prEN ISO 3679

Determination of flash point - Method for flash no-flash and flash point by small scale closed cup tester (ISO/DIS 3679:2022)

This document describes three procedures (A, B and C) covering determinations of flash no-flash and flash point.
Rapid equilibrium procedures A and B are applicable to flash no-flash and flash point tests of paints, including water-borne paints, varnishes, binders for paints and varnishes, adhesives, solvents, petroleum products including aviation turbine, diesel and kerosene fuels, fatty acid methyl esters and related products over the temperature range –30 °C to 300 °C. The rapid equilibrium procedures are used to determine whether a product will or will not flash at a specified temperature (flash no-flash procedure A) or the flash point of a sample (procedure B). When used in conjunction with the flash detector (A.1.6), this document is also suitable to determine the flash point of fatty acid methyl esters (FAME). The validity of the precision is given in Table 2.
Non-equilibrium procedure C is applicable to petroleum products including aviation turbine, diesel and kerosine fuels, and related petroleum products, over the temperature range –20 °C to 300 °C. The non-equilibrium procedure is automated to determine the flash point. Precision has been determined over the range 40 °C to 135 °C.
For specifications and regulations, procedures A or B are routinely used (see 10.1.1).

Bestimmung des Flammpunkts - Verfahren zur Bestimmung des Flammpunkts und des Nicht-Flammpunkts mit einem kleinen geschlossenen Tiegelprüfgerät (ISO/DIS 3679:2022)

Détermination du point d'éclair - Détermination de l'éclair de type passe / ne passe pas et méthode du point d'éclair en vase clos à petite échelle (ISO/DIS 3679:2022)

Določanje plamenišča - Metoda pojavnosti plamena in plamenišča v zaprti posodi z majhno prostornino (ISO/DIS 3679:2022)

General Information

• Status: Not Published
• ICS: 75.080 - Petroleum products in general
• ICS: 75.180.10 - Exploratory, drilling and extraction equipment
• ICS: 87.040 - Paints and varnishes
• Technical Committee: CEN/TC 19 - Petroleum products, lubricants and related products
• Ref Project: oSIST prEN ISO 3679:2022 - Determination of flash point – Method for flash no-flash and flash point by small scale closed cup tester (ISO/DIS 3679:2022)

RELATIONS

• Revised: EN ISO 3679:2015 - Determination of flash no-flash and flash point - Rapid equilibrium closed cup method (ISO 3679:2015)
• Effective Date: 21-Jul-2021

Standards Content (sample)

SLOVENSKI STANDARD
oSIST prEN ISO 3679:2022
01-junij-2022
Določanje plamenišča - Metoda pojavnosti plamena in plamenišča v zaprti posodi
z majhno prostornino (ISO/DIS 3679:2022)

Determination of flash point – Method for flash no-flash and flash point by small scale

closed cup tester (ISO/DIS 3679:2022)
Bestimmung des Flammpunkts – Verfahren zur Bestimmung des Flammpunkts und des
Nicht-Flammpunkts mit einem kleinen geschlossenen Tiegelprüfgerät (ISO/DIS
3679:2022)

Détermination du point d'éclair – Détermination de l'éclair de type passe / ne passe pas

et méthode du point d'éclair en vase clos à petite échelle (ISO/DIS 3679:2022)
Ta slovenski standard je istoveten z: prEN ISO 3679
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
oSIST prEN ISO 3679:2022 en,fr,de

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

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oSIST prEN ISO 3679:2022
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oSIST prEN ISO 3679:2022
DRAFT INTERNATIONAL STANDARD
ISO/DIS 3679
ISO/TC 28 Secretariat: NEN
Voting begins on: Voting terminates on:
2022-03-30 2022-06-22
Determination of flash point – Method for flash no-flash
and flash point by small scale closed cup tester

Détermination du point d'éclair –Détermination de l'éclair de type passe / ne passe pas – Méthode rapide à

l'équilibre en vase clos
ICS: 87.040; 75.080
This document is circulated as received from the committee secretariat.
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
ISO/CEN PARALLEL PROCESSING
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
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 3679:2022(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 2022
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oSIST prEN ISO 3679:2022
ISO/DIS 3679:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022

All rights reserved. Unless otherwise specified, or required in the context of its implementation, 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 the requester.
ISO copyright office
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Phone: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
© ISO 2022 – All rights reserved
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Contents Page

Foreword ..........................................................................................................................................................................................................................................v

Introduction .............................................................................................................................................................................................................................. vi

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ..................................................................................................................................................................................... 1

