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IP 170

INFORMATIVE NOTE

An Energy Institute European interlaboratory study, conforming to ISO 4259 requirements, has indicated that
the precision of this test method should be considered to be as follows:

Repeatability (r) = 1,4 °C


Reproducibility (R) = 3,2 °C

170.i.0
IP 170/09 ISO 13736 : 2008 BS EN ISO 13736 : 2008
BS 2000 : Part 170 : 2008

EUROPEAN STANDARD EN ISO 13736

NORME EUROPÉENNE

EUROPÄISCHE NORM September 2008

ICS 75.080 Supersedes EN ISO 13736:1997

English version

Determination of flash point — Abel closed-cup method


(ISO 13736:2008)

Détermination du pont d'éclair – Méthode Abel en vase Bestimmung des Flammpunktes – Verfahren mit
clos (ISO 13736:2008) geschlossenen Tiegel nach Abel (ISO 13736:2008)

This European Standard was approved by CEN on 16 August 2008.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions
for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and
bibliographical references concerning such national standards may be obtained on application to the CEN
Management Centre or to any CEN member.

This European Standard exists in three official versions (English, French, German). A version in any other
language made by translation under the responsibility of a CEN member into its own language and notified
to the CEN Management Centre has the same status as the official versions.

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

EUROPEAN COMMITTEE FOR STANDARDIZATION


COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2008 CEN All rights of exploitation in any form and by any means Ref. No. EN ISO 13736:2008 E
reserved worldwide for CEN national Members.

170.ii.1
FLASH POINT – ABEL CLOSED-CUP, IP 170

Foreword

This document (EN ISO 13736:2008) has been prepared by Technical Committee ISO/TC 28 "Petroleum
products and lubricants" in collaboration with Technical Committee CEN/TC 19 "Gaseous and liquid fuels,
lubricants and related products of petroleum, synthetic and biological origin", the secretariat of which is held
by NEN.

This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by March 2009, and conflicting national standards shall be withdrawn
at the latest by March 2009.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN ISO 13736:1997.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic,
Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden,
Switzerland and the United Kingdom.

Endorsement notice

The text of ISO 13736:2008 has been approved by CEN as a EN ISO 13736:2008 without any modification.

170.iii.2
FLASH POINT – ABEL CLOSED-CUP, IP 170

Contents Page

Foreword . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . v
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . vi
1 Scope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
2 Normative references . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
3 Term and definition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
4 Principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
5 Chemicals and materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
6 Apparatus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
7 Apparatus preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
8 Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
9 Sample handling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
10 Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
11 Calculation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
12 Expression of results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
13 Precision . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
14 Test report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
Annex A (normative) Abel flash-point apparatus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
Annex B (normative) Positioning and fixing of test cup and heating vessel thermometers into
thermometer collar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
Annex C (normative) Thermometer specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Annex D (informative) Apparatus verification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

170.iv.3
FLASH POINT – ABEL CLOSED-CUP, IP 170

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 13736 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants.

This second edition cancels and replaces the first edition (ISO 13736:1997), which has been technically
revised.

170.v.4
FLASH POINT – ABEL CLOSED-CUP, IP 170

Introduction

Flash-point values can 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.

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 that flash-point determinations 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 do 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.

ISO/TR 29662[6] (CEN/TR 15138[7]) gives useful advice in carrying out flash-point tests and interpreting
results.

170.vi.5
INTERNATIONAL STANDARD ISO 13736:2008(E)

Determination of flash point — Abel closed-cup method

CAUTION — The use of this International Standard can involve hazardous materials 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 a barometric pressure of 101,3 kPa, at which


application of a test flame causes the vapour of the
This International Standard specifies a method for test portion to ignite momentarily and the flame to
the determination of the closed-cup flash point of propagate across the surface of the liquid under the
combustible liquids having flash points between specified conditions of test
! 30,0 °C and 70,0 °C, inclusive. However, the
precision given for this method is only valid for flash 4 Principle
points in the range ! 5,0 °C to 66,5 °C.
4.1 General
This International Standard is not applicable to
water-borne paints, which can, however, be tested Since it is necessary to detect the presence of small
using ISO 3679[4]. proportions of highly volatile materials, this test
should be the first determination on a received
NOTE 1 - See 4.1 for the importance of this test to avoid sample to help avoid the loss of these volatile
loss of volatile materials. materials.

