SIST-TP CEN/TR 17309:2019

SLOVENSKI STANDARD
kSIST-TP FprCEN/TR 17309:2018
01-september-2018
[Not translated]
Test methods for environmental characterization of solid matrices - Guide to flash point
testing
Charakterisierung von Abfällen - Anleitung zur Prüfung des Flammpunkts
Caractérisation des déchets - Lignes directrices pour la détermination du point d'éclair
Ta slovenski standard je istoveten z: FprCEN/TR 17309
ICS:
13.030.01 Odpadki na splošno Wastes in general
13.220.40 Sposobnost vžiga in Ignitability and burning
obnašanje materialov in behaviour of materials and
proizvodov pri gorenju products
kSIST-TP FprCEN/TR 17309:2018 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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kSIST-TP FprCEN/TR 17309:2018


FINAL DRAFT
TECHNICAL REPORT
FprCEN/TR 17309
RAPPORT TECHNIQUE

TECHNISCHER BERICHT

July 2018
ICS 13.220.40; 13.030.01
English Version

Test methods for environmental characterization of solid
matrices - Guide to flash point testing



This draft Technical Report is submitted to CEN members for Vote. It has been drawn up by the Technical Committee CEN/TC
444.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.

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.

Warning : This document is not a Technical Report. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a Technical Report.


EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TR 17309:2018 E
worldwide for CEN national Members.

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Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 Outline . 6
5 Brief history . 7
6 Flash point, and sustained combustion and burning . 7
7 The need of flash point tests . 7
8 Selection of flash point method . 7
8.1 First considerations . 7
8.2 Open or closed cup . 8
8.3 Non-equilibrium, equilibrium and rapid equilibrium tests . 8
8.4 Flash point automation . 9
8.5 Correlation between methods . 9
8.6 Valid temperature ranges . 9
9 Testing environment . 10
10 Safety . 10
11 Calibration and verification . 10
11.1 General . 10
11.2 Calibration . 10
11.3 Verification . 10
12 Test samples . 11
12.1 Sample handling . 11
12.2 Samples containing volatile components . 11
12.3 Viscous, semi-solid and solid samples . 11
13 Apparatus . 12
13.1 Ignition sources . 12
13.2 Flash detection . 12
13.3 Stirring . 12
13.4 Temperature measurement . 13
13.5 Care of the instrument . 13
13.6 Sub ambient testing . 13
14 Flash point testing effects . 13
15 Test results . 14
15.1 Barometric pressure correction . 14
15.2 Expression and reporting of results . 14
15.3 Precision . 14
Annex A (normative) Major test methods used in specifications and regulations . 16
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Annex B (informative) Verification of apparatus . 17
B.1 General . 17
B.2 Verification check standards . 17
B.3 Procedure . 17
B.4 Evaluation of the test result . 18
B.4.1 General . 18
B.4.2 Single test . 18
B.4.3 Multiple tests . 18
Bibliography . 20

