ISO 2719:2016
(Main)Determination of flash point — Pensky-Martens closed cup method
Determination of flash point — Pensky-Martens closed cup method
ISO 2719:2016 describes three procedures, A, B and C, using the Pensky-Martens closed cup tester, for determining the flash point of combustible liquids, liquids with suspended solids, liquids that tend to form a surface film under the test conditions, biodiesel and other liquids in the temperature range of 40 °C to 370 °C. CAUTION - For certain mixtures no flash point, as defined, is observed; instead a significant enlargement of the test flame (not halo effect) and a change in colour of the test flame from blue to yellowish-orange can occur. Continued heating can result in significant burning of vapours outside the test cup, and can be a potential fire hazard. NOTE 1 Although, technically, kerosene with a flash point above 40 °C can be tested using this International Standard, it is standard practice to test kerosene according to ISO 13736.[5] Similarly, lubricating oils are normally tested according to ISO 2592[2]. Procedure A is applicable to distillate fuels (diesel, biodiesel blends, heating oil and turbine fuels), new and in-use lubricating oils, paints and varnishes, and other homogeneous liquids not included in the scope of Procedures B or C. Procedure B is applicable to residual fuel oils, cutback residua, used lubricating oils, mixtures of liquids with solids, liquids that tend to form a surface film under test conditions or are of such kinematic viscosity that they are not uniformly heated under the stirring and heating conditions of Procedure A. Procedure C is applicable to fatty acid methyl esters (FAME) as specified in specifications such as EN 14214[11] or ASTM D6751[13]. ISO 2719:2016 is not applicable to water-borne paints and varnishes. NOTE 2 Water-borne paints and varnishes can be tested using ISO 3679[3]. Liquids containing traces of highly volatile materials can be tested using ISO 1523[1] or ISO 3679.
Détermination du point d'éclair — Méthode Pensky-Martens en vase clos
ISO 2719:2016 décrit trois méthodes, A, B, et C, pour la détermination du point d'éclair des liquides combustibles, des liquides contenant des matières solides en suspension, des liquides ayant tendance à former un film en surface dans les conditions d'essai, des biocarburants et d'autres liquides, au moyen de l'appareil d'essai Pensky-Martens en vase clos, dans la plage de température entre 40 °C et 370 °C. ATTENTION ? Pour certains mélanges, aucun point d'éclair, tel que défini, n'est observé; à la place, il peut y avoir un élargissement significatif de la flamme d'essai (pas de phénomène de halo) et un changement de couleur de la flamme passant du bleu à l'orange jaunâtre. Le maintien du chauffage peut faire qu'une quantité significative de vapeurs soit brûlée à l'extérieur du vase d'essai, ce qui peut constituer un danger d'incendie. NOTE 1 Techniquement les kérosènes ayant un point d'éclair supérieur à 40 °C peuvent être soumis à essai selon la présente Norme internationale. Cependant, il est d'usage courant de déterminer le point d'éclair des kérosènes selon l'ISO 13736[5]. De façon analogue, les huiles lubrifiantes sont normalement soumises à essai suivant l'ISO 2592[2]. La Méthode A est applicable aux distillats de pétrole (carburant diesel, mélanges de biocarburant, fioul domestique et turbocombustibles), aux huiles lubrifiantes neuves et en service, aux peintures et vernis, et à d'autres liquides homogènes ne faisant pas partie du champ d'application des Méthodes B ou C. La Méthode B est applicable aux combustibles résiduels, aux résidus de bitumes fluidifiés, aux huiles lubrifiantes usagées, aux mélanges de liquides contenant des matières solides, aux liquides ayant tendance à former un film en surface dans les conditions d'essai ou ayant une viscosité cinématique telle qu'ils ne sont pas chauffés de manière uniforme sous agitation et dans les conditions de chauffage de la Méthode A. La Méthode C est applicable aux esters méthyliques d'acides gras (EMAG) tels que définis dans des spécifications telles que l'EN 14214[11] ou l'ASTM D 6751[13]. La présente Norme internationale n'est pas applicable aux peintures et vernis renfermant de l'eau. NOTE 2 Le point d'éclair des peintures et vernis renfermant de l'eau peut être déterminé suivant l'ISO 3679[3]. Les liquides contenant des traces de produits hautement volatils peuvent être analysés conformément à l'ISO 1523[1] ou l'ISO 3679.
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INTERNATIONAL ISO
STANDARD 2719
Fourth edition
2016-06-15
Determination of flash point —
Pensky-Martens closed cup method
Détermination du point d’éclair — Méthode Pensky-Martens en
vase clos
Reference number
ISO 2719:2016(E)
©
ISO 2016
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ISO 2719:2016(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2016, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
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ii © ISO 2016 – All rights reserved
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ISO 2719:2016(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 2
5 Chemicals and materials . 2
6 Apparatus . 2
7 Apparatus preparation . 3
7.1 General . 3
7.2 Location of the apparatus . 3
7.3 Cleaning the test cup . 3
7.4 Apparatus assembly . 3
7.5 Apparatus verification . 3
8 Sampling . 4
9 Sample handling . 4
9.1 Petroleum products . 4
9.1.1 Sub-sampling . 4
9.1.2 Samples containing undissolved water . 4
9.1.3 Samples that are liquid at ambient temperature . 4
9.1.4 Samples that are very viscous, semi-solid or solid at ambient temperature . 4
9.2 Paints and varnishes . 5
10 Procedure. 5
10.1 General . 5
10.2 Procedure A . 5
10.3 Procedure B . 6
10.4 Procedure C . 7
11 Calculation . 8
11.1 Conversion of barometric pressure reading . 8
11.2 Correction of observed flash point to standard atmospheric pressure . 8
12 Expression of results . 8
13 Precision . 8
13.1 General . 8
13.2 Repeatability, r .8
13.3 Reproducibility, R .9
14 Test report .10
Annex A (informative) Apparatus verification .11
Annex B (normative) Pensky-Martens closed cup test apparatus .14
Annex C (normative) Temperature measuring device specification .20
Bibliography .22
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ISO 2719:2016(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 documents 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).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on 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 the following URL: www.iso.org/iso/foreword.html.
The committee responsible for this document is ISO/TC 28, Petroleum products and related products of
synthetic or biological origin, in conjunction with ISO/TC 35, Paints and varnishes.
This fourth edition cancels and replaces the third edition (ISO 2719:2002), which has been technically
revised.
The main technical updates include:
a) introduction of procedure C for FAME products;
b) revision of temperature measuring device requirements, allowing alternatives for Hg-containing
thermometers;
c) removal of the original Annex D on the adaptor for the low-range thermometer, it being optional
when a permanent ferrule is attached to the thermometer;
d) revision of procedures regarding sampling and sample handling;
e) inclusion, for automated apparatus, manufactured after 1 January 2017, of a device to automatically
dispense an inert gas or vapour over the test cup in the event of a test cup fire.
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ISO 2719:2016(E)
Introduction
Flash point values are used in shipping, storage, handling, and safety regulations, as a classification
property to define “flammable” and “combustible” materials. Precise definition of the classes is given in
each particular regulation.
A flash point value can indicate the presence of highly volatile material(s) in a relatively non-volatile or
non-flammable material and flash point testing can be a preliminary step to other investigations into
the composition of unknown materials.
It is not appropriate for flash point determinations to be carried out on potentially unstable,
decomposable, or explosive materials, unless it has been previously established that heating the
specified quantity of such materials in contact with the metallic components of the flash point
apparatus, within the temperature range required for the method, does not induce decomposition,
explosion or other adverse effects.
Flash point values are not a constant physical-chemical property of materials tested. They are a
function of the apparatus design, the condition of the apparatus used, and the operational procedure
carried out. Flash point can therefore be defined only in terms of a standard test method, and no general
valid correlation can be guaranteed between results obtained by different test methods or with test
apparatus different from that specified.
