Calculation of acceptable tolerance zone (band) to determine
conformance with a certified reference material.......................................................................................................... 22
Bibliography..............................................................................................................................................................................................................................24

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ISO 3104:2023(E)

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO document should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use
of (a) patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed
patent rights in respect thereof. As of the date of publication of this document, ISO had not received
notice of (a) patent(s) which may be required to implement this document. However, implementers are
cautioned that this may not represent the latest information, which may be obtained from the patent
database available at www.iso.org/patents. ISO shall not be held responsible for identifying any or all
such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to
the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 28, Petroleum and related products, fuels
and lubricants from natural or synthetic sources, in collaboration with the European Committee for
Standardization (CEN) Technical Committee CEN/TC 19, Gaseous and liquid fuels, lubricants and related
products of petroleum, synthetic and biological origin, in accordance with the Agreement on technical
cooperation between ISO and CEN (Vienna Agreement).
This fourth edition cancels and replaces the third edition (ISO 3104:2020), which has been technically
revised.
The main changes are as follows:
— manual Procedure A has been designated as the referee test method in case of dispute;
— the DCT requirements have been updated in Table 1;
— allowable DCT drift in 7.3 has been aligned with Table 1;
— extra instructions for quality control have been added referring to ISO 4259-4;
— complying thermometers have been updated in Table B2;
— the calculation has been corrected in Annex D.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.

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 ISO 3104:2023(E)

Introduction
Many petroleum products and some non-petroleum materials are used as lubricants. The correct
operation of 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 measurement of viscosity is essential to many product
specifications.
This document describes two test methods: Procedure A (manual) and Procedure B (automated).
Procedure A is the referee test method (or reference test method) to resolve doubts or dispute.

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INTERNATIONAL STANDARD ISO 3104:2023(E)

Petroleum products — Transparent and opaque liquids

— Determination of kinematic viscosity and calculation of
dynamic viscosity
WARNING — This document does not purport to address all of the safety problems, if any,
associated with its use. It is the responsibility of users of this document to take appropriate
measures to ensure the safety and health of personnel prior to the application of this document,
and to determine the applicability of any other restrictions.

1 Scope
This document specifies Procedure A, using manual glass viscometers, and Procedure B, using glass
capillary viscometers in an automated assembly, for the determination of the kinematic viscosity, ν, of
both transparent and opaque products. The scope includes liquid petroleum products, fatty acid methyl
ester (FAME), paraffinic diesel, hydrotreated vegetable oil (HVO), gas to liquid (GTL) and biofuel diesel
mixtures up to 50 % FAME. The kinematic viscosity is determined by measuring the time for a volume
of liquid to flow under gravity through a calibrated glass capillary viscometer. The dynamic viscosity,
η, is obtained by multiplying the measured kinematic viscosity by the density, ρ, of the liquid. The range
of kinematic viscosities covered in this test method is from 0,2 mm2/s to 300 000 mm2/s over the
temperature range –20 °C to +150 °C.
NOTE The result obtained from this document is dependent upon the behaviour of the sample and is intended
for application to liquids for which primarily the shear stress and shear rates are proportional (Newtonian flow
behaviour). If, however, the viscosity varies significantly with the rate of shear, different results can be obtained
from viscometers of different capillary diameters. The procedure and precision values for residual fuel oils,
which under some conditions exhibit non-Newtonian behaviour, have been included.

2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3105:1994, Glass capillary kinematic viscometers — Specifications and operating instructions
ISO 3696, Water for analytical laboratory use — Specification and test methods
ASTM E2877-12, Standard Guide for Digital Contact Thermometers

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://​w ww​.iso​.org/​obp
— IEC Electropedia: available at https://​w ww​.electropedia​.org/​

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3.1
kinematic viscosity
ν
resistance to flow of a fluid under gravity
Note 1 to entry: For gravity flow under a given hydrostatic head, the pressure head of a liquid is proportional to
its density, ρ. For any particular viscometer, the time of flow of a fixed volume of fluid is directly proportional to
its kinematic viscosity, ν:

ν=η/ρ

where η is the dynamic viscosity (3.2) coefficient.

3.2
dynamic viscosity
η
ratio between the applied shear stress and rate of shear of a liquid
Note 1 to entry: It is a measure of the resistance to flow or deformation of a liquid.

Note 2 to entry: The term dynamic viscosity is also used in a different context to denote a frequency-dependent
quantity in which shear stress and shear rate have a sinusoidal time dependence.

Note 3 to entry: Dynamic viscosity may also be called coefficient of dynamic viscosity or absolute viscosity.

3.3
density
ρ
mass per unit volume of a substance at a given temperature

4 Principle
The time is measured for a fixed volume of liquid to flow under gravity through the glass capillary
of a calibrated viscometer under a reproducible driving head and at a known and closely controlled
temperature. The kinematic viscosity is the product of the measured flow time and the calibration
constant of the viscometer.

5 Reagents and materials

5.1 Cleaning solution, strongly-oxidizing cleaning solution or alkaline cleaning solutions can be
used.

Alkaline cleaning solutions with a pH of greater than 10 are not recommended as they have been shown
to change the viscometer calibration. If these are used, then the viscometer calibration should be
verified to ensure there is no change.

5.2 Sample solvent, completely miscible with the sample. A prewash of an aromatic solvent such as
toluene or heptane can be necessary to remove asphaltenic material. When cleaning capillaries inside
the bath, the boiling point of the cleaning solution shall be higher than the bath temperature.

5.3 Drying solvent, suitable and volatile at the used temperature. Filter before use. If moisture
remains, use a drying solvent miscible with water (5.4).
NOTE When cleaning capillaries inside the bath and if the bath temperature is higher than 50 °C, acetone is
not suitable.

5.4 Water, deionized or distilled, conforming to Grade 3 of ISO 3696. Filter before use.

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5.5 Certified viscosity reference standards (CRM), produced by a reference material producer and
meeting the requirements of ISO 17034. They shall be characterized in accordance with a standard
practice for the basic calibration of master viscometers and characterization of viscosity oils, such as
in ASTM D2162-21. The certified values shall be traceable to the international agreed value of distilled
water (1,003 4 mm2/s at 20 °C as specified in ISO/TR 3666).

6 Apparatus

6.1 Drying tubes, consisting of a desiccant drying system of either externally mounted drying tubes
or an integrated desiccant drying system which is designed to remove ambient moisture from the
capillary tube. Ensure that they are packed loosely and that the desiccant is not saturated with water.

