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

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.

Charakterisierung von Abfällen - Anleitung zur Prüfung des Flammpunkts

Caractérisation des déchets - Lignes directrices pour la détermination du point d'éclair

L’essai de détermination du point d’éclair peut être brièvement défini comme un processus consistant à introduire une prise d’essai dans un vase d’essai à température contrôlée et à appliquer une source d’inflammation au contact des vapeurs dégagées par la prise d’essai, afin de déterminer si le mélange vapeur/air est inflammable ou la température à laquelle il est inflammable.
Le présent document n’est pas destiné à être un manuel explicatif traitant des méthodes de détermination du point d’éclair et de l’interprétation des résultats ; il couvre néanmoins les aspects fondamentaux relatifs à ces sujets.

Preskusne metode za karakterizacijo trdnih matriksov z vidika okolja - Vodilo za preskušanje plamenišča

Preskušanje plamenišča je mogoče povzeti kot postopek, pri katerem se preskusni del vstavi v preskusno posodo z nadzorovano temperaturo in se vir vžiga prenese na hlape, ki jih proizvaja preskusni del, da se ugotovi, ali je zmes hlapi/zrak vnetljiva oziroma pri kateri temperaturi se mešanica hlapi/zrak vname.
Ta dokument ni celovit priročnik o preskušanju plamenišča in razlagi rezultatov preskušanja, vendar zajema ključne vidike teh tem.

General Information

Status
Published
Public Enquiry End Date
04-Oct-2018
Publication Date
06-Jun-2019
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
31-May-2019
Due Date
05-Aug-2019
Completion Date
07-Jun-2019

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SLOVENSKI STANDARD
SIST-TP CEN/TR 17309:2019
01-julij-2019
Preskusne metode za karakterizacijo trdnih matriksov z vidika okolja - Vodilo za
preskušanje plamenišča

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: CEN/TR 17309:2019
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
SIST-TP CEN/TR 17309:2019 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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CEN/TR 17309
TECHNICAL REPORT
RAPPORT TECHNIQUE
May 2019
TECHNISCHER BERICHT
ICS 13.220.40; 13.030.01
English Version
Test methods for environmental characterization of solid
matrices - Guide to flash point testing

Caractérisation des déchets - Lignes directrices pour la Prüfverfahren für die umweltbezogene

détermination du point d'éclair Charakterisierung fester Matrices - Anleitung zur

Prüfung des Flammpunkts

This Technical Report was approved by CEN on 19 November 2018. 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.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 17309:2019 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 ...................................................................................................................................................... 6

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 .......................................................................................................................................................... 15

Annex A (normative) Major test methods used in specifications and regulations ............................ 16

Annex B (informative) Verification of apparatus .......................................................................................... 17

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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 .................................................................................................................................................. 19

Bibliography ................................................................................................................................................................. 20

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European foreword

This document (CEN/TR 17309:2019) 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.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

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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
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.

5 Brief history

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

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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.

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.
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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.

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’.

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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.

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.

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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 tolerances, by ensuring all key parts are clean and

function correctly and by testing using a reference material.

Incorrect dimensions, faulty ignitors, and the use of incorrect heating media and incorrect heating rates

or stirring speeds may affect test results.
Using instruments that are damaged, dirty or contam
...

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