3 Terms and definitions .................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 2

4.1 Rapid equilibrium Procedures A and B ............................................................................................................................ 2

4.2 Non-equilibrium Procedure C ................................................................................................................................................... 2

5 Reagents and materials ................................................................................................................................................................................ 3

6 Apparatus .................................................................................................................................................................................................................... 3

7 Preparation of apparatus ...........................................................................................................................................................................4

7.1 General ........................................................................................................................................................................................................... 4

7.2 Location of apparatus ....................................................................................................................................................................... 4

7.3 Cleaning of the test cup assembly and accessories ................................................................................................ 4

7.4 Apparatus verification ..................................................................................................................................................................... 4

8 Sampling ....................................................................................................................................................................................................................... 5

9 Sample handling ...................................................................................................................................................................................................5

9.1 Petroleum products and fatty acid methyl esters................................................................................................... 5

9.1.1 Subsampling ........................................................................................................................................................................... 5

9.1.2 Samples liquid at ambient temperature ........................................................................................................ 6

9.1.3 Samples solid or semi-solid at ambient temperature ........................................................................ 6

9.1.4 Samples containing dissolved or free water that is not part of the product ................ 6

9.2 Paints, varnishes, and related materials ......................................................................................................................... 6

10 Procedures ................................................................................................................................................................................................................. 6

10.1 General ........................................................................................................................................................................................................... 6

10.2 Procedure A — Flash no-flash test ....................................................................................................................................... 7

10.3 Procedure B — Flash point determination ................................................................................................................... 8

10.4 Procedure C — Flash point determination ................................................................................................................... 9

11 Calculation .................................................................................................................................................................................................................. 9

11.1 Conversion of barometric pressure reading ................................................................................................................ 9

11.2 Correction of the detected flash point............................................................................................................................... 9

12 Expression of results ....................................................................................................................................................................................10

13 Precision ....................................................................................................................................................................................................................10

13.1 General ........................................................................................................................................................................................................ 10

13.2 Repeatability, r..................................................................................................................................................................................... 10

13.3 Reproducibility, R .............................................................................................................................................................................. 11

13.4 Relative bias between the Procedure C and Procedure B ............................................................................. 11

14 Test report ...............................................................................................................................................................................................................12

Annex A (normative) Flash point apparatus ............................................................................................................................................13

Annex B (normative) Verification of apparatus ....................................................................................................................................18

Annex C (informative) The use of a cup insert .......................................................................................................................................22

Annex D (normative) Sub-ambient Procedures A and B testing for manual apparatus

without integral test cup cooling facilities ...........................................................................................................................23

Annex E (normative) Temperature measuring device specifications ..........................................................................24

Annex F (informative) Flash point values of chemicals ................................................................................................................25

iii
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Bibliography .............................................................................................................................................................................................................................26

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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 WTO principles in the Technical

Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information

The committee responsible for this document is ISO/TC 28, Petroleum products and lubricants, 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 fourth edition cancels and replaces ISO 3679:2015, which has been technically revised. The main

technical changes are:

— Introduction, title and scope change to present a more generic method description;

— Definitions revised;

— Revised verification clause and generic verification data for flash point methods annexed;

— Revised procedures to include new Procedure C;
— Revision of precision wording and inclusion of precision for Procedure C;
— Revision of Annex A on the apparatus description;
— Revision of Annex B on verification and made that procedure mandatory.
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Introduction

This document includes three procedures (A, B and C) covering determinations of flash no-flash and

flash point. Rapid equilibrium procedures A and B (see 3.1) enable the determination of the flash/no-

flash and flash point respectively. Non-equilibrium procedure (C) (see 3.5) uses automated test cup

temperature control for flash point determination.
[1] [2]

ISO 1516 and ISO 1523 are also closed cup equilibrium test methods that are to be considered when

selecting a method.

The apparatus specified in this document enables a similar test result to be determined using more

rapid procedures, A or B, and a smaller test portion (2 ml or 4 ml) than that required in ISO 1516 or

ISO 1523 respectively. In addition, the apparatus can be made portable to the extent of being suitable

[18]

for on-site testing in addition to its more normal use in laboratories. Collaborative work has shown

[20]

that results obtained by these methods are comparable. Procedure C is based on test methods IP 534

[16]
and ASTM D7236 .

The interpretation of flash point results obtained on solvent mixtures containing halogenated

[4]

hydrocarbons should be considered with caution, as these mixtures can give anomalous results .

A limited study has indicated that some water borne paints can give an elevated flash point when an

electric ignitor is used with ISO 3679.