NOTE 2 - Liquids containing halogenated compounds can 4.2 Test principle


give anomalous results.
The test portion is placed in the test cup of an Abel
2 Normative references apparatus and heated to give a constant
temperature increase with continuous stirring. A
The following referenced documents are small test flame is directed through an opening in
indispensable for the application of this document. the test cup cover at regular temperature intervals
For dated references, only the edition cited applies. with simultaneous interruption of stirring. The
For undated references, the latest edition of the lowest temperature at which application of the test
referenced document (including any amendments) flame causes the vapour of the test portion to ignite
applies. and propagate over the surface of the liquid is
recorded as the flash point at the ambient
ISO 3170:2004, Petroleum liquids — Manual barometric pressure. The temperature is corrected to
sampling. standard atmospheric pressure using an equation.
Separate test procedures are defined for liquids with
ISO 3171:1988, Petroleum liquids — Automatic expected flash points between ! 30,0 °C and
pipeline sampling. 18,5 °C, inclusive, and between 19,0 °C and
70,0 °C, inclusive.
ISO 15528:2000, Paints, varnishes and raw
materials for paints and varnishes — Sampling. 5 Chemicals and materials

3 Terms and definitions 5.1 Cleaning solvent, for the removal of traces
of sample from the test cup and cover.
For the purposes of this document, the following
terms and definitions apply. NOTE - The choice of solvent depends on the previous
material tested and the tenacity of the residue.
3.1 Low-volatility aromatic (benzene-free) solvents can be
used to remove traces of oil, and mixed solvents can be
flash point
efficacious for the removal of gum-type deposits.
lowest temperature of the test portion, corrected to

170.1.6
FLASH POINT – ABEL CLOSED-CUP, IP 170

5.2 Coolant, ethanediol (ethylene glycol), Barometers pre-corrected to give sea-level readings,
glycerol or silicone oil (optional), for use in the such as those used at weather stations and airports,
cooling bath or in the Abel apparatus. shall not be used.

See 10.1.2. 6.6 Cooling bath, either liquid or metal block, or


a recirculating cooler.
5.3 Silicone lubricant (optional), to inhibit the
formation of ice crystals on the lid and shutter See 10.1.4 and 10.2.4.
mechanism when carrying out tests at temperatures
below 5,0 °C. 6.7 Test cup thermal insulating cover (optional),
to reduce the formation of ice crystals on the cup
See the Note to 10.1.6. and cover assembly during sub-ambient testing.

5.4 Verification liquids, as described in Annex D. See 10.1.5.

6 Apparatus 7 Apparatus preparation

6.1 Flash-point apparatus, as specified in Annex 7.1 Location of the apparatus


A.
Support the Abel apparatus (6.1) on a level and
If automated equipment is used, ensure that it has steady surface in a draught-free position.
been established that the results obtained are within
the precision of this International Standard, that the NOTE - When draughts cannot be avoided, it is good
test cup and cover assembly conform to the key practice to surround the apparatus with a shield.
dimensions specified in Annex A, and the procedure
described in Clause 10 is followed. The user shall DANGER – When testing materials that produce
ensure that all of the manufacturer’s instructions for toxic vapours, the apparatus should be located in a
adjusting and operating the instrument are followed. fume hood with an individual control of air flow,
adjusted such that the vapours can be withdrawn
6.2 Test cup thermometer, conforming to the without causing air currents around the test cup
specification given in Annex C. during the test.