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European foreword
This document (FprCEN/TR 17309:2018) has been prepared by Technical Committee CEN/TC 444 “Test
methods for environmental characterization of solid matrices”, the secretariat of which is held by NEN.
This document is currently submitted to the Vote on TR.
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Introduction
Flash point values are used in transporting, 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. For products material safety data sheets provide further information
also for flash point, but e. g. material safety data sheets for waste do not exist.
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 material 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 material tested. They are a function
of the apparatus design, the condition of apparatus used, and no general valid correlation can be
guaranteed between results obtained by different test methods or with test apparatus different from that
specified.
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1 Scope
The flash point test can be summarised as a procedure where a test portion is introduced into a
temperature controlled test cup and an ignition source is applied to the vapours produced by the test
portion to determine if the vapour / air mixture is flammable or at what temperature the vapour / air
mixture is flammable.
This document is not intended to be a comprehensive manual on flash point tests and the interpretation
of test results, however it covers the key aspects on these subjects.
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.
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
4 Outline
There are many, slightly different, definitions of flash point, however the following definition is widely
used in standard test methods:
The flash point is the lowest temperature of the test portion, corrected to a barometric pressure of
101,3 kPa, at which the application of an ignition source causes the vapour of the test portion to ignite
momentarily and the flame to propagate across the surface of the liquid under the specified test
conditions.
It is important to realise that the value of the flash point is not a physical constant but it is the result of a
flash point test and is dependent on the apparatus and procedure used. This fact is so important that a
general statement similar to the following will be incorporated into all the main flash point methods:
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 only be defined 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.
Due to the importance of flash point test results for both safety and regulatory purposes, the test method
identification should always be included with the test result.
In general specific products specifications indicate which standard test method should be employed.
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5 Brief history
th
The discovery of petroleum and the increased use of flammable distillates in the 19 century, for lighting
and heating in place of animal and vegetable oils, led to a large number of explosions and other fire related
accidents.
Legislation, such as the UK Petroleum Act in 1862 and the German Petroleum Regulations in 1882, quickly
spread around the world and led to the development of many types of test instruments. The following list
shows the dates when the major surviving instruments were in a form probably recognisable today:
— 1870 – 1880 Abel closed cup, Pensky-Martens closed cup
— 1910 – 1920 Tag closed cup, Cleveland open cup
6 Flash point, and sustained combustion and burning
The flash point is essentially the lowest temperature of the liquid or semi-solid at which vapours from a
test portion combine with air to give a flammable mixture and ‘flash’ when an ignition source is applied.
Sustained combustion and burning tests are usually carried out with the test portion at a fixed
temperature and tests whether vapour combustion and burning commences when an ignition source is
applied and thereafter is continuous and where the heat produced is self sustaining and supplies enough
vapours to combine with air and burn even after the removal of the ignition source.
7 The need of flash point tests
The fundamental reason for the requirement of flash point measurements is to assess the safety hazard
of a liquid or semi-solid with regard to its flammability and then classify the liquid into a group. The lower
the flash point temperature the greater the risk. This classification is then used to warn of a risk and to
enable the correct precautions to be taken when using, storing or transporting the liquid.
Specifications quote flash point values for quality control purposes as well as for controlling the
flammability risk.
A change in flash point may indicate the presence of potentially dangerous volatile contaminants or the
adulteration of one product by another.
8 Selection of flash point method
8.1 First considerations
Firstly, if a flash point method has been specified in a product specification or regulation, then that
method should be the first choice. If a number of alternative methods are specified then the choice will
be influenced by availability and other factors such as sample size requirements, speed of testing or
precision. In certain circumstances the choice of the stated referee method may be of special importance.
Annex A gives an overview of the most common methods and their use in specifications and regulations.
When testing specifically for contamination or contaminants, certain test methods and procedures are
more appropriate than others. In general an equilibrium test method is recommended for testing samples
that may contain traces of volatile contaminants.
When selecting a flash point method for incorporation into a product specification or regulation, it is
important that the product type is included in the scope of the test method and that the temperature
range of the product is covered by the test method. If the product is not included in the scope then the
test may be unsuitable for the product or the quoted precision does not apply. Where the scope of a test
method is general or not suitable it is recommended to contact an appropriate standardization body for
advice.
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When testing chemicals, mineral products or corrosive materials it is recommended to check that the test
cup material is suitable and will not produce flammable gases or be damaged by any possible chemical
reaction.
NOTE For example alkaline liquids or samples with aluminium cause problems.
8.2 Open or closed cup
There are two general classes of flash point tests - open cup and closed cup:
The open cup was initially developed to assess the potential hazards of liquid spillage. In this test a test
portion is introduced into a cup that is open at the top. An ignition source is passed horizontally over the
surface of the liquid, while the cup and liquid are being heated, to test if the vapours "flash". If the test is
repeated at increasing test portion temperatures a point may be reached when the test portion continues
to burn without further application of the ignition source, this is the fire point. The precision of open cup
tests is somewhat poorer than closed cup tests as the vapours produced by heating the test portion are
free to escape to the atmosphere and are more affected by local conditions in the laboratory. When open
cup tests are made at temperatures above ambient the result is usually higher than a result from a closed
cup test due to the reduced concentration of vapours.
The closed cup test contains any vapours produced and essentially simulates the situation where a
potential source of ignition is accidentally introduced into a container. In this test a test portion is
introduced into a cup and a close fitting lid is fitted to the top of the cup. The cup and test portion is heated
and apertures are then opened in the lid to allow air into the cup and the ignition source to be dipped into
the vapours to test for a flash.
The closed cup test predominates in specifications and regulations due to its better precision and ability
to detect contaminants.
8.3 Non-equilibrium, equilibrium and rapid equilibrium tests
These three types of tests and associated instruments are characterised by the level of temperature
stabilisation of the test portion and resultant vapours, and by the test portion size and test time.
Test methods such as Pensky-Martens, Tag, Abel and Cleveland are referred to as non-equilibrium tests