Flash point is be 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.

The flash point indicates the presence of highly volatile material(s) in a relatively non-volatile or non-

flammable material and flash point testing is often used as 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.

The flash point is not a constant physical-chemical property of a material tested. It is 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.
[8]

ISO/TR 29662 gives useful advice in carrying out flash point tests and interpreting results.

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oSIST prEN ISO 3679:2022
DRAFT INTERNATIONAL STANDARD ISO/DIS 3679:2022(E)
Determination of flash point – Method for flash no-flash
and flash point by small scale closed cup tester

WARNING — The use of this document can involve hazardous materials, operations and

equipment. This document does not purport to address all of the safety problems associated with

its use. It is the responsibility of users of this document to take appropriate measures to ensure

the safety and health of personnel prior to the application of the standard, and to determine the

applicability of any other restrictions for this purpose.
1 Scope

This document describes three procedures (A, B and C) covering determinations of flash no-flash and

flash point.

Rapid equilibrium procedures A and B are applicable to flash no-flash and flash point tests of paints,

including water-borne paints, varnishes, binders for paints and varnishes, adhesives, solvents,

petroleum products including aviation turbine, diesel and kerosene fuels, fatty acid methyl esters and

related products over the temperature range –30 °C to 300 °C. The rapid equilibrium procedures are

used to determine whether a product will or will not flash at a specified temperature (flash no-flash

Procedure A) or the flash point of a sample (Procedure B). When used in conjunction with the flash

detector (A.1.6), this document is also suitable to determine the flash point of fatty acid methyl esters

(FAME). The validity of the precision is given in Table 2.

Non-equilibrium Procedure C is applicable to petroleum products including aviation turbine, diesel and

kerosine fuels, and related petroleum products, over the temperature range –20 °C to 300 °C. The non-

equilibrium procedure is automated to determine the flash point. Precision has been determined over

the range 40 °C to 135 °C.

For specifications and regulations Procedures A or B are routinely used (see 10.1).

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

3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
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3.1
equilibrium

in flash point test methods, the condition where the vapour above the test portion, and the test portion

are at the same temperature at the time the ignition source is applied.

Note 1 to entry: This condition may not be fully achieved in practice, since the temperature might not be uniform

throughout the test portion, and the test cover and shutter on the apparatus can be cooler or warmer.

Note 2 to entry: Examples of equilibrium test methods are ISO 3679 Procedures A and B, ISO 1516 and ISO 1523.

3.2
fatty acid methyl ester
FAME

fuel comprising mono-alkyl esters of long chain fatty acids derived from vegetable oil or animal fats,

designated B100 or biodiesel (100 %).
[12] [15]

Note 1 to entry: FAME is specified in specifications such as EN 14214 and ASTM D6751 .

3.3
flash no-flash

application of an ignition source at the specified temperature of the test portion, as measured in the

prescribed manner, adjusted to account for variations in atmospheric pressure from 101,3 kPa, to

determine whether the vapour of the test portion ignites and the flame propagates across the surface of

the liquid under the specified conditions of test.
3.4
flash point

lowest temperature of the test portion, adjusted to account for variations in atmospheric pressure from

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.

3.5
non-equilibrium

in flash point test methods, the condition where the vapour above the test portion and the test portion

are not in temperature equilibrium at the time that the ignition source is applied.

Note 1 to entry: This condition is primarily caused by the heating of the test portion at the constant prescribed

rate with the vapour temperature lagging behind the test portion temperature.
[24]

Note 2 to entry: Examples of non-equilibrium test methods are ISO 3679 Procedure C, ISO 2719 and

[25]
ISO 13736 .
4 Principle
4.1 Rapid equilibrium Procedures A and B

A 2 ml or 4 ml test portion is introduced into the test cup that is set and maintained at the required test

temperature. After a specific time, when the vapours and test portion are deemed to be in temperature

equilibrium, an ignition source is applied and a determination is made (Procedure A) as to whether

or not a flash occurred. In order to determine the actual flash point of the sample, further tests, with

fresh test portions at different test cup temperatures, are carried out (Procedure B) until the flash

point is determined. The temperature is adjusted to account for variation in atmospheric pressure from

101,3 kPa, using a formula.
4.2 Non-equilibrium Procedure C

A 2 ml test portion is introduced into the test cup that is set and maintained at the required start

temperature. The test cup is then heated at a ramp rate of 1,5 °C /min to 2,5 °C / min and the ignition

source is applied at 1 °C temperature intervals until a flash point is detected. The detected flash point

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temperature is adjusted to account for variation in atmospheric pressure from 101,3 kPa, using a

formula.
5 Reagents and materials

5.1 Cleaning solvent, for the 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 can be used to remove traces of oil, and mixed solvents can

be effective for the removal of gum-type deposits.