6.2 Sample filter, micron screen or fretted (sintered) glass filter, no more than 75 µm.

6.3 Reagent filter, micron screen or fretted (sintered) glass filter, no more than 11 µm.

6.4 Ultrasonic bath, unheated, with an operating frequency between 25 kHz to 60 kHz and a typical
power output of ≤100 W, of suitable dimensions to hold container(s) placed inside of bath, for use in
effectively dissipating and removing air or gas bubbles that can be entrained in viscous sample types
prior to analysis. It is permitted to use ultra-sonic 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 the results determined with and without the use of such ultrasonic baths do not
materially impact results.

6.5 Manual apparatus

6.5.1 Glass capillary viscometer, calibrated in accordance with ISO 3105.

The viscometer shall have a certificate of calibration provided by a laboratory that meets ISO/IEC 17025.
The calibration constant should be checked before first use of the capillary and only changed if
necessary.
The calibration constant, C, is dependent upon the gravitational acceleration at the place of calibration.
The variation in the value of g across the earth’s surface is about 0,5 % due to latitude plus approximately
0,003 % per 100 m altitude. Apply a gravity correction to the viscometer calibration constant as in
Formula (1), if the acceleration of gravity of the testing laboratory differs by more than 0,1 % of the
calibration laboratory.

g 
C2 =  2  C (1)
 g1 
where the g1 and g2 are, respectively, the calibration laboratory and the testing laboratory.
NOTE Calculation of acceleration of gravity values can be found in Reference [25].

IMPORTANT — Viscometers used for silicone fluids, fluorocarbons and other liquids, which are
difficult to remove using a cleaning agent, shall be reserved for the exclusive use of those fluids,
except during their calibration. Subject such viscometers to calibration checks at frequent
intervals. The solvent washings from these viscometers shall not be used for the cleaning of
other viscometers. If the viscometer is cleaned using the material in 5.1 then the user shall
verify the calibration before further use.

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6.5.2 Viscometer holder or mounting device within the temperature-controlled bath, enabling
the glass viscometer to be suspended so that the upper meniscus is directly above the lower meniscus
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 in accordance with ISO 3105.
The proper alignment of vertical parts may be confirmed by using a plumb line, but for rectangular
baths with opaque ends, this may not be possible.

6.5.3 Temperature-controlled bath, containing a transparent liquid of sufficient depth such that at
no time during the measurement is any portion of the sample in the viscometer less than 20 mm below
the surface of the bath liquid or less than 20 mm above the bottom of the bath.

Temperature control of the bath liquid shall be such that, for each series of flow-time measurements,
within the range of 15 °C to 100 °C, the temperature of the bath medium does not vary by more
than ±0,02 °C from the selected temperature over the length of the viscometer, and/or between the
position of each viscometer, and/or at the location of the temperature measuring device. In other words,
the temperature shall be constant at the capillary and at the position of the temperature measuring
device within a maximum difference of 0,04 °C. For temperatures outside this range, the deviation from
the desired temperature shall not exceed ±0,05 °C.
Adjust and maintain the viscometer bath at the required test temperature within the limits given
in 6.5.3, in accordance with the conditions given in Annex B and any corrections supplied on the
certificates of calibration for the temperature measuring device. Maintain the bath temperature at the
test temperature using the readings of the temperature measuring device with the corrections supplied
by the certificate of calibration.
The temperature measuring device shall be held in an upright position under the same conditions of
immersion as when calibrated.

6.5.4 Temperature-measuring device, for the range 0 °C to 100 °C, being either:

a) a calibrated liquid-in-glass thermometer, as listed in Annex B with a calibration and measurement

capability (CMC) of ±0,04 °C after correction or better, or
b) a digital contact thermometer (DCT) as described in Table 1 for this temperature with equal or
better CMC.
NOTE 1 A DCT is preferred due to the lower uncertainty of measurement.

The calibration data should be traceable to a calibration or metrology standards body and meet the
uncertainty of measurement required. The calibration certificate shall include data covering the
series of temperature test points which are appropriate for its intended use. When two temperature
measuring devices are used in the same bath in this range, they shall agree within 0,04 °C.
If calibrated liquid-in-glass thermometers are used, the use of two thermometers is recommended.
Outside the range 0 °C to 100 °C, a calibrated liquid in-glass thermometer with a CMC of ±0,1 °C or
better shall be used, and when two temperature measuring devices are used in the same bath, they
shall agree within ±0,1 °C.
When using liquid-in-glass thermometers, use a magnifying device to read the thermometer to
the nearest 1/5 division (e.g. 0,01 °C or 0,02 °C) to ensure that the required test temperature and
temperature control capabilities are met. 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.

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 ISO 3104:2023(E)

A DCT which meets the requirements in Table 1 shall be used. The DCT shall be dependent upon
temperature range in use.
NOTE 2 The resulting uncertainty of calibration can be dependent upon the immersion depth.

The DCT probe shall be immersed no less than the immersion depth stated on the calibration certificate.
NOTE 3 With respect to DCT probe immersion depth, a procedure is available in ASTM E563​-11:​2019,
Section 7,1) for determining the minimum depth. With respect to an ice bath, ASTM E563-22 provides guidance
on the preparation of an ice bath, however variance from the specific steps is permitted, provided preparation is
consistent as it is being used to track change in calibration.

The DCT probe calibration drift should be verified periodically while in use, and not less than once a
year. If the measurement of DCT calibration drift exceeds the specified limit, it shall be fully recalibrated
consistent with its range-of-use. If the drift exceeds the noted limit for calibration drift, then it shall be
reverified at a shorter time period, and not less than once per month, until this is noted as stable.
NOTE 4 The procedures contained in ASTM E563-22 and ASTM E644-11 provide guidance on the steps
required to check calibration drift.

Table 1 — DCT requirements

Criteria Minimum requirements
DCT ASTM E2877-12
Display resolution 0,01 °C, recommended 0,001 °C
Display maximum Range: −80 °C −0 °C, 0,05 °C
permissible error for
Range: 0 °C −100 °C, 0,02 °C
combined probe and
sensor Range: >100 °C, 0,05 °C
Sensor type Resistance temperature detector (RTD), such as a platinum resistance thermometer
(PRT) or thermistor
Drift less than 20 mK (0,02 °C) per year
Linearity Less than 0,01 °C over range of intended use
Calibration report The DCT shall have a report of temperature calibration which should be traceable to
a national calibration or metrology standards body issued by a calibration laboratory
with demonstrated competency in temperature calibration
Calibration data The calibration report shall include at least 3 calibration temperatures including 0 °C
and two other points including the test temperature of use and state the immersion
depth under which this was calibrated and the resulting uncertainty. The calibration
data should be distributed over the calibration range of the DCT

6.6 Automated apparatus

6.6.1 General

Automated viscometers, which use the technical principles of this document, are acceptable provided
they meet the accuracy and precision of all the equipment listed in 6.5. In addition, if they are used to
measure viscosity in samples subject to conditioning using the steps in Annex C, a heated sample tray
shall be used if the sample is not analysed immediately after conditioning. This sample tray (6.6.2) shall
be heated to a temperature which will ensure the sample will not drop below its WAT (wax appearance
temperature) or 20 °C above its pourpoint. For samples required to be analysed at 100 °C or above,
heating the sample above these temperatures can cause evaporation of light components and is not
appropriate.