[6] [12]
ISO/TR 29662 (CEN/TR 15138 ) gives useful advice in carrying out flash point tests and
interpreting their results.
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INTERNATIONAL STANDARD ISO 2719:2016(E)
Determination of flash point — Pensky-Martens closed
cup method
WARNING — The use of this International Standard can involve hazardous materials, operations
and equipment. This International Standard does not purport to address all of the safety
problems associated with its use. It is the responsibility of users of this International Standard
to take appropriate measures to ensure the safety and health of personnel prior to application of
this International Standard, and fulfil statutory and regulatory requirements for this purpose.
1 Scope
This International Standard describes three procedures, A, B and C, using the Pensky-Martens closed
cup tester, for determining the flash point of combustible liquids, liquids with suspended solids, liquids
that tend to form a surface film under the test conditions, biodiesel and other liquids in the temperature
range of 40 °C to 370 °C.
CAUTION — For certain mixtures no flash point, as defined, is observed; instead a significant
enlargement of the test flame (not halo effect) and a change in colour of the test flame from blue
to yellowish-orange can occur. Continued heating can result in significant burning of vapours
outside the test cup, and can be a potential fire hazard.
NOTE 1 Although, technically, kerosene with a flash point above 40 °C can be tested using this International
[5]
Standard, it is standard practice to test kerosene according to ISO 13736. Similarly, lubricating oils are
[2]
normally tested according to ISO 2592 .
Procedure A is applicable to distillate fuels (diesel, biodiesel blends, heating oil and turbine fuels), new
and in-use lubricating oils, paints and varnishes, and other homogeneous liquids not included in the
scope of Procedures B or C.
Procedure B is applicable to residual fuel oils, cutback residua, used lubricating oils, mixtures of liquids
with solids, liquids that tend to form a surface film under test conditions or are of such kinematic
viscosity that they are not uniformly heated under the stirring and heating conditions of Procedure A.
Procedure C is applicable to fatty acid methyl esters (FAME) as specified in specifications such as
[11] [13]
EN 14214 or ASTM D6751 .
This International Standard is not applicable to water-borne paints and varnishes.
[3]
NOTE 2 Water-borne paints and varnishes can be tested using ISO 3679 . Liquids containing traces of highly
[1]
volatile materials can be tested using ISO 1523 or ISO 3679.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 1513, Paints and varnishes — Examination and preparation of test samples
ISO 3170, Petroleum liquids — Manual sampling
ISO 3171, Petroleum liquids — Automatic pipeline sampling
ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling
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ISO 2719:2016(E)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
flash point
lowest temperature of the test portion, corrected to a standard barometric pressure of 101,3 kPa, at
which application of an ignition source causes the vapour of the test portion to ignite and the flame to
propagate across the surface of the liquid under the specified conditions of test
4 Principle
The test portion is placed into the test cup of a Pensky-Martens apparatus and heated to give a constant
temperature increase with continuous stirring. An ignition source is directed through an opening in
the test cup lid at regular temperature intervals with simultaneous interruption of stirring. The lowest
temperature at which the application of the ignition source causes the vapour of the test portion to
ignite and a flame propagate over the surface of the liquid is recorded as the flash point at the absolute
barometric pressure. This temperature is corrected to standard atmospheric pressure using a specified
formula.
5 Chemicals and materials
5.1 Cleaning solvent, for removal of traces of sample from the test cup and cover.
The choice of solvent will depend upon the previous material tested and the tenacity of the residue. Low
volatility aromatic (benzene free) solvents may be used to remove traces of oil, and mixed solvents such
as toluene-acetone-methanol can be efficacious for the removal of gum-type deposits.
5.2 Liquids for verification, see Annex A.
6 Apparatus
6.1 Flash point apparatus, as described in Annex B.
If automated equipment is used, ensure that the test cup and cover assembly conform to the key
dimensions specified in Annex B and the procedure described in Clause 10 is followed. The user shall
ensure that all of the manufacturer’s instructions for adjusting and operating the instrument are
followed.
NOTE Under certain circumstances, the use of electric ignition sources can give different results to those
obtained when using a flame ignition source.
In cases of dispute, unless explicitly agreed otherwise, the flash point as determined using a flame
ignition source shall be considered the referee test.
6.2 Temperature measuring devices, meeting the requirements for accuracy and have the response
as specified in Annex C.
6.3 Barometer, absolute pressure reading, accuracy of ±0,5 kPa, and with a resolution of 0,1 kPa.
Barometers pre-corrected to give sea level readings, such as those used at weather stations and
airports, shall not be used.
NOTE Some automated apparatus include an integral barometer that automatically measures and records
the absolute barometric pressure and makes the required corrections to the detected flash point.
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ISO 2719:2016(E)
6.4 Heating bath or oven, capable of controlling the temperature to ±5 °C, for warming the sample if
required.
The oven shall be ventilated and constructed in such a way that it will not cause ignition of any
flammable vapours that can be produced when the sample is heated.
It is recommended that the oven is an explosion-protected type.
7 Apparatus preparation
7.1 General
Follow the manufacturer’s instructions for the correct setup, calibration, verification (7.5) and
operation of the apparatus including the integral barometer (if fitted) and temperature measuring
device (see Annex C), especially the operation and setting of the ignition source.
7.2 Location of the apparatus
Support the flash point apparatus (6.1) on a level and steady surface in a draught-free position.
NOTE When draughts cannot be avoided, it is good practice to surround the apparatus with a shield.
The flash point apparatus may be located in a fume hood with individual air flow control, adjusted so
that vapours can be withdrawn without causing air currents around the test cup during the test.
7.3 Cleaning the test cup
Wash the test cup, cover and its accessories with an appropriate cleaning solvent (5.1) to remove any
traces of gum or residue remaining from a previous test. Dry using a stream of clean air to ensure
complete removal of the solvent used.
7.4 Apparatus assembly
Examine the test cup, the cover and other parts to ensure that they are free from signs of damage and
deposits. Assemble the apparatus in accordance with Annex B.
7.5 Apparatus verification
7.5.1 Verify the correct functioning of the apparatus at least once a year by testing a certified reference
material (CRM) (5.2). The result obtained shall be equal to or less than R/ 2 from the certified value of
the CRM, where R is the reproducibility of the method as shown in Table 4.
Use the reproducibility for Procedure A (Table 4) to calculate the verification tolerance for verification
materials certified for Procedures A, B or C.
It is recommended that more frequent verification checks are made using secondary working standards
(SWSs) (5.2).
A recommended procedure for apparatus verification using CRMs and SWSs, and the production of
SWSs, is described in Annex A.
7.5.2 The numerical values obtained during the verification check shall not be used to provide a bias
statement, nor shall they be used to make any correction to the flash points subsequently determined
using the apparatus.
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ISO 2719:2016(E)
8 Sampling
8.1 Unless otherwise specified, obtain representative samples for analysis in accordance with the
procedures given in ISO 3170, ISO 3171, ISO 15528 or an equivalent National Standard.
8.2 When obtaining a sample of residual fuel oil, the sample container shall be from 85 % to 95 % full.
For FAME samples, a typical one litre container filled to 85 % volume is recommended. For other types
of samples, the size of the container shall be chosen such that the container is not more than 85 % full or
less than 50 % full prior to any sample aliquot being taken.
8.3 Erroneously high flash points can be obtained if precautions are not taken to avoid the loss of
volatile material. Do not open containers unnecessarily, to prevent loss of volatile material or possible
introduction of moisture. Avoid storage of samples at temperatures in excess of 30 °C. For samples for
storage, ensure that the sample container is tightly closed and leak free. Do not make a transfer unless
the sample temperature is at least the equivalent of 18 °C below the expected flash point.