5.2 Reference materials, for flash point, certified reference materials (CRM) and/or secondary

working standards (SWS), as described in Annex B.

5.3 Gas for ignitor and pilot flame, not required if an electric ignitor is used. Butane, propane, coal

gas, or natural gas may be used.
6 Apparatus
6.1 Flash point apparatus, as specified in Annex A.

6.2 Barometer, absolute pressure reading, accurate to ±0,5 kPa. Barometers pre-corrected to give

sea level readings, such as those used at weather stations and airports, shall not be used.

6.3 Heating bath or oven (optional), for warming the sample, if required.

The bath and oven shall be suitable for use with volatile and flammable materials.

6.4 Cooling bath or freezer (optional), for cooling the samples, if required, and capable of cooling

the sample to 10 °C below the expected flash point.

The bath and freezer shall be suitable for use with volatile and flammable materials.

6.5 Draught shield (optional), if required to minimize draughts, a shield fitted at the back and on

two sides of the instrument.
6.6 Cup insert (optional), see Annex C.

For samples that are difficult to remove, a thin metal cup insert can be used but the precision has not

been determined.
6.7 Syringes

6.7.1 Syringe, capable of delivering 2,00 ml ± 0,05 ml and equipped with a nozzle suitable for the

required test temperature and apparatus.
To enable a 4 ml test portion to be used, this syringe can be used twice.

6.7.2 Syringe, capable of delivering 4,00 ml ± 0,10 ml and equipped with a nozzle suitable for the

required test temperature and apparatus.
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7 Preparation of apparatus
7.1 General

7.1.1 Select the appropriate instrument for the relevant Procedure and the expected flash point

temperature. Follow the manufacturer’s instructions for the correct set-up, verification (see 7.4) and

operation of the apparatus, especially the operation and setting of the ignition source.

7.1.1.1 Procedure C is automated and requires automated temperature ramp control; sub ambient

testing requires integrated cooling (see A.1.5).

7.1.2 The use of a cup insert (6.6) for potentially adherent materials is described in Annex C.

7.1.3 When testing FAME (Procedures A and B) use a 2 ml ± 0,05 ml test portion and a 60 s ± 2 s test

time, combined with an electronic thermal flash detector (see A.1.6).

7.1.4 For sub-ambient test temperatures use Annex D, unless the apparatus has integral test cup

cooling facilities.
7.2 Location of apparatus

Support the apparatus (Annex A) on a level and steady surface in a draught-free position.

A draught shield (6.5) is recommended to be used when protection from draughts is not available.

WARNING — When testing materials which can produce toxic vapours, the apparatus should be

located in a fume hood with an individual control of air flow, adjusted such that the vapours are

withdrawn without causing air currents around the test cup during the test.
7.3 Cleaning of the test cup assembly and accessories

Clean the test cup cover and its accessories with an appropriate solvent (5.1) to remove traces of gum or

residue from the previous test. Wipe dry to remove all traces of solvent.

Follow the manufacturer’s instructions for the care and servicing of the instrument, especially

regarding electronic ignitors and flash detectors which can be fragile.

A stream of clean dry air, such as compressed air, can be used to remove the last traces of solvent used.

The filler orifice can be cleaned using a suitable cleaning device such as a small brush.

7.4 Apparatus verification

7.4.1 Check the temperature measuring devices and barometer at least once a year to ensure that

they are in accordance with A.1.4, Annex E and 6.2 requirements respectively.

7.4.2 Ensure the correct operation of ignition sources, in accordance with the manufacturers’

instructions and this test method.

7.4.3 Verify the accuracy of the apparatus at least once a year by testing a certified reference material

(CRM) (5.2 and Annex B). It is recommended that more frequent verification checks are made using a

reference material (5.2 and Annex B).
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7.4.4 The result of a single test obtained for a reference material shall be equal to or less than R /√2

from the certified value of the CRM or from the accepted reference value (ARV) of the SWS, where R is

the reproducibility of the test procedure.

NOTE These reference materials (RM) and in-house quality control samples can also be used to monitor

[26]

stability and establish statistical control limits, in accordance with ISO 4259-4 or equivalent standard, if

required.

7.4.5 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.

7.4.6 If the instrument fails the verification test, it is recommended that the operator should follow

the manufacturers’ instructions and check the following,
...