1) Withdrawn.

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ISO 3104:2023(E)

Flow times of less than 200 s are acceptable, however, the kinetic energy correction shall be calculated
and should not exceed 3 % of the measured viscosity. Where a value of greater than 3 % is achieved, the
analysis should be repeated using a smaller diameter viscometer tube.
NOTE ISO 3105 describes in more detail the principles and calculation of kinematic viscosity as related to
the dimensions of the viscometer.

6.6.2 Sample trays

Some automated equipment contain sample loading trays for analysis of multiple samples. When a
sample has been subjected to conditioning using the steps in Annex C, the sample shall not be allowed
to cool below the testing temperature on the loading tray as this will result in an increase in measured
viscosity as compared to the manual procedure. The sample delivery path should be heated as the
temperature of the conditioned sample can drop very quickly. For analysis of these samples, the sample
loading trays shall be heated above the test temperature where practical, (see 6.6.1 for samples analysed
at 100 °C or above) to ensure the temperature of the sample has reached the test temperature at the
time of analysis and the nature of the sample is not changed. For analysis of these samples at 50 °C, a
sample tray heated at 54 °C has been shown to be sufficient to maintain the sample temperature above
50 °C for at least 40 min. For analysis of these samples at other temperatures, the lab should establish
the correct sample tray temperature and time before analysis.

6.6.3 Temperature measuring device

If embedded, a temperature measuring device shall fully meet the requirements of 6.5.4 and be
removable for an external calibration. The embedded device provides an independent reference
temperature read-out, allowing the temperature control of the automated apparatus to be adjusted at
the required set-point of test.

6.7 Timing device, capable of taking readings with a discrimination of 0,1 s or better, and having an
uncertainty within ±0,07 % of the reading when tested over intervals of 200 s and 1 000 s.

Regularly verify these readings and maintain records of such checks.

The time signals which are broadcast by the National Institute of Standards and Technology (NIST),
National Physical Laboratory (NPL) or other time signal stations, are a convenient and primary
standard reference for calibrating timing devices.
NOTE Many broadcast networks put out a standard frequency signal, as do many telephone networks. Such
signals are suitable for checking the timing devices used to an accuracy of 0,1 s.

Timing devices employed in automated viscometers can be an integral part of the apparatus and
typically are digital (using a precision crystal oscillator) with precision discriminations of 0,01 s
or better. As such, it is possible that the timing devices are not able to be individually verified once
installed. Documentation of the accuracy of the timing device over the intended measuring range of the
viscometer tube should therefore be provided by the manufacturer. Independent verification of timing
devices should be provided in cases where the above-mentioned limits are not satisfied.
Electrical timing devices may be used if the current frequency is controlled to an uncertainty of 0,05 %
or better. Alternating currents, as provided by some public power systems, are controlled intermittently
rather than continuously. When used to actuate electrical timing devices, such control can cause large
errors in viscosity flow measurements.

7 ​Verification

7.1 Viscometer
Verify the calibration of the viscometer using a certified viscosity reference standard (5.5) following
Procedure A (manual, Clause 11) or Procedure B (automated, Clause 12). Acceptable tolerance bands

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 ISO 3104:2023(E)

for this verification check shall be as detailed in Annex D. If the measured kinematic viscosity does
not fall within this acceptable range, recheck each step in the procedure, including thermometer and
viscometer calibrations and cleaning to locate the source of error. ISO 3105:1994, Table 1 gives details
of standards available.
Alternatively, verify working viscometers against a reference viscometer having a certificate of
calibration in accordance with ISO 3105.
Verification is required at least prior to first use of the viscometer and whenever a physical change is
made to the apparatus e.g. re-calibrating the temperature set-point, after cleaning or investigating the
failure of quality assurance (QA)/ quality control (QC) protocol in place.

7.2 Liquid-in-glass thermometer

Verify the calibration of the liquid in a glass thermometer on a periodic basis in line with B.2 at least
at the frequencies described, and maintain records of such checks. A complete new recalibration of the
thermometer, while permitted, is not necessary in order to meet the accuracy ascribed to the design of
the thermometer until the ice point change from the last full calibration amounts to one scale division,
such as 0,05 °C. Some thermometers have an ice point scale for this activity.

7.3 Digital contact thermometer

Verify the calibration of the DCT 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 or an ice bath.
ASTM standard practices given in ASTM E563-22, ASTM E1750, and ASTM E2593 may be used as
references for checking calibrations.

7.4 Timer
Verify the precision of the timer in use at regular periods and maintain records of such checks.
NOTE Many broadcast networks put out a standard frequency signal, as do many telephone networks. Such
signals are suitable for checking the timing devices to a maximum permissible error of 0,1 s.

8 Re-calibration
Glass capillary viscometer recalibration, if required, shall be undertaken using the procedures in
ISO 3105.
CAUTION — Users are cautioned that recalibrating equipment in situ when a verification fails
potentially calibrates in an error. The most common sources of error are caused by particles
of dust lodged in the capillary bore and temperature measurement errors. It should be
appreciated that a correct result obtained on standard oil does not preclude the possibility of a
counterbalancing combination of the possible sources of error.

9 Quality control
Use statistical control charts to validate “in-statistical-control” status for the execution of a standard
test method in a single laboratory. For examples, see ISO 4259‑4.
Use a quality control (QC) sample that is representative of the product(s) routinely tested by the
laboratory to confirm that the instrument is in statistical control.
This may not be possible if the product under test cannot be used as a QC material due to its nature
(unstable or subject to thermal treatment).

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ISO 3104:2023(E)

Where the testing facility lab uses a CRM material as a measure of quality control, Annex D shall be
used as the procedure to construct suitable acceptable tolerance zones for the QC/QA system.

10 Sample preparation

10.1 Pre-analysis sample conditioning

10.1.1 Using Table 2, verify whether the sample type under analysis requires conditioning before
analysis and, if so, follow the relevant procedure and steps noted, before charging the viscometer.

10.1.2 If the sample is transparent, but not liquid at room temperature, for example samples with a
high pour point value, then the sample shall be sufficiently heated to ensure it can flow freely before
charging the viscometer.

10.2 Visual inspection and filtering

When the sample is liquid, visually inspect it. If the sample contains fibres or solid particles, use a
sample filter (6.2) prior to or during charging of the viscometer tube. At all stages, protect the sample
from contamination.