8.4 Do not store samples in gas-permeable containers, since volatile material may diffuse through the
walls of the enclosure. Samples in leaky containers are suspect and not a source of valid results.
9 Sample handling
9.1 Petroleum products
9.1.1 Sub-sampling
9.1.1.1 Sub-sample at a temperature at least 18 °C below the expected flash point.
9.1.1.2 Successive test portions may be taken from the same sample container. Repeat tests have been
shown to be within the precision of the method when the second test portion is taken with the sample
container at least 50 % filled.
IMPORTANT — Results of flash point determinations can be affected if the sample volume falls
below 50 % of the container capacity.
9.1.2 Samples containing undissolved water
9.1.2.1 Flash point results can be affected by the presence of water. If a sample contains undissolved
water, decant a water-free aliquot prior to mixing.
9.1.2.2 For certain fuel oils and lubricants, it is not always possible to decant the sample from the
free water. In such cases, separate the water from the aliquot physically, prior to mixing, or, if this is not
[3]
possible, test the material in accordance with ISO 3679 .
9.1.3 Samples that are liquid at ambient temperature
Mix samples by gentle manual shaking prior to removal of the test portion, taking care to minimize the
loss of volatile components and proceed in accordance with Clause 10.
9.1.4 Samples that are very viscous, semi-solid or solid at ambient temperature
Samples shall be heated in their containers, with lid/cap slightly loosened to avoid build-up of
dangerous pressure, at the lowest temperature adequate to liquefy any solids, not exceeding 18 °C
below the expected flash point, for 30 min. If the sample is then not completely liquefied, extend the
heating period for additional 30 min periods as necessary. Then gently agitate the sample to provide
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ISO 2719:2016(E)
mixing, such as orbiting the container horizontally, before transferring to the test cup. No sample shall
be heated and transferred unless its temperature is more than 18 °C below its expected flash point.
IMPORTANT — Volatile vapours can escape during heating when the sample container lid/cap is
too loose.
9.2 Paints and varnishes
Prepare the samples in accordance with ISO 1513.
10 Procedure
10.1 General
10.1.1 The applicability of the three procedures A, B and C is explained in Clause 1.
Electronic flash point detection shall be used for procedure C, as it is difficult to observe a flash by
visual means, and may be used for procedures A and B.
10.1.2 Care should be taken when testing samples of residual fuel oil that contain significant amounts of
water, as heating these samples can cause them to foam and eject from the test cup.
10.1.3 As a safety practice, it is strongly advised to apply the ignition source to the test portion in the cup
before heating the test cup and test portion, to check for the presence of unexpected volatile material.
10.1.4 As a safety practice, it is strongly advised that, for an expected flash point above 130 °C, to dip
the ignition source every 10 °C throughout the test until the sample temperature reaches 28 °C below the
expected flash point and then follow the prescribed dipping procedure. This practice has been shown to
reduce the possibility of a fire and not to significantly affect the result.
10.1.5 At the end of a test, when the apparatus has cooled down to a safe handling temperature, remove
the test cover and the test cup and clean the apparatus as recommended by the manufacturer.
10.2 Procedure A
10.2.1 Record the laboratory absolute barometric pressure reading at the time of test (see 6.3).
It is not necessary to correct the barometric pressure to 0 °C, although some barometers are designed
to make this correction automatically.
10.2.2 Fill the test cup (see 7.3) with the test portion to the level indicated by the filling mark. Place
the lid on the test cup and put them in the heating chamber. Ensure that the locating or locking device
is properly engaged and insert the temperature measuring device (6.2). Light the test flame and adjust
to a diameter of 3,2 mm to 4,8 mm or enable the alternative ignition source. Supply heat at such a rate
that the temperature of the test portion, as indicated by the temperature measuring device, increases
at 5,0 °C/min to 6,0 °C/min, and maintain this heating rate throughout the test. Stir the test portion at a
rotational rate of 90 r/min (1,5 Hz) to 120 r/min (2,0 Hz), stirring in a downward direction.
10.2.3 When the test portion is expected to have a flash point of 110 °C or below, make the first
application of the ignition source when the temperature of the test portion is 23 °C ±5 °C below the
expected flash point, and thereafter at 1 °C temperature intervals. Cease stirring and apply the ignition
source by operating the mechanism on the cover, that controls the shutter and ignition source, so that
the source is lowered into the vapour space of the test cup in 0,5 s, left in its lowered position for 1 s, and
quickly raised to its high position.
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ISO 2719:2016(E)
10.2.4 When the test portion is expected to have a flash point of above 110 °C, make the first application
of the ignition source when the temperature of the test portion is 23 °C ±5 °C below the expected flash
point, and thereafter at temperatures that are a multiple of 2 °C. Cease stirring and apply the ignition
source by operating the mechanism on the cover, that controls the shutter and ignition source, so that
the source is lowered into the vapour space of the test cup in 0,5 s, left in its lowered position for 1 s, and
quickly raised to its high position.
10.2.5 When testing a material of unknown flash point, conduct a preliminary test at a suitable starting
temperature. Make the first ignition source application at 5 °C above the starting temperature and follow
the procedure given in 10.2.3 or 10.2.4, as applicable.
10.2.6 Record, as the detected flash point, the temperature of the test portion read on the temperature
measuring device at the time when ignition source application causes a distinct flash in the interior of the
test cup. Do not confuse the true flash point with the bluish halo that sometimes surrounds the ignition
source at applications preceding the actual flash point.
10.2.7 When a flash point is detected on the first application
...
DRAFT INTERNATIONAL STANDARD
ISO/DIS 2719
ISO/TC 28 Secretariat: NEN
Voting begins on: Voting terminates on:
2015-06-18 2015-09-18
Determination of flash point — Pensky-Martens closed cup
method
Détermination du point d’éclair — Méthode Pensky-Martens en vase clos
ICS: 75.080
ISO/CEN PARALLEL PROCESSING
This draft has been developed within the International Organization for
Standardization (ISO), and processed under the ISO lead mode of collaboration
as defined in the Vienna Agreement.
This draft is hereby submitted to the ISO member bodies and to the CEN member
bodies for a parallel five month enquiry.
Should this draft be accepted, a final draft, established on the basis of comments
received, will be submitted to a parallel two-month approval vote in ISO and
THIS DOCUMENT IS A DRAFT CIRCULATED
formal vote in CEN.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
To expedite distribution, this document is circulated as received from the
IN ADDITION TO THEIR EVALUATION AS
committee secretariat. ISO Central Secretariat work of editing and text
BEING ACCEPTABLE FOR INDUSTRIAL,
composition will be undertaken at publication stage.