as the test temperature of the test portion is increased during the test and the temperature of the vapours
is not the same (not in equilibrium) as the test portion temperature when the ignition source is dipped
at regular intervals into the cup. This type of test has the advantage that it produces a definitive flash
point result. Under normal circumstances the increasing temperature is not a problem, but when volatile
contaminants or components are present the short time between each dip of the ignition source,
combined with the rate of temperature increase, does not allow enough time for flammable vapours to
evolve and this may cause unreliable results. For this reason non-equilibrium tests with lower rates of
heating usually perform better than those using higher rates of heating, when volatile contaminants or
components are present in the test portion.
Equilibrium tests are preferred for liquids and semi-solids containing volatile components or
contaminants and for confirmatory purposes in regulations as the sample temperature is constant or is
increased at a very slow rate. This allows enough time for vapours to build up and for the vapours to be
in equilibrium with the test portion before the ignition source is dipped into the cup. The ignition source
is dipped in the cup at different test portion temperatures thus resulting in a measurement of a flash
point, or the ignition source is dipped only once to carry out a flash no flash test to check conformance
against specifications and flammability criteria. These equilibrium tests use any type of closed cup in a
liquid bath and limits the difference of temperature between the test portion and the liquid bath. The
liquid bath is specified because it gives a very even temperature distribution on the outside of the test
cup thus ensuring that hot spots are not present on the cup surface that could cause the localised increase
of flammable vapours and thus a low flash point. Unfortunately these procedures take a long time to
complete.
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Rapid equilibrium (small scale) tests are not primarily aimed to give the actual flash point of a test
portion. The test is a flash no flash test to determine if the test portion’s vapours flash at the test
temperature. This is useful for checking conformance against specifications and flammability criteria. The
test cup is heated to the test temperature, a small test portion is introduced into the cup, and when the
test portion is deemed to be at the test temperature, the ignition source is used to test for a ‘flash’. Actual
flash point temperature is determined by repeating the flash no flash test at different temperatures with
a new test portion. The constant temperature of the test cup ensures that the test portion cannot be
overheated and that there is a reasonable time for vapours to build up before the ignition source is
applied.
8.4 Flash point automation
For a manual flash point test the operator is in control throughout the test and ensures that the
temperature, stirring and ignition requirements are met throughout the test and determines when and if
a flash has occurred. Some semi-auto instruments may assist the operator in detecting a flash or
controlling the temperature, but the operator is in control. This is why manual tests are the referee in
cases of dispute.
Automated flash point testers conform to all the specified requirements of the manual test method such
as dimensions, heating rate and flash detection, however the electronics, software and mechanics mimic
the manual operations. This may significantly reduce operator time but this does have the disadvantage
that more frequent validation of tester operation is required as the instrument operates mainly
unattended and is more complex.
Automatic flash point testers are not based on a manual test and often only key dimensions and
parameters are defined in a test method written just for this instrument type. A unique type of test may
be advantageous to the user but the complexity of the tester makes it difficult for conformance to the test
method to be measured. More frequent validation of the tester parameters and operation is required.
Some automated and automatic instruments are available with carousels that allow a number of tests to
be carried out unattended. This is particularly advantageous where large numbers of samples are tested.
However, accurate and reliable measurements may be compromised if the sample temperature does not
meet the recommendations stated in the test method. This is especially relevant to samples that are
volatile or contain volatile contaminants.
In general automated instruments are accepted in test methods provided that the instrument shows
conformation to the method requirements, including precision.
8.5 Correlation between methods
It is well known that open cup tests usually give higher flash point results than closed cup tests for test
temperatures above ambient. Some specifications list equivalent flash point methods and sometimes
relative bias information for specific products. However flash point methods employ different apparatus,
heating and stirring rates, procedures and sample handling which have an effect on relative biases,
especially when the liquid is volatile, or volatile contaminants or components are present. It is therefore
not possible and not correct to claim correlation or a fixed relative bias between different test methods
for all test samples.
8.6 Valid temperature ranges
Flash point instruments often have a wider temperature range than the temperatures covered by the
precision of the test method. Temperatures outside those covered by the precision may result in different
precision or give unpredictable results. The temperature ranges covered by the precision are shown in
the test method; otherwise it may be necessary to consult the relevant standardisation body for advice.
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Test method procedures include information on the required temperature of the test portion when the
flash point test commences and usually defines a temperature band over which a result is valid. It is
important to follow the specified procedure as failure to do so may result in an incorrect measurement.
9 Testing environment
The flash point instrument should be located on a flat and stable platform. It is important to carry flash
point tests in a draught free area as draughts may affect the evolution of flammable vapours as well as
cooling or extinguishing the ignition source. If there are draughts then a draught screen is recommended.
It is good practice to carry out flash point tests under a fume hood; in these circumstances the airflow
should be kept to a minimum. Visual identification of a flash point may be enhanced by carrying out the
test in subdued lighting.
10 Safety
The handling of samples for flash point determinations should be in accordance with local health and
safety practices, as the sample could be flammable or toxic.
When handling samples close to a flash point instrument it should be remembered that the flash point
apparatus uses a heated hotplate and an ignition source.
Due to the nature of the test the use of safety glasses and the provision of a suitable local fire extinguisher
are strongly advised.
Provision should be made (such as a fume hood) to minimise the effects of any toxic or objectionable
vapours.
Where the product type is not known it is safer to test using a procedure that uses a smaller volume test
portion such as the rapid equilibrium test.
11 Calibration and verification
11.1 General
In general a calibration process leads to either an adjustment of the apparatus or the identification of a
correction to be applied to a result.
In general a verification process checks that the apparatus and test procedure gives a result that is within
the expected tolerances but no adjustment or corrections are made.
11.2 Calibration
The flash point instrument and its sensors are required to work in accordance with the tolerances stated
in the standard method of test. If a sensor such as the thermometer is within the requirement for accuracy
then calibration to a higher level of accuracy is not required. If the sensor is outside the specification it
shall either be replaced or calibrated.
Reference materials with a certified flash point are for verification purposes only; they shall not be used
to establish an offset, bias or any other form of correction.
11.3 Verification
Verification that an instrument conforms to a standard method of test is implemented by checking that
all the physical parameters are within allowable
...