Table 2 — Sample types and conditioning procedures

Sample type Is sample conditioning Is sample filter Conditioning procedure
required before required? reference
analysis?
Base oils No Noa Not required
Gas oils No Noa Not required
Distillate No Noa Not required
Kerosene No Noa Not required
Jet fuel No Noa Not required
Formulated oils No Noa 10.1.2
Lubricant additives No Noa 10.1.2
Biofuel blend No Noa 10.1.2
Biodiesel B100 (transparent) No Noa 10.1.2
Petroleum wax (transparent) No Noa 10.1.2
Biodiesel B100 (opaque) Yes Yes Annex C
Petroleum wax (opaque) Yes Yes Annex C
Residual fuel oils Yes Yes Annex C
Steam-refined cylinder oils Yes Yes Annex C
Black lubricating oils Yes Yes Annex C
Used oils No Yes Not required
a Unless it contains fibres, solid particles or is not transparent.

11 Procedure A — Manual equipment (referee test method)

11.1 Procedure A is the referee test method (or reference test method) to resolve doubts or dispute.

Check the bath temperature using the temperature measuring device, ensuring that the set point is
within the acceptable tolerance and accuracy of the test temperature, and record this data.

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With certain products which exhibit “gel-like” behaviour, users should take care that measurements
are made at temperatures sufficiently high for such materials to flow freely, so that similar kinematic
viscosity results are obtained in viscometers of different capillary diameter.

11.2 Select suitable clean, dry calibrated viscometer(s) having a range covering the estimated
kinematic viscosity at the specified test temperature. The flow time shall not be less than 200 s, or less
than the minimum flow time for viscometer types and/or sizes specified in Annex A, and the maximum
flow time stated in ISO 3105.

The specific details of operation vary depending on the type of viscometer. The operating instructions
for the different types of viscometers listed in Table A.1 are given in ISO 3105. In general, the viscometers
used for opaque liquids are of the reverse-flow type listed in Table A.1 (type C).
For the measurement of kinematic viscosity of jet fuels at −20 °C, only suspended-level type ISO 3105
viscometers as noted in Table A.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.

11.3 Charge the viscometer with the sample in accordance with the operating instructions in ISO 3105
for the particular type of viscometer, as described in Annex A. Then place in the bath in the manner
dictated by the design of the instrument. This operation shall be in conformity with that employed
when the instrument was calibrated.

Allow the charged viscometer to remain in the bath long enough to reach the test temperature, and to
ensure that all air bubbles in the sample have dispersed. As the equilibration time in the bath varies for
different products, different viscometer tubes, for different temperatures and for different kinematic
viscosities, establish and document a safe equilibrium time by trial. A minimum of 30 min is required
for jet fuel at −20 °C.
Where the design of the viscometer requires it, adjust the volume of the sample to the mark after the
sample has reached temperature equilibrium.
NOTE Some viscometers require charging outside of the bath due to their design.

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. However, it is essential that they do not set up a pressure differential and
affect the rate of flow. Before 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.
Special conditions apply when the test temperature is below the dew point, such as for analysis at
−20 °C. To ensure moisture does not condense or freeze on the walls of the capillary, it is recommended
to charge the viscometer outside the bath and if used affix loosely packed drying tubes to the open
ends of the viscometer. The drying tubes shall fit the design of the viscometer and not restrict the flow
of the sample by changing the pressure in the instrument. Carefully flush the moist room air from the
viscometer by applying vacuum to one of the drying tubes.
Finally, it is recommended before placing the viscometer in the bath to draw up the sample into the
working capillary and timing bulb and allow to drain back, as an additional safeguard against moisture
condensing or freezing on the walls.
Do not use viscometers which cannot be removed from the constant temperature bath for charging the
sample portion.
Where one bath is used to accommodate several viscometers, never add or withdraw a viscometer
while any other viscometer is being used to measure flow time.
For samples which have been subjected to conditioning as described in Annex C, ensure that the
determinations are started within 1 h of completing this pre-treatment.

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ISO 3104:2023(E)

11.4 Perform the determinability test.

11.4.1 Use suction (if the sample contains no volatile constituents) or pressure to position the sample
level in accordance with the operating instructions as set out in ISO 3105 for the type of viscometer
in use. 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, select a viscometer with a capillary of smaller diameter and repeat the operation.

11.4.2 On all fluids except those subject to conditioning in Annex C, repeat the procedure. For direct
flow viscometers described in 11.4.1, without recharging the viscometer make a second measurement
of flow time. In the case of a reverse flow viscometer, either charge two viscometer tubes, or carry out a
complete cleaning and drying of a single tube before re-charging and performing a second measurement
of flow time.

11.4.3 Repeat 11.3 and 11.4.1. Record both flow time measurements. The intent is that the same sample
of fluid is measured in the same timing bulb successively. In the case of a reverse flow viscometer with
two bulbs, only the lower bulb shall be used for flow time measurement.

On fluids subject to conditioning in Annex C, charge two viscometer tubes and follow the procedure
described in 11.4.1. Record both measurements.
From the two measurements of flow time, calculate two determined values of kinematic viscosity as
shown in 14.1.1.
If the two measurements agree with the stated determinability figure for the product, calculate the
average of the two determinations and use this value to report the kinematic viscosity. Record the
result.

11.4.4 If two successive measurements do not meet the determinability figure for the product, repeat
the above operation from 7.1.

Poor determinability can be attributed to: an unsuccessfully filtered sample, ice forming in the capillary,
a contaminated viscometer or sample, unstable temperature conditions, insufficient equilibrium time,
heterogeneity of sample or that the viscometer may require cleaning. Consider these points before
starting a new analysis.
If the material or temperature (or both) is not listed in Clause 16 then use 0,01 y for temperatures
between 15 °C and 100 °C and for temperatures outside this range use 0,015 y as an estimate of
determinability, where y is the average of the determinations being compared. In addition, the user
can establish a reasonable determinability by trial. Document and use this “trial” determinability value
against which to judge if determinability has been met in subsequent analysis.

12 Procedure B — Automated equipment

12.1 Set up the automated viscometer in accordance with the manufacturer’s instructions for use and
verify that the equipment is fit for use by applying suitable quality control measures.

12.2 Check the bath temperature using the temperature measuring device, ensuring that the set point
is within the acceptable accuracy and tolerance of the test temperature. Do not start the test if the
measurement is outside the tolerance.

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 ISO 3104:2023(E)

12.3 Perform the determinability test.

12.3.1 Charge the viscometer, on completion of the equilibrium time, ensure that the sample is drawn
up the capillary to a position in the capillary tube above the timing bulb.