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 2719:2015(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
©
PROVIDE SUPPORTING DOCUMENTATION. ISO 2015
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ISO/DIS 2719:2015(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2015
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
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Published in Switzerland
ii © ISO 2015 – All rights reserved
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ISO/DIS 2719
Contents Page
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle. 2
5 Chemicals and materials . 2
6 Apparatus . 2
7 Apparatus preparation . 3
7.1 General . 3
7.2 Location of the apparatus. 3
7.3 Cleaning the test cup . 3
7.4 Apparatus assembly . 3
7.5 Apparatus verification . 3
8 Sampling. 4
9 Sample handling . 4
9.1 Petroleum products . 4
9.1.1 Subsampling . 4
9.1.2 Samples containing undissolved water . 4
9.1.3 Samples that are liquid at ambient temperature . 4
9.1.4 Samples that are very viscous, semi- solid or solid at ambient temperature. . 4
9.2 Paints and varnishes . 5
10 Procedure . 5
10.1 General . 5
10.2 Procedure A . 5
10.3 Procedure B . 6
10.4 Procedure C . 7
11 Calculation . 7
11.1 Conversion of barometric pressure reading . 7
11.2 Correction of observed flash point to standard atmospheric pressure . 8
12 Expression of results . 8
13 Precision. 8
13.1 General . 8
13.2 Repeatability, r . 8
13.3 Reproducibility, R . 9
The test report shall contain at least the following information: . 10
Annex A (informative) Apparatus verification . 11
Annex B (normative) Pensky-Martens closed cup test apparatus . 14
Annex C (normative) Temperature measuring device specification . 20
© ISO 2015 – All rights reserved iii
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ISO/DIS 2719
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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 2719 was prepared by Technical Committee ISO/TC 28, Petroleum products and related products of
synthetic or biological origin, Working Group 9, in conjunction with Technical Committee ISO/TC 35, Paints
and varnishes, Technical Committee CEN/TC 19, Gaseous and liquid fuels, lubricants and related products of
petroleum, synthetic and biological origin, and Technical Committee CEN/TC 139, Paints and varnishes.
This third edition cancels and replaces the second edition (ISO 2719:2002).
The main technical updates are:
a) Introduction of procedure C for FAME products,
b) Revision of temperature measuring device requirements, allowing alternatives for Hg-containing
thermometers,
c) Removal of the original Annex D on the adaptor for the low-range thermometer,
d) Revision of procedures regarding sampling and sample handling, and
e) Inclusion, for automated apparatus, manufactured after 1 January 2017, of a device to automatically
dispense an inert gas or vapour over the test cup in the event of a test cup fire.
iv © ISO 2015 – All rights reserved
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ISO/DIS 2719
Introduction
Flash point values are used in shipping, storage, handling, and safety regulations, as a classification property
to define “flammable” and “combustible” materials. Precise definition of the classes is given in each particular
regulation.
A flash point value can indicate the presence of highly volatile material(s) in a relatively non-volatile or
non-flammable material and flash point testing can be a preliminary step to other investigations into the
composition of unknown materials.
It is not appropriate for flash point determinations to be carried out on potentially unstable, decomposable, or
explosive materials, unless it has been previously established that heating the specified quantity of such
materials in contact with the metallic components of the flash point apparatus, within the temperature range
required for the method, does not induce decomposition, explosion or other adverse effects.
Flash point values are not a constant physical-chemical property of materials tested. They are a function of
the apparatus design, the condition of the apparatus used, and the operational procedure carried out. Flash
point can therefore be defined only in terms of a standard test method, and no general valid correlation can be
guaranteed between results obtained by different test methods or with test apparatus differ rent from that
specified.
[2]
[1]
ISO TR 29662 (CEN/TR 15138 ) gives useful advice in carrying out flash point tests and interpreting their
results.
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DRAFT INTERNATIONAL STANDARD ISO/DIS 2719
Determination of flash point — Pensky-Martens closed cup
method
WARNING — The use of this International Standard may involve hazardous materials, operations and
equipment. This International Standard does not purport to address all of the safety problems
associated with its use. It is the responsibility of the user of this International Standard to establish
appropriate safety and health practices and determine the applicability of regulatory limitations prior
to use.
1 Scope
This International Standard describes three procedures, A, B and C, using the Pensky-Martens closed cup
tester, for determining the flash point of combustible liquids, liquids with suspended solids, liquids that tend to
form a surface film under the test conditions, biodiesel and other liquids in the temperature range of 40 C to
370 C.
CAUTION — For certain mixtures no flash point, as defined, is observed; instead a significant
enlargement of the test flame (not halo effect) and a change in colour of the test flame from blue to
yellowish-orange can occur. Continued heating can result in significant burning of vapours outside
the test cup, and can be a potential fire hazard.
NOTE 1 Although, technically, kerosenes with a flash point above 40 C can be tested using this International
[3]
Standard, it is standard practice to test kerosenes according to ISO 13736 . Similarly, lubricating oils are normally tested
[4]
according to ISO 2592 .
Procedure A is applicable to distillate fuels (diesel, biodiesel blends, heating oil and turbine fuels), new and in-
use lubricating oils, paints and varnishes, and other homogeneous liquids not included in the scope of
Procedures B or C.
Procedure B is applicable to residual fuel oils, cutback residua, used lubricating oils, mixtures of liquids with
solids, liquids that tend to form a surface film under test conditions or are of such kinematic viscosity that they
are not uniformly heated under the stirring and heating conditions of Procedure A.
Procedure C is applicable to fatty acid methyl esters (FAME) as specified in specifications such as
[5] [6]
EN 14214 or ASTM D 6751 .
This International Standard is not applicable to water-borne paints and varnishes.
[7]
NOTE 2 Water-borne paints and varnishes can be tested using ISO 3679 . Liquids containing traces of highly volatile
[8]
materials can be tested using ISO 1523 or ISO 3679.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
ISO 1513, Paints and varnishes — Examination and preparation of samples for testing.
ISO 3170 , Petroleum liquids — Manual sampling.
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ISO/DIS 2719
ISO 3171, Petroleum liquids — Automatic pipeline sampling.
ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
flash point
lowest temperature of the test portion, corrected to a barometric pressure of 101,3 kPa, at which application of
an ignition source causes the vapour of the test portion to ignite and the flame to propagate across the surface
of the liquid under the specified conditions of test.
4 Principle
The test portion is placed into the test cup of a Pensky-Martens apparatus and heated to give a constant
temperature increase with continuous stirring. An ignition source is directed through an opening in the test cup
lid at regular temperature intervals with simultaneous interruption of stirring. The lowest temperature at which
the application of the ignition source causes the vapour of the test portion to ignite and a flame propagate over
the surface of the liquid is recorded as the flash point at the absolute barometric pressure. This temperature is
corrected to standard atmospheric pressure using the specified equation.
5 Chemicals and materials
5.1 Cleaning solvent, for removal of traces of sample from the test cup and cover.
The choice of solvent will depend upon the previous material tested, and the tenacity of the residue. Low
volatility aromatic (benzene free) solvents may be used to remove traces of oil, and mixed solvents such as
toluene-acetone-methanol can be efficacious for the removal of gum-type deposits.
5.2 Liquids for verification, see Annex A.
6 Apparatus
6.1 Flash point apparatus, as described in Annex B.
If automated equipment is used, ensure that the test cup and cover assembly conform to the key dimensions
specified in Annex B, and the procedure described in Clause 10 is followed. The user shall ensure that all of
the manufacturer’s instructions for adjusting and operating the instrument are followed.
NOTE Under certain circumstances, the use of electric ignition sources can give different results to those obtained
when using a flame ignition source.
In cases of dispute, unless explicitly agreed otherwise, the flash point as determined using a flame ignition
source shall be considered the referee test.
6.2 Temperature measuring device, meeting the requirements for accuracy and have the response as
specified in Annex C.
The aperture in the cover assembly and the fitting required to hold the temperature measuring device may be
modified to closely fit the temperature measuring device utilized.
6.3 Barometer, absolute pressure reading, accuracy of ± 0,5 kPa, and with a resolution of 0,1 kPa.
Barometers pre-corrected to give sea level readings, such as those used at weather stations and airports,
shall not be used.
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ISO/DIS 2719
NOTE Some automated apparatus include an integral barometer that automatically measures and records the
absolute barometric pressure, and makes the required corrections to the detected flash point.
6.4 Heating bath or oven, capable of controlling the temperature to 5 C, for warming the sample if
required.
The oven shall be ventilated and constructed in such a way that it will not cause ignition of any flammable
vapours that can be produced when the sample is heated.
It is recommended that the oven is an explosion-protected type.
7 Apparatus preparation
7.1 General
Follow the manufacturer’s instructions for the correct set-up, calibration, verification (7.5) and operation of the
apparatus including the integral barometer (if fitted) and temperature measuring device (see Annex C),
especially the operation and setting of the ignition source,
7.2 Location of the apparatus
Support the apparatus (6.1) on a level and steady surface in a draught-free position.
NOTE When draughts cannot be avoided, it is good practice to surround the apparatus with a shield.
The apparatus may be located in a fume hood with an individual control of air flow, adjusted so that vapours
can be withdrawn without causing air currents around the test cup during the test.
7.3 Cleaning the test cup
Wash the test cup, cover and its accessories with an appropriate solvent (5.1) to remove any traces of gum or
residue remaining from a previous test. Dry using a stream of clean air to ensure complete removal of the
solvent used.
7.4 Apparatus assembly
Examine the test cup, the cover and other parts to ensure that they are free from signs of damage and
deposits. Assemble the apparatus in accordance with Annex B.
7.5 Apparatus verification
7.5.1 Verify the correct functioning of the apparatus at least once a year by testing a certified reference
material (CRM) (5.2). The result obtained shall be equal to or less than R 2 from the certified value of the
CRM, where R is the reproducibility of the method as shown in Table 4.
7.5.1.1 Use the reproducibility for Procedure A (Table 4) to calculate the verification tolerance for
verification materials certified for Procedures A, B or C.
It is recommended that more frequent verification checks are made using secondary working standards
(SWSs) (5.2).
A recommended procedure for apparatus verification using CRMs and SWSs, and the production of SWSs, is
described in Annex A.
7.5.2 The numerical values obtained during the verification check shall not be used to provide a bias
statement, nor shall they be used to make any correction to the flash points subsequently determined using
the apparatus.
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ISO/DIS 2719
8 Sampling
8.1 Unless otherwise specified, obtain representative samples for analysis in accordance with the
procedures given in ISO 3170, ISO 3171, ISO 15528 or an equivalent National Standard.
8.2 When obtaining a sample of residual fuel oil, the sample container shall be from 85 % to 95 % full. For
FAME samples, a typical one litre container filled to 85 % volume is recommended. For other types of
samples, the size of the container shall be chosen such that the container is not more than 85 % full or less
than 50 % full prior to any sample aliquot being taken.
8.3 Erroneously high flash points can be obtained if precautions are not taken to avoid the loss of volatile
material. Do not open containers unnecessarily, to prevent loss of volatile material or possible introduction of
moisture. Avoid storage of samples at temperatures in excess of 30 °C . Samples for storage shall be capped
tightly with inner seals. Do not make a transfer unless the sample temperature is at least the equivalent of
18 °C below the expected flash point.
8.4 Do not store samples in gas-permeable containers, since volatile material may diffuse through the walls
of the enclosure. Samples in leaky containers are suspect and not a source of valid results.
9 Sample handling
9.1 Petroleum products
9.1.1 Subsampling
9.1.1.1 Sub sample at a temperature at least 18 °C below the expected flash point.
9.1.1.2 Successive test portions may be taken from the same sample container. Repeat tests have been
shown to be within the precisions of the method when the second test portion is taken with the sample
container at least 50 % filled (See Note 1 to 10.1.1)
9.1.2 Samples containing undissolved water
9.1.2.1 Flash point results can be affected by the presence of water, if a sample contains undissolved
water, decant an aliquot from the water prior to mixing.
9.1.2.2. For certain fuel oils and lubricants it is not always possible to decant the sample from the free
water. In such cases, separate the water from the aliquot physically, prior to mixing, or, if this is not possible,
[7]
test the material in accordance with ISO 3679 .
9.1.3 Samples that are liquid at ambient temperature
Mix samples by gentle manual shaking prior to removal of the test portion, taking care to minimize the loss of
volatile components and proceed in accordance with clause 10.
9.1.4 Samples that are very viscous, semi- solid or solid at ambient temperature.
Samples shall be heated in their containers, with lid/cap slightly loosened to avoid build-up of dangerous
pressure, at the lowest temperature adequate to liquefy any solids, not exceeding 18 °C below the expected
flash point, for 30 min. If the sample is then not completely liquefied, extend the heating period for additional
30 min periods as necessary. Then gently agitate the sample to provide mixing, such as orbiting the container
horizontally, before transferring to the test cup. No sample shall be heated and transferred unless its
temperatures is more than 18 °C below its expected flash point.
IMPORTANT — Volatile vapours can escape during heating when the sample container lid/cap is too
loose.
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ISO/DIS 2719
9.2 Paints and varnishes
Prepare the samples in accordance with ISO 1513.
10 Procedure
10.1 General
10.1.1 The applicability of the three procedures A, B and C is given in the Scope.
Electronic flash point detection shall be used for this procedure as it is difficult to observe a flash by visual
means.
NOTE Results of flash point determinations can be affected if the sample volume falls below 50 % of the container
capacity.
Care should be taken when testing samples of residual fuel oil that contain significant amounts of water as
heating these samples can cause them to foam and eject from the test cup.
10.1.2 As a safety practice it is strongly advised to apply the ignition source to the test portion in the cup
before heating the test cup and test portion, to check for the presence of unexpected volatile material.
10.1.3 As a safety practice, it is strongly advised that, for an expected flash point above 130 °C, to dip the
ignition source every 10 °C throughout the test until the sample temperature reaches 28 °C below the
expected flash point and then follow the prescribed dipping procedure. This practice has been shown to
reduce the possibility of a fire, and not to significantly affect the result.
10.1.4 At the end of a test, when the apparatus has cooled down to a safe handling temperature, remove the
test cover and the test cup and clean the apparatus as recommended by the manufacturer.
10.2 Procedure A
10.2.1 Record the laboratory absolute barometric pressure at the time of test.(see 6.3)
It is not necessary to correct the barometric pressure to 0 C, although some barometers are designed to
make this correction automatically.
10.2.2 Fill the test cup (see 7.3) with the test portion to the level indicated by the filling mark. Place the lid on
the test cup and put them in the heating chamber. Ensure that the locating or locking device is properly
engaged and insert the temperature measuring device (6.2). Light the test flame and adjust to a diameter of
3,2 mm to 4,8 mm or enable the alternative ignition source. Supply heat at such a rate that the temperature of
the test portion, as indicated by the temperature measuring device, increases at 5,0 C/min to 6,0 C/min, and
maintain this heating rate throughout the test. Stir the test portion at a rate of plus minus 90 r/min to 120 r/min,
stirring in a downward direction.
10.2.3 When the test portion is expected to have a flash point of 110 C or below, make the first application
of the ignition source when the temperature of the test portion is 23 C 5 C below the expected flash point,
and thereafter at 1 C temperature intervals. Cease stirring and apply the ignition source by operating the
mechanism on the cover, that controls the shutter and ignition source, so that the source is lowered into the
vapour space of the test cup in 0,5 s, left in its lowered position for 1 s, and quickly raised to its high position.
10.2.4 When the test portion is expected to have a flash point of above 110 C, make the first application of
the ignition source when the temperature of the test portion is 23 C 5 C below the expected flash point,
and thereafter at temperatures that are a multiple of 2 C. Cease stirring and apply the ignition source by
operating the mechanism on the cover, that controls the shutter and ignition source, so that the source is
lowered into the vapour space of the test cup in 0,5 s, left in its lowered position for 1 s, and quickly raised to
its high position.
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ISO/DIS 2719
10.2.5 When testing a material of unknown flash point, conduct a preliminary test at a suitable starting
temperature. Make the first ignition source application at 5 C above the starting temperature and follow the
procedure given in 10.2.3 or 10.2.4, as applicable.