The sample may also be drawn up once and released without timing to “wet” the tube if required.
For sub-zero temperature measurements, the sample shall be held in the viscometer tube during the
temperature equilibrium period. The time required is dependent upon the sample type, viscometer tube
and temperature of analysis, and should be determined individually for each automated equipment.
For analysis of jet fuel at −20 °C, the automated viscometer shall maintain the sample in position for a
minimum of 20 min for the temperature to equilibrate.

12.3.2 Allow the sample to flow freely and measure in seconds, to a resolution of at least 0,01 s, the time
required for the bottom of the meniscus to pass from one timing position to the next timing position.

Flow times of less than 200 s are permitted as long as the kinetic energy correction is calculated and
does not exceed 3 % of the measured viscosity. If the kinetic energy correction exceeds 3 %, select a
viscometer with a smaller diameter capillary and repeat the test.

12.3.3 On all fluids except those subject to conditioning in Annex C, repeat the procedure described
in 12.3.1 to 12.3.2, without recharging the viscometer, to make a second measurement of flow time.
The equilibrium time in this case is not required. Record the flow time measurements, kinetic energy
correction and the bath temperature readings at the beginning of each flow time measurement.

12.3.4 On fluids subject to conditioning in Annex C, two viscometer tubes can be charged and follow
the procedure described in 12.3.1 to 12.3.3, or all measurements can be undertaken in one viscometer
tube if the sample is sufficiently fluid, and the sample is not allowed to cool below the test temperature.
Record the flow time measurements, kinetic energy correction and the bath temperature readings at
the beginning of each flow time measurement. These may be automatically captured by the equipment
or manually by the analyst.

12.3.5 Repeat the procedure described in 12.3.1 to 12.3.2 until two successive determinations agree
within the required determinability given in this document. If the two determinations agree with the
stated determinability figure for the product, calculate the average of the two measurements and use
this value to report the kinematic viscosity. Record the result.

12.3.6 If two successive determinations do not meet the determinability figure for the product, repeat
the above operation from 12.3.1.

If the material or temperature or both is not listed in Clause 16 then use 0,01 y for temperatures between
15 °C and 100 °C and for temperatures outside this range use 0,015 y as an estimate of determinability
(where y is is the average of the determinations being compared). In addition, the user can establish a
reasonable determinability by trial. Document and use this “trial” determinability value against which
to judge if determinability has been met in subsequent analysis.

13 Cleaning of the viscometer tube

13.1 After each analysis, clean the viscometer thoroughly by several rinses with the sample solvent
(5.2), followed by the drying solvent (5.3). Dry the tube by passing a slow stream of filtered dry air
through the viscometer for 2 min or until the last trace of solvent is removed.

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ISO 3104:2023(E)

13.2 When the verification of the viscometer calibration using certified reference material is
outside of the acceptable tolerance band, the viscometer should be cleaned using the manufacturer's
recommended cleaning solution and methodology to remove organic deposits.

Sometimes insoluble particles can be removed by use of an ultrasonic bath. Inorganic deposits may be
removed using acid treatment before the use of cleaning solution, particularly if the presence of barium
salts is suspected. Following the removal of inorganic deposits, clean with the cleaning solution (5.1) to
remove residual traces of organic deposits, rinse thoroughly with water (5.4) and drying solvent (5.3),
and dry with filtered dry air or a vacuum line as required by the manufacturer of the equipment.

14 Calculation

14.1 Procedure A — Manual viscometers

14.1.1 Calculate the determinability value, d, from two measured flow times, t1 and t 2, and the
viscometer constant, C, by means of Formulae (2) and (3):

ν1 = C × t 1 (2)

ν2 = C × t 2 (3)

where

ν1 is the kinematic viscosity, in millimetres squared per second for the first flow time;

ν2 is the kinematic viscosity, in millimetres squared per second for the second flow time;

C is the calibration constant of the viscometer, in millimetres squared per second squared;

t1 is the measured flow time, in seconds of the first analysis;

t2 is the measured flow time, in seconds of the second analysis.

Calculate the difference between ν1 and ν2 and compare to the determinability value stated in Table 3.
If the difference between ν1 and ν2 is less than the determinability value stated in Table 3, calculate the
final reported kinematic viscosity result v as an average ν1 and ν2 as given by Formula (4):
ν = (ν1 + ν2)/2 (4)

where ν is the kinematic viscosity, in millimetres squared per second of the final reported result.

14.1.2 If required, calculate the dynamic viscosity, η, from the calculated kinematic viscosity, ν, and
the density, ρ, by means of Formula (5):

η = ν × ρ × 10−3 (5)

where

η is the dynamic viscosity, in millipascal seconds;

ρ is the density, in kilograms per cubic metre, at the same temperature used for the determination
of the kinematic viscosity.
The density of the sample may be determined by an appropriate method such as ISO 12185 .or ISO 3675
and corrected to the temperature of determination by means of ISO 91:2017.

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 ISO 3104:2023(E)

14.2 Procedure B — Automated viscometers

14.2.1 The equipment should calculate the determinability values as described in 14.1.1. The
determinability values should be recorded and available for reference. If the difference between ν1 and
ν2 is less than the determinability value stated in Table 4, the equipment should calculate the kinematic
viscosity value for the sample. If it is greater than the value stated in Table 4, then the equipment should
indicate that the result should not be reported.

14.2.2 Calculate the kinematic viscosity, v, from the average of the measured flow time, t, and the
viscometer constant, C, taking into account the kinetic energy factor E, by means of Formula (6):

ν = C × t - (E / t 2) (6)

where

ν is the kinematic viscosity, in millimetres squared per second;

C is the calibration constant of the viscometer, in square millimetres per second squared;

t is the mean flow time, in seconds;

E is the kinetic energy factor, in square millimetre seconds.

Although the kinetic energy factor, E, is not a constant, it can be approximated by means of Formula (7):
3
52 , 5V 2
E= (7)
1
L (C × d ) 2
where

V is the volume of the timing bulb, in millilitres;

L capillary working length, in millimetres;

d capillary diameter, in millimetres;

C is the calibration constant of the viscometer, in square millimetres per second squared.

15 Expression of results
Report the test results for kinematic viscosity or dynamic viscosity, or both, to four significant figures,
together with test temperature.

16 Precision

16.1 Determinability, d
The difference between successive determinations obtained by the same operator in the same
laboratory using the same apparatus for a series of operations leading to a single result, in the normal
and correct operation of this test method, would exceed in the long run the values indicated in Table 3
with an approximate probability of 5 % due to random variation.

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ISO 3104:2023(E)

16.2 Repeatability, r
The difference between two independent results obtained using this method for test material
considered to be the same in the same laboratory, by the same operator using the same equipment
within short intervals of time, in the normal and correct operation of the method, would exceeed the
values calculated in Table 3 with an approximate probability of 5 % due to random variation.

16.3 Reproducibility, R
The difference between two independent results obtained using this method for test material
considered to be the same in different laboratories, where different laboratory means a different
operator, different equipment, different geographic location, and under different supervisory control,
in the normal and correct operation of the method, would exceed the values calculated in Table 3 with
an approximate probability of 5 % due to random variation.

16.4 Procedure A — Manual viscometers

Precision estimates are summarized in Table 3.

16.5 Procedure B — Automated viscometers

Precision estimates are summarized in Table 4.

Table 3 — Precision estimations Procedure A

Type of product Determinability Repeatability Reproducibility
d r R
mm2/s mm2/s mm2/s
Base oils at 40 °C [15] 0,003 7 y 0,010 1 X 0,013 6 X
Base oils at 100 °C [15] 0,003 6 y 0,008 5 X 0,019 0 X
Formulated oils at 40 °C [15] 0,003 7 y 0,007 4 X 0,012 2 X
Formulated oils at 100 °C [15] 0,003 6 y 0,008 4 X 0,013 8 X
Formulated oils at 150 °C [16] 0,015 y 0,005 6 X 0,018 X
Petroleum wax at 100 °C [17] 0,008 0 y 0,014 1 X1,2 0,036 6 X1,2
Residual fuel oils at 100 °C [18] 0,03 y 0,080 88 X 0,120 6 X
Residual fuel oils at 50 °C [18] 0,024 4 y 0,078 85 X 0,084 61 X
Lubricant additives at 100 °C [19] 0,001 06 y1,1 0,001 92 X1,1 0,008 62 X1,1
Gas oils at 40 °C [20] 0,001 3 ( y + 1) 0,004 3 (X + 1) 0,008 2 (X+1)
Jet fuel at −20 °C [21] 0,007 608 0,001 368 X1,4 0,002 899 X1,4
Marine fuels, diesel, biofuel and 0,008 093 0,004 094 (x + 1,5) 0,006 133 (x + 1,5)
biofuel blends at 40 °C [22]
Key
y   average of determinations being compared
X   average of results being compared
NOTE 1 The precision values refer to kinematic viscosity only, not dynamic viscosity.
NOTE 2 See references [15] to [22] for further details on how the precision values were obtained.
NOTE 3 The precision values for used (in-service) formulated oils at 40 °C and 100 °C using Procedure A has not been
determined as most laboratories use automated equipment.

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 ISO 3104:2023(E)

Table 4 — Precision estimations Procedure B

Type of product Determinability Repeatability Reproducibility
d r R
mm2/s mm2/s mm2/s
Used (in-service) formulated a 0,000 233 X1,722 0,000 594 X1,722
oils at 40 °C [23]
Used (in-service) formulated a 0,001 005 X1,463 3 0,003 361 X1,463 3
oils at 100 °C [23]
Marine fuels, diesel, biofuel 0,004 667 0,010 07 0,020 92
and biofuel blends at 40 °C [22]
Key
X    average of results being compared
NOTE 1 The precision values refer to kinematic viscosity only, not dynamic viscosity.
NOTE 2 The precision values for automated viscometers has been determined for base oils at 40 °C and 100 °C and
formulated oils at 40 °C and 100 °C. These were shown to be no worse than the precision for manual instruments, and the
results between manual and automated instruments were considered practically equivalent for these sample types[23].
NOTE 3 See references [22] and [23] for further details on how the precision values were obtained.
a The determinability for used (in-service) formulated oils has not been determined, however a limit of 0,01 y where y is
the average of the determinations being compared for temperatures between 15 °C and 100 °C may be used. Alternatively,
users may reference DIN 51659-1 as a guide.

17 Test report
The test report shall contain at least the following information:
a) sufficient details for complete identification of the product tested;
b) a reference to this document, i.e. ISO 3104:2023;
c) the procedure used i.e. Procedure A (as specified in Clause 11) or Procedure B (as specified in
Clause 12);
d) the result of the test (see Clause 15);
e) any deviation, by agreement or otherwise, from the procedure specified;
f) any unusual features observed;
g) the date of the test;
h) the name and address of the test laboratory (if relevant to the customer).

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ISO 3104:2023(E)

Annex A
(normative)

Viscometer types, calibration and verification

Table A.1 lists capillary viscometers commonly in use for viscosity determinations on petroleum
products. For specifications and operating instructions, see ISO 3105.

Table A.1 — Viscometer types

Type Viscometer identification Kinematic viscosity rangea
mm2/s
Ostwald types for transparent liquids
0,5 to 20 000
Cannon-Fenske routineb
Zeitfuchs 0,6 to 3 000
BS/U-tubeb 0,9 to 10 000
A
BS/U/M miniature 0,2 to 100
SILb 0,6 to 10 000
Cannon-Manning semi-micro 0,4 to 20 000
Pinkevitchb 0,6 to 17 000
Suspended-level types for transparent liquids
3,5 to 100 000
BS/IP/SLb
BS/IP/SL (S)b 1,05 to 10 000
BS/IP/MSL 0,6 to 3 000
Ubbelohdeb 0,3 to 100 000
B
FitzSimons 0,6 to 1 200
Atlanticb 0,75 to 5 000
Cannon-Ubbelohde (A), Cannon-Ubbelohde dilution (B)b 0,5 to 100 000
Cannon-Ubbelohde semi-micro 0,4 to 20 000
DIN Ubbelohde 0,35 to 50 000
Reverse-flow types for transparent and opaque liquids
0,4 to 20 000
Cannon-Fenske opaque
C 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 for a kinetic energy correction, these
viscometers are designed for a flow time in excess of 200 s, except where noted in ISO 3105.
b In this series, the minimum flow time for the viscometers with lowest constants exceeds 200 s.

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 ISO 3104:2023(E)

Annex B
(normative)

Thermometers for kinematic viscosity test

B.1 Thermometer designs and specifications

Use a short-range specialized thermometer conforming to the generic specification given in Table B.1
and to one of the designs shown in Figure B.1 a) to c). Table B.2 gives a range of ASTM, IP and ASTM/
IP thermometers that comply with the specification in Table B.1, together with their designated test
temperatures. As an alternative, use a DCT as defined in 6.5.4.

a) Design 1

b) Design 2

c) Design 3
Key
B total length C stem outside diameter
D bulb length E bulb outside diameter
G length of scale range

NOTE The difference in the designs rests mainly in the position of the ice point scale. In design 1, the ice
point is within the scale range, in design 2, the ice point is below the scale range and in design 3, the ice point is
above the scale range.