10.2.6 Record, as the detected flash point, the temperature of the test portion read on the temperature
measuring device at the time when ignition source application causes a distinct flash in the interior of the test
cup. Do not confuse the true flash point with the bluish halo that sometimes surrounds the ignition source at
applications preceding the actual flash point.
10.2.7 When a flash point is detected on the first application, the test shall be discontinued, the result
discarded, and the test repeated with a fresh test portion. The first application of the ignition source with the
fresh test portion is recommended to be approximately 23 °C below the temperature at which a flash point
was detected on the first application.
10.2.8 When the temperature at which the flash point is detected is less than 18 C or greater than 28 C
from the temperature of the first application of the ignition source, the result shall be considered approximate.
Repeat the test using a fresh test portion, adjusting the temperature of the first application of the ignition
source until a valid determination is obtained, that is where the flash point is 18 C to 28 C above the
temperature of the first application of the ignition source.
10.3 Procedure B
10.3.1 Record the laboratory absolute barometric pressure at the time of test (see 10.2.1).
10.3.2 Fill the test cup (see 7.3) with the test portion to the level indicated by the filling mark. Place the lid on
the test cup and put them in the heating chamber. Ensure that the locating or locking device is properly
engaged and insert the temperature measuring device (6.2). Light the test flame and adjust to a diameter of
3,2 mm to 4,8 mm or enable the alternative ignition source. Supply heat at suc
...
NORME ISO
INTERNATIONALE 2719
Quatrième édition
2016-06-15
Détermination du point d'éclair —
Méthode Pensky-Martens en vase clos
Determination of flash point — Pensky-Martens closed cup method
Numéro de référence
ISO 2719:2016(F)
©
ISO 2016
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ISO 2719:2016(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2016, Publié en Suisse
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ii © ISO 2016 – Tous droits réservés
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ISO 2719:2016(F)
Sommaire Page
Avant-propos .iv
Introduction .v
1 Domaine d'application . 1
2 Références normatives . 1
3 Termes et définitions . 2
4 Principe . 2
5 Produits chimiques et matériaux . 2
6 Appareillage . 2
7 Préparation de l’appareil . 3
7.1 Généralités . 3
7.2 Emplacement de l'appareil . 3
7.3 Nettoyage du vase d'essai . 3
7.4 Assemblage de l'appareil . 3
7.5 Vérification de l'appareil . 3
8 Échantillonnage . 4
9 Manutention des échantillons . 4
9.1 Produits pétroliers . 4
9.1.1 Sous-échantillonnage . 4
9.1.2 Échantillons contenant de l'eau libre . 5
9.1.3 Échantillons liquides à température ambiante . 5
9.1.4 Échantillons hautement visqueux, semi-solides ou solides à
température ambiante . 5
9.2 Peintures et vernis . 5
10 Mode opératoire. 5
10.1 Généralités . 5
10.2 Méthode A . 6
10.3 Méthode B . 7
10.4 Méthode C . 8
11 Calculs . 8
11.1 Conversion des indications de pression barométrique . 8
11.2 Correction du point d'éclair observé à la pression atmosphérique standard . 9
12 Expression des résultats. 9
13 Fidélité . 9
13.1 Généralités . 9
13.2 Répétabilité, r .9
13.3 Reproductibilité, R .10
14 Rapport d'essai .11
Annexe A (informative) Vérification de l’appareil .12
Annexe B (normative) Appareil Pensky-Martens en vase clos .15
Annexe C (normative) Spécifications du dispositif de mesure de la température .21
Bibliographie .23
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ISO 2719:2016(F)
Avant-propos
L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes
nationaux de normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est
en général confiée aux comités techniques de l'ISO. Chaque comité membre intéressé par une étude
a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,
gouvernementales et non gouvernementales, en liaison avec l'ISO participent également aux travaux.
L'ISO collabore étroitement avec la Commission électrotechnique internationale (IEC) en ce qui
concerne la normalisation électrotechnique.
Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont
décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier de prendre note des différents
critères d'approbation requis pour les différents types de documents ISO. Le présent document a été
rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir www
.iso .org/ directives).
L'attention est attirée sur le fait que certains des éléments du présent document peuvent faire l'objet de
droits de propriété intellectuelle ou de droits analogues. L'ISO ne saurait être tenue pour responsable
de ne pas avoir identifié de tels droits de propriété et averti de leur existence. Les détails concernant
les références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de
l'élaboration du document sont indiqués dans l'Introduction et/ou dans la liste des déclarations de
brevets reçues par l'ISO (voir www .iso .org/ brevets).
Les appellations commerciales éventuellement mentionnées dans le présent document sont données
pour information, par souci de commodité, à l’intention des utilisateurs et ne sauraient constituer un
engagement.
Pour une explication de la signification des termes et expressions spécifiques de l'ISO liés à l'évaluation
de la conformité, ou pour toute information au sujet de l'adhésion de l'ISO aux principes de l’Organisation
mondiale du commerce (OMC) concernant les obstacles techniques au commerce (OTC), voir le lien
suivant: www .iso .org/ avant -propos.
Le comité responsable du présent document est l’ISO/TC 28, Produits pétroliers et produits connexes
d'origine synthétique ou biologique, en collaboration avec le comité technique ISO/TC 35, Peintures et vernis.
Cette quatrième édition annule et remplace la troisième (ISO 2719:2002), qui a fait l’objet d’une révision
technique.
Les principales mises à jour techniques sont les suivantes:
a) introduction d'une méthode C pour les produits d'esters méthyliques d'acides gras (EMAG),
b) révision des exigences en matière de dispositifs de mesure de la température, autorisant l'emploi
de thermomètres contenant du mercure,
c) suppression de l'Annexe D de l'édition d'origine sur l'adaptateur pour thermomètre à échelle basse,
celui-ci étant facultatif lorsqu'une bague est fixée au thermomètre en permanence,
d) révision des méthodes d'échantillonnage et de manutention des échantillons, et
er
e) inclusion, pour les appareils automatisés, fabriqués après le 1 janvier 2017, d'un dispositif de
fourniture automatique d'un gaz inerte sur le vase d'essai en cas de feu dans le vase d'essai.
iv © ISO 2016 – Tous droits réservés
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ISO 2719:2016(F)
Introduction
Les valeurs de points d'éclair sont utilisées pour le transport, le stockage, la manutention et la
réglementation de sécurité, comme caractéristique de classification pour définir les produits
«inflammables» et «combustibles». Une définition précise des différentes classes est donnée dans
chaque réglementation particulière.
Une valeur de point d'éclair peut indiquer la présence de produits hautement volatils dans un produit
relativement non volatil ou ininflammable. L'essai de point d'éclair peut donc constituer une étape
préliminaire dans l'étude de la composition de produits inconnus.
Il n'est pas approprié d'effectuer une détermination de point d'éclair sur des produits potentiellement
instables, décomposables ou explosifs, sauf s'il a préalablement été établi que le chauffage de la quantité
spécifiée de tels produits en contact avec les éléments métalliques de l'appareil de point d'éclair, dans la
plage de température requise par la méthode, n'induira pas de décomposition, d'explosion ou tout autre
effet néfaste.
Les valeurs de points d'éclair ne constituent pas une propriété physico-chimique constante des produits
soumis à essai. Elles sont fonction de la conception de l’appareil, des conditions de son utilisation, et du
mode opératoire mis en œuvre. C’est pourquoi un point d’éclair ne peut être défini que par rapport à
une méthode d’essai normalisée, et il n’est pas possible d’établir une corrélation générale valable entre
les résultats obtenus par des méthodes d’essai différentes ou avec des appareils autres que ceux qui
sont spécifiés.
[6] [12]
L'ISO/TR 29662 (CEN/TR 15138 ) donne des conseils utiles concernant la réalisation des essais de
point d'éclair et l'interprétation des résultats.
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NORME INTERNATIONALE ISO 2719:2016(F)
Détermination du point d'éclair — Méthode Pensky-
Martens en vase clos
ATTENTION — L'utilisation de la présente Norme internationale peut impliquer la mise en
œuvre de produits, d'opérations et d'équipements à caractère dangereux. La présente Norme
internationale n'est pas censée aborder tous les problèmes de sécurité concernés par son usage.
Il est de la responsabilité des utilisateurs de la présente Norme internationale de prendre les
mesures appropriées pour assurer la sécurité et préserver la santé du personnel avant son
application.
1 Domaine d'application
La présente Norme internationale décrit trois méthodes, A, B, et C, pour la détermination du point d'éclair
des liquides combustibles, des liquides contenant des matières solides en suspension, des liquides ayant
tendance à former un film en surface dans les conditions d'essai, des biocarburants et d'autres liquides,
au moyen de l'appareil d'essai Pensky-Martens en vase clos, dans la plage de température entre 40 °C
et 370 °C.
ATTENTION — Pour certains mélanges, aucun point d'éclair, tel que défini, n'est observé; à la
place, il peut y avoir un élargissement significatif de la flamme d'essai (pas de phénomène de
halo) et un changement de couleur de la flamme passant du bleu à l'orange jaunâtre. Le maintien
du chauffage peut faire qu'une quantité significative de vapeurs soit brûlée à l'extérieur du vase
d'essai, ce qui peut constituer un danger d'incendie.
NOTE 1 Techniquement les kérosènes ayant un point d'éclair supérieur à 40 °C peuvent être soumis à essai
selon la présente Norme internationale. Cependant, il est d'usage courant de déterminer le point d'éclair des
[5]
kérosènes selon l'ISO 13736 . De façon analogue, les huiles lubrifiantes sont normalement soumises à essai
[2]
suivant l'ISO 2592 .
La Méthode A est applicable aux distillats de pétrole (carburant diesel, mélanges de biocarburant, fioul
domestique et turbocombustibles), aux huiles lubrifiantes neuves et en service, aux peintures et vernis,
et à d'autres liquides homogènes ne faisant pas partie du champ d'application des Méthodes B ou C.
La Méthode B est applicable aux combustibles résiduels, aux résidus de bitumes fluidifiés, aux huiles
lubrifiantes usagées, aux mélanges de liquides contenant des matières solides, aux liquides ayant
tendance à former un film en surface dans les conditions d'essai ou ayant une viscosité cinématique
telle qu'ils ne sont pas chauffés de manière uniforme sous agitation et dans les conditions de chauffage
de la Méthode A.
La Méthode C est applicable aux esters méthyliques d'acides gras (EMAG) tels que définis dans des
[11] [13]
spécifications telles que l'EN 14214 ou l'ASTM D 6751 .
La présente Norme internationale n'est pas applicable aux peintures et vernis renfermant de l'eau.
[3]
NOTE 2 Le point d'éclair des peintures et vernis renfermant de l'eau peut être déterminé suivant l'ISO 3679 .
Les liquides contenant des traces de produits hautement volatils peuvent être analysés conformément à
[1]
l'ISO 1523 ou l'ISO 3679.
2 Références normatives
Les documents suivants cités dans le texte constituent, pour tout ou partie de leur contenu, des
exigences du présent document. Pour les références datées, seule l’édition citée s’applique. Pour les
références non datées, la dernière édition du document de référence s'applique (y compris les éventuels
amendements).
© ISO 2016 – Tous droits réservés 1
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ISO 2719:2016(F)
ISO 1513, Peintures et vernis — Examen et préparation des échantillons pour essai
ISO 3170, Produits pétroliers liquides — Échantillonnage manuel
ISO 3171, Produits pétroliers liquides — Échantillonnage automatique en oléoduc
ISO 15528, Peintures, vernis et matières premières pour peintures et vernis — Échantillonnage
3 Termes et définitions
Pour les besoins du présent document, les termes et définitions suivants s'appliquent.
3.1
point d’éclair
température la plus basse de la prise d'essai, corrigée à la pression barométrique standard de 101,3 kPa,
à laquelle l'application d'une source d'inflammation provoque l'inflammation des vapeurs émises par
la prise d'essai avec propagation de la flamme sur toute l'étendue de la surface du liquide, dans les
conditions d'essai spécifiées
4 Principe
La prise d'essai est placée dans le vase d'un appareil Pensky-Martens, puis chauffée de manière à
produire un accroissement constant de sa température, ceci sous agitation continue. Une source
d'inflammation est dirigée à travers une ouverture du couvercle du vase d'essai à des intervalles de
température réguliers avec interruption simultanée de l'agitation. La température la plus basse à
laquelle l'application de la source d'inflammation provoque l'inflammation des vapeurs émises par la
prise d'essai avec propagation de la flamme sur toute l'étendue de la surface du liquide est notée comme
étant le point d'éclair à la pression barométrique ambiante. Cette température est corrigée à la pression
atmosphérique normale au moyen d'une équation.
5 Produits chimiques et matériaux
5.1 Solvant de nettoyage, pour débarrasser le vase et le couvercle de toute trace d'échantillon
Le solvant utilisé sera choisi en fonction de la nature du produit ayant été soumis à essai précédent
et de la ténacité du résidu. Des solvants aromatiques peu volatils (exempts de benzène) peuvent être
utilisés pour enlever des traces d'huile, et un mélange de solvants tel que toluène-acétone-méthanol
peut être efficace pour éliminer des dépôts du type gomme.
5.2 Liquides de vérification, voir l’Annexe A.
6 Appareillage
6.1 Appareil de point d'éclair, tel que décrit dans l’Annexe B.
Lorsqu'un équipement automatisé est utilisé, s'assurer que le vase d'essai et l'ensemble couvercle sont
conformes aux dimensions clés données à l'Annexe B, et que le mode opératoire décrit à l'Article 10 est
respecté. L'utilisateur doit s'assurer que toutes les instructions du fabricant relatives au réglage et à la
mise en œuvre de l'appareil sont respectées.
NOTE Dans certaines conditions, les sources d'inflammation électriques peuvent donner des résultats
différents de ceux obtenus avec une flamme.
En cas de litige, à moins qu'il n'en soit décidé autrement, le point d'éclair déterminé avec une flamme
comme source d'inflammation doit être considéré comme la méthode de référence.
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ISO 2719:2016(F)
6.2 Dispositifs de mesure de la température, satisfaisant aux exigences de précision et dont la
réponse est telle que spécifiée à l'Annexe C.
6.3 Baromètre, à lecture de pression absolue, d'une précision de ±0,5 kPa et ayant une résolution
de 0,1 kPa.
Ne pas utiliser de baromètres précorrigés pour donner directement la pression régnant au niveau de la
mer, tels que ceux employés dans les stations météorologiques et les aéroports.
NOTE Certains appareils automatisés incluent un baromètre intégré qui mesure et enregistre
automatiquement la pression barométrique absolue, et réalise les corrections requises pour le point d'éclair
détecté.
6.4 Bain chauffant ou étuve, pouvant réguler la température à ±5 °C, pour réchauffer l'échantillon si
nécessaire.
L'étuve doit être ventilée et construite de telle manière qu'elle ne pourra être la cause de l'ignition de
toutes vapeurs inflammables qui peuvent être produites quand l'échantillon est chauffé.
Il est recommandé d'utiliser une étuve antidéflagrante.
7 Préparation de l’appareil
7.1 Généralités
Suivre les instructions du fabricant pour une configuration, un étalonnage, une vérification (7.5) et une
mise en œuvre corrects de l'appareil avec baromètre intégré (le cas échéant) et dispositif de mesure de
la température (voir Annexe C), en particulier pour la mise en œuvre et la configuration de la source
d'inflammation.