Figure B.1 — Thermometer designs

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ISO 3104:2023(E)

Table B.1 — General specification for thermometers

Immersion depth Unit 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 0,1
Scale error at test temperature, max. °C 0,1
Expansion chamber to permit heating to °C 105 for thermometer scale up to 90,
120 between 90 and 95,
130 between 95 and 105,
170 above 105
Total length, B mm 300 to 310
Stem outside diameter, C mm 6,0 to 8,0
Bulb length, D mm 45 to 55
Bulb outside diameter, E mm no greater than stem
Length of scale range, G mm 40 to 90

Table B.2 — Examples of complying thermometers

Thermometer number Test temperature °C
ASTM 132C/IP 102C 150
ASTM 110C/IP 93C 135
ASTM 121C/IP 32C 98,9 and 100
ASTM 129C/IP 36C 93,3
ASTM 48C/IP 90C 82,2
IP 100C 80
ASTM 47C/IP 35C 60
ASTM 29C/IP 34C 54,4
ASTM 46C/IP 66C 50
ASTM 120C/IP 92C 40
ASTM 28C/IP 31C 37,8
ASTM 118C 30
ASTM 45C/IP 30C 25
ASTM 44C/IP 29C 20
ASTM 128C/IP 33C 0
ASTM 72C/IP 67C −17,8
ASTM 127C/IP 99C −20
ASTM 126C/IP 71C −26,1
ASTM 73C/IP 68C −40
ASTM 74C/IP 69C −53,9

B.2 Thermometer calibration and verification

B.2.1 Report of temperature calibration
When using a liquid-in-glass thermometer, it shall have a report of temperature calibration traceable to
a national calibration or metrology standards body, issued by a competent calibration laboratory with

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 ISO 3104:2023(E)

demonstrated competency in temperature calibration. The calibration report shall include data for a
series of temperatures which are appropriate for its intended use.

B.2.2 Ice point verifications

The scale correction of liquid-in-glass thermometers can change during storage and use. Therefore,
regular in-house ice point verifications are required, and can be achieved within the working laboratory,
using an ice melting bath. However, these checks may not be an adequate means of recalibration as
the use of a single-point recalibration at the ice point adds an additional uncertainty to the updated
thermometer calibration result at every temperature except for the ice point. The user shall determine
if the thermometer requires complete re-calibration to continue to meet the expanded measurement
uncertainty requirements of this clause.
NOTE NIST Special Publication 1 088, 2009, Section 7.9[14] on determining the uncertainty of correction can
be helpful to the user in making this decision. If in-house ice point verification brings the expanded measurement
uncertainty out of the requirements of B.2.1, a complete recalibration at a laboratory meeting the requirements
of B.2.1 is required.

B.2.3 Liquid-in-glass thermometer checks

For liquid-in-glass thermometers, the interval for ice-point verification shall be no longer than six
months. For new thermometers, monthly checking for the first six months is recommended. A change
of one or more scale divisions in the ice point means that the thermometer may have been overheated
or damaged, and it may be out of calibration. Such thermometers shall be removed from service until
inspected, or recalibrated, or both.

B.2.4 Records of calibration

Keep records of all recalibrations.

B.2.5 Procedure for ice-point verification of liquid-in-glass thermometers

B.2.5.1 Unless otherwise listed on the certificate of calibration, the recalibration of calibrated
kinematic viscosity thermometers requires that the ice-point reading shall be taken within 60 min
after being at test temperature for not less than 3 min.
NOTE NIST Special Publication 1 088 from the NIST website[14] describes an effective procedure for ice
point verification, including all formulae necessary for calculations of change of correction and measurement
uncertainty.

B.2.5.2 Select clear pieces of ice, preferably made from distilled or pure water. Discard any cloudy
or unsound portions. Rinse the ice with distilled water and shave or crush into small pieces, avoiding
direct contact with the hands or any chemically unclean objects. Fill the Dewar vessel with the crushed
ice and add sufficient water to form slush, but not enough to float the ice. As the ice melts, drain off
some of the water and add more crushed ice. Insert the thermometer, and pack the ice gently about the
stem, to a depth approximately one scale division below the 0 °C graduation.

B.2.5.3 After at least 3 min have elapsed, tap the thermometer gently and repeatedly at right angles
to its axis while making observations. Successive readings taken at least 1 min apart shall agree within
0,005 °C. Record the ice-point readings and determine the thermometer correction at this temperature
from the mean reading. If the correction is found to be higher or lower than that corresponding to a
previous calibration, change the correction at all other temperatures by the same value. During the
procedure, apply the following conditions.

a) The thermometer shall be supported vertically.

b) View the thermometer with an optical aid that gives a magnification of approximately five and also
eliminates parallax.

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ISO 3104:2023(E)

c) Express the ice-point reading to the nearest 0,01 °C.

B.2.5.4 When in use, immerse the thermometric device to the same depth as when it was fully
calibrated. For example, if a liquid-in-glass thermometer was calibrated at the normal total immersion
condition, it shall be immersed to the top of the mercury column with the remainder of the stem and the
expansion volume at the uppermost end exposed to room temperature and pressure. In practice, this
means that the top of the mercury column shall be within a length equivalent to four scale divisions of
the surface of the medium whose temperature is being measured. If this condition cannot be met, then
an extra correction may be necessary.

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 ISO 3104:2023(E)

Annex C
(normative)

Conditioning of samples prior to manual or automated analysis

C.1 For steam-refined cylinder oils, black lubricating oils, residual fuel oils and similar opaque waxy
products as noted in Table 2, whose kinematic viscosity can be affected by their thermal history, the
procedure described in this annex shall be followed to minimize this effect.
NOTE Black lubricating oils is not synonymous with used oils. Used oils are not required to follow this
procedure.

C.2 Heat the sample in its original container, in an oven, between 60 °C to 65 °C for 1 h.

Thoroughly stir the sample with a suitable rod of sufficient length to reach the bottom of the container.
Continue stirring until there is no sludge or wax adhering to the rod. Recap the container tightly
and shake vigorously for 1 min to complete the mixing. It can be necessary to increase the heating
temperature above 60 °C to achieve proper mixing. The sample should be sufficiently fluid after heating
for ease of stirring and shaking.

C.3 Immediately thereafter, pour sufficient sample to fill two viscometer tubes into a 100 ml glass
flask and loosely stopper the flask. Immerse the flask in a heated liquid bath or other equipment which
will maintain the sample at 100 °C for 30 min.

CAUTION — Take care as vigorous boil-over may occur when opaque liquids which contain high
levels of water are heated to high temperatures.
Remove the flask from the bath (or other equipment), stopper tightly and shake for 1 min.
The following two determinations of the kinematic viscosity of the test material are required.
a) For those viscometers that require a complete cleaning after each flow time measurement, two
viscometers may be used. A single viscometer (as shown in Table A.1) can be used if an immediate,
repeat flow time measurement can be made without cleaning and not adversely affect the
determinability value.
NOTE Reverse flow viscometers as per Table A.1 cannot be used for an immediate repeat flow time
measurement without cleaning unless a second viscometer tube is used.

b) Viscometer types which require charging prior to being inserted into the bath may require
preheating to ensure that the sample does not cool below the test temperature as this adversely
affects the accuracy of the final result.