7.2 Emplacement de l'appareil
Installer l'appareil (6.1) sur une surface stable et à niveau, située dans un local exempt de courants d'air.
NOTE Lorsque les courants d'air ne peuvent être évités, il est recommandé d'entourer l'appareil d'un écran
de protection.
L'appareil peut être placé sous une hotte de laboratoire dotée d'une régulation individuelle de débit
d'air, réglée de sorte que les vapeurs émises puissent être extraites sans provoquer de courants d'air
autour du vase d'essai pendant l'essai.
7.3 Nettoyage du vase d'essai
Nettoyer le vase d'essai, le couvercle et ses accessoires avec un solvant approprié (5.1) pour enlever
toute trace de gomme ou de résidu subsistant d'un essai précédent. Sécher sous un courant d'air propre
jusqu'à élimination complète du solvant utilisé.
7.4 Assemblage de l'appareil
Vérifier que le vase d'essai, le couvercle et les autres parties ne présentent aucun signe de détérioration
et qu'ils sont exempts de dépôts. Assembler l'appareil conformément à l'Annexe B.
7.5 Vérification de l'appareil
7.5.1 Vérifier le fonctionnement correct de l'appareil au moins une fois par an, en effectuant un essai
sur un matériau de référence certifié (MRC) (5.2). Le résultat obtenu doit être égal ou inférieur à R2
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ISO 2719:2016(F)
de la valeur certifiée du MRC, où R est la reproductibilité de la méthode telle que présentée dans le
Tableau 4.
Utiliser la reproductibilité de la Méthode A (Tableau 4) pour calculer la tolérance de vérification
applicable aux matériaux de vérification certifiés pour les Méthodes A, B ou C.
Il est recommandé d'effectuer des vérifications plus fréquentes à l'aide d'étalons de travail secondaires
(ETS) (5.2).
L'Annexe A décrit une méthode recommandée pour effectuer la vérification des appareils à l'aide de
MRC et d'ETS, et pour préparer des ETS.
7.5.2 Les valeurs numériques obtenues lors de la vérification ne doivent pas être utilisées pour
établir un biais ni pour apporter une quelconque correction aux points d'éclair déterminés ensuite avec
l'appareil.
8 Échantillonnage
8.1 Sauf indication contraire, prélever des échantillons pour analyse représentatifs conformément aux
méthodes données dans l'ISO 3170, l'ISO 3171, l'ISO 15528 ou dans une norme nationale équivalente.
8.2 Lors de l'échantillonnage d'un combustible contenant des résidus, le récipient d'échantillon doit
être rempli entre 85 % et 95 % de sa capacité. Pour les échantillons d'EMAG, il est recommandé d'utiliser
un récipient classique d'un litre et de le remplir à 85 % de sa capacité. Pour les échantillons d'un autre
type, le volume du récipient doit être choisi avant de prélever toute partie aliquote d'échantillon de
manière à ne jamais dépasser les 85 % de sa capacité et à toujours dépasser les 50 % de sa capacité.
8.3 Si aucune précaution n'est prise pour éviter la perte de produits volatils, les points d'éclair peuvent
être anormalement élevés. Pour prévenir toute perte de produit volatil ou toute éventuelle introduction
d'humidité, ne pas ouvrir inutilement les récipients. Éviter de stocker les échantillons à des températures
supérieures à 30 °C. Pour les échantillons destinés à être stockés, vérifier que le récipient d'échantillon est
soigneusement fermé et qu’il ne fuit pas. Ne pas faire de transfert sauf si la température de l'échantillon
est inférieure d'au moins 18 °C à celle du point d'éclair présumé.
8.4 Ne pas conserver les échantillons dans des récipients perméables aux gaz, car les produits volatils
pourraient se diffuser au travers de leurs parois. Les échantillons placés dans des récipients non étanches
sont douteux et ne sont pas une source de résultats valides.
9 Manutention des échantillons
9.1 Produits pétroliers
9.1.1 Sous-échantillonnage
9.1.1.1 Sous-échantillonner à une température inférieure d'au moins 18 °C à celle du point d'éclair
présumé.
9.1.1.2 Plusieurs prises d'essai peuvent être successivement prélevées à partir du même récipient
d'échantillon. Des essais effectués plusieurs fois ont montré que les limites de fidélité de la méthode
étaient respectées lorsque la deuxième prise d'essai était prélevée dans un récipient d'échantillon rempli
au moins à 50 % de sa capacité
IMPORTANT — Les résultats des déterminations de point d’éclair peuvent être altérés si le
volume d’échantillon est inférieur à la moitié de la capacité du récipient.
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ISO 2719:2016(F)
9.1.2 Échantillons contenant de l'eau libre
9.1.2.1 Les résultats de point d'éclair peuvent être affectés par la présence d'eau. Si l'échantillon
contient de l'eau libre, laisser décanter une partie aliquote exempte d’eau avant de la mélanger.
9.1.2.2 Dans le cas de certains combustibles et lubrifiants, l'eau libre ne se décante pas toujours
facilement. Dans de tels cas, procéder à une séparation de l'eau par un procédé physique avant de
[3]
mélanger l'échantillon ou, si cela n'est pas possible, analyser le produit selon l'ISO 3679 .
9.1.3 Échantillons liquides à température ambiante
Avant de prélever la prise d'essai, mélanger l'échantillon en le secouant doucement à la main, et en
prenant soin de minimiser les pertes de composés volatils, puis poursuivre conformément à l'Article 10.
9.1.4 Échantillons hautement visqueux, semi-solides ou solides à température ambiante
Les échantillons doivent être chauffés pendant 30 min dans leur récipient (dont le couvercle/bouchon
aura été préalablement légèrement desserré pour éviter l'accumulation dangereuse de pression) à
la plus basse température permettant la liquéfaction des matières solides, ne dépassant pas le point
d'éclair présumé diminué de 18 °C. Si au terme de cette période, l'échantillon n'est pas complètement
liquide, prolonger la durée du chauffage par tranches de 30 min supplémentaires jusqu'à liquéfaction
complète. Ensuite agiter doucement l'échantillon pour l'homogénéiser, par exemple en agitant le
récipient de manière à décrire des orbites horizontales, avant de le transférer dans le vase d'essai.
Aucun échantillon ne doit être chauffé et transféré sauf si sa température est inférieure de plus de 18 °C
à son point d'éclair présumé.
IMPORTANT — Les vapeurs de produits volatils peuvent s'échapper au cours du chauffage si le
couvercle/bouchon du récipient est trop desserré.
9.2 Peintures et vernis
Préparer les échantillons conformément à l'ISO 1513.
10 Mode opératoire
10.1 Généralités
10.1.1 L'applicabilité des trois méthodes A, B et C est précisée dans l’Article 1.
Une détection électronique des points d'éclair doit être utilisée pour le mode opératoire C, car il est
difficile d'observer un éclair par de simples moyens visuels; ce moyen de détection peut également être
utilisé pour les procédures A et B.
10.1.2 Il convient de prendre garde lorsque sont soumis à essai des échantillons de combustibles
résiduels contenant une quantité d'eau significative, car le chauffage de ces produits peut occasionner
une formation de mousse et un débordement hors du vase d'essai.
10.1.3 À titre de mesure de sécurité, il est vivement recommandé d'appliquer la source d'inflammation
à la prise d'essai dans le vase avant de chauffer le vase d'essai et la prise d'essai, de sorte à vérifier
l'éventuelle présence de produits volatils non attendus.
10.1.4 À titre de mesure de sécurité, il est vivement recommandé pour un point d'éclair présumé
supérieur
...
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