C.4 Filter the sample either prior to or during the charge of the viscometer. Use a preheated sample
filter to prevent the sample coagulating during the filtration. For example, for the cross-arm or the BS
U-tube viscometers for opaque liquids, filter the sample through a sample filter into two viscometers
previously placed in the bath.

Charge the viscometer(s) and place in the temperature-controlled bath in the manner dictated by the
design of the instrument.

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ISO 3104:2023(E)

Annex D
(normative)

Calculation of acceptable tolerance zone (band) to determine

conformance with a certified reference material

D.1 Determine the standard deviation for site uncertainty, σsite, from a laboratory quality control
programme. If the standard deviation for the laboratory site uncertainty is not known, use the value
0,19 %.

D.2 The certified reference material (CRM) will have an accepted reference value (ARV) stated on the
suppliers certificate or documentation. Also stated will be a value for combined extended uncertainty
(U) with a coverage factor of k.
NOTE Combined extended uncertainty (CEU ) is equivalent to the expanded uncertainty (U) and the terms
are used interchangeably.

D.2.1 Calculate the standard error of the accepted reference value (SE,ARV ) of the CRM by dividing the
expanded uncertainty U by the factor k (if k is not known use the value 2), see Formula (D.1).

U
S E,ARV = (D.1)
k
NOTE Standard error of the accepted reference value (SE,ARV ) is equivalent to combined standard uncertainty
(UC) and the terms are used interchangeably.

D.2.2 Construct the acceptable tolerance zone, ZT, for the CRM, see Formula (D.2).

Z T = ±1,44 σ site
2
+ S E,ARV 2 (D.2)

D.3 The following is a worked out example for kinematic viscosity acceptable tolerance zone (band):

σsite = 0,19 % (default value)

ARV = 4,161 (from the CRM label or documentation)
Expanded uncertainty (U) = 0,16 % (from the CRM label or documentation)
Coverage factor k = 2 (from the CRM label or documentation)
0 ,16
S E,ARV = = 0 , 08
2

         Z T = ±1,44 0,192 +0,082

         ZT = ±1, 44 0,036 1 + 0,006 4

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 ISO 3104:2023(E)

          ZT = ±0,297 %

In this example, the tolerance zone ZT will be ±0,297 % of the certified viscosity reference standard
value on the report of test or bottle label. If this site uses a CRM (for example) with a kinematic viscosity
4,161 mm2/s, the ZT equals 4,149 mm2/s to 4,173 mm2/s, with 95 % certainty. Viscosity measurements
made with this CRM at that site should fall within that tolerance zone (band) 19 out of 20 times.

© ISO 2023 – All rights reserved  23


ISO 3104:2023(E)

Bibliography

[1] ISO 91:2017, Petroleum and related products — Temperature and pressure volume correction
factors (petroleum measurement tables) and standard reference conditions
[2] ISO/TR 3666, Viscosity of water
[3] ISO 3675, Crude petroleum and liquid petroleum products — Laboratory determination of density
— Hydrometer method
[4] ISO 12185, Crude petroleum and petroleum products — Determination of density — Oscillating
U-tube method
[5] ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
[6] ISO 17034, General requirements for the competence of reference material producers
[7] DIN 51659-1, Lubricants — Test methods — Part 1: Determination of the kinematic viscosity of
used lubricating oils by glass capillary viscometer
[8] ASTM D2162-21, Standard Practice for Basic Calibration of Master Viscometers and Viscosity Oil
Standards
[9] ASTM E563-22, Standard Practice for Preparation and Use of an Ice-Point Bath as a Reference
Temperature
[10] ASTM E563​-11:​20192), Standard Practice for Preparation and Use of an Ice-Point Bath as a
Reference Temperature
[11] ASTM E644-11: 2019, Standard Test Methods for Testing Industrial Resistance Thermometers
[12] ASTM E1750-10, Standard Guide for Use of Water Triple Point Cells
[13] ASTM E2593-17, Standard Guide for Accuracy Verification of Industrial Platinum Resistance
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[14] NIST Special Publication 1088, Maintenance, Validation, and Recalibration of Liquid-in-
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Standards and Technology, USA
[15] Interlaboratory Research Report RR:​D02​-1788 using baseoils and formulated oils.
ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA, 19428-2959,
USA
[16] Interlaboratory Research Report RR:​D02​-1333 using fully formulated engine oils.
ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA, 19428-2959,
USA
[17] Interlaboratory Research Report RR:​D02​-1334 using petroleum wax. ASTM International, 100
Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA, 19428-2959, USA.
[18] Interlaboratory Research Report RR:​D02​-1837 using residual fuel oil conforming to
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[19] Interlaboratory Research Report RR:​D02​-1421 using lubricant additives with viscosities greater
than 145 Cst. ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken,
PA, 19428-2959, USA

2) Withdawn.

24  © ISO 2023 – All rights reserved


 ISO 3104:2023(E)

[20] Interlaboratory Research Report ILS1996_71_1 using non automotive (red) diesel (Gasoil).
Energy Institute, 61 New Cavendish St., London W1G 7AR, United Kingdom
[21] Interlaboratory Research Report ILS2017_71_1_3 using commercial jet fuel, semi synthetic and
TS1 fuels. Energy Institute, 61 New Cavendish St., London W1G 7AR, United Kingdom.
[22] Interlaboratory Research Report ILS2019_71_1_1 using fuels designed to meet ISO 8217:2020
and EN 590. Energy Institute, 61 New Cavendish St., London W1G 7AR, United Kingdom.
[23] Interlaboratory Research Report RR:​D02​-1852 using turbine and engine formulated used oils.
ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA, 19428-2959,
USA
[24] Interlaboratory Research Report RR:​D02​-1820 Study of manual and automated precision using
baseoils, formulated oils, diesel and biofuel blends. ASTM International, 100 Barr Harbor Drive,
P.O. Box C700, West Conshohocken, PA, 19428-2959, USA
[25] www​.isobudgets​.com - how to calculate your local gravity https://​w ww​.isobudgets​.com/​how​
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Part 4: Use of statistical control charts to validate 'in-statistical-control' status for the execution of
a standard test method in a single laboratory
[27] ISO 8217:2017, Petroleum products — Fuels (class F) — Specifications of marine fuels

© ISO 2023 – All rights reserved  25


ISO 3104:2023(E)

ICS 75.080
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