It shall be fitted into a collar as described in Annex 7.2 Cleaning the test cup
B.
Wash the test cup with an appropriate solvent (5.1)
6.3 Heating vessel thermometer, conforming to to remove any traces of gum or residue remaining
the specification given in Annex C. from a previous test. Dry using a stream of clean air
to ensure complete removal of the solvent used.
It shall be fitted into a collar as described in Annex
B. 7.3 Apparatus examination

NOTE - Other types of temperature-measuring devices can Examine the test cup, the cover and other parts to
be used, provided that they meet the requirements for ensure that they are free from signs of damage and
accuracy and have the same response as the deposits. If any damage is found, either rectify or,
thermometers specified in Annex C. if this is not possible, obtain a replacement. If
deposits are found, remove them.
6.4 Timing device, use one of the following:
7.4 Apparatus verification
a) electric/electronic timing device, which can
indicate intervals of 1 s; 7.4.1 Verify the correct functioning of the
b) pendulum, of 610 mm effective length, apparatus at least once a year by testing a certified
counting one beat from one extremity of the reference material (CRM) (see 5.4 and Annex D).
swing to the other; The result obtained shall be equal to or less than
c) metronome, that beats at a frequency of 75 R 2 from the certified value of the CRM, where R
beats per minute to 80 beats per minute. is the reproducibility of the test. More frequent
verification checks shall be made using secondary
6.5 Barometer, accurate to 0,5 kPa. working standards (SWS).

170.2.7
FLASH POINT – ABEL CLOSED-CUP, IP 170

A recommended procedure for apparatus verification 9.4 Samples containing water as a separate
using CRMs and SWSs and for the production of phase
SWSs is given in Annex D.
If a sample contains water as a separate phase,
7.4.2 Do not use the numerical values obtained decant an aliquot from the water prior to mixing.
during the verification check to provide a bias
statement, or to make any correction to the flash Flash-point results can be affected by the presence
points subsequently determined using the apparatus. of water. For certain fuels, it might not always be
possible to decant the sample from the free water.
8 Sampling In such cases, the water should be separated from
the aliquot physically, prior to mixing, or, if this is
8.1 Obtain samples in accordance with the not possible, the material should be tested in
procedures given in ISO 3170, ISO 3171, ISO accordance with ISO 3679[4].
15528 unless otherwise agreed.
9.5 Sample mixing
8.2 Place sufficient sample volume for testing in
a tightly sealed container appropriate to the material Mix samples by gentle manual shaking prior to the
being sampled and, for safety purposes, ensure that removal of the test portion, taking care to minimise
the sample container is filled only to between 85 % the loss of volatile components, and proceed in
and 95 % of its capacity. accordance with Clause 10.

8.3 Store the samples in conditions that 10 Procedure


minimize vapour loss and pressure build-up. Avoid
storing the samples at temperatures in excess of 10.1 Liquids with expected flash points between
30,0 °C. ! 30,0 °C and 18,5 °C

9 Sample handling 10.1.1 Using a barometer (6.5), record the ambient


pressure in the vicinity of the apparatus at the time
9.1 Storage prior to testing of test.

If an aliquot of the original sample is stored prior to NOTE - It is not necessary to correct the barometric
pressure for ambient temperature, although some
testing, ensure that the container is filled to more
barometers are designed to make this correction
than 50 % of its capacity.
automatically.
NOTE - Results of flash-point determinations can be
affected if the sample volume falls below 50 % of the 10.1.2 Use either a mixture of equal volumes of
container’s capacity. ethanediol (5.2) and water, or glycerol (5.2) and
water, or silicone oil (5.2) to completely fill the
9.2 Liquids with expected flash points between heating vessel (Clause A.5) and to fill the inner air
! 30,0 °C and 18,5 °C chamber, which surrounds the test cup (Clause
A.2), to a depth of at least 38 mm.
9.2.1 Cool the sample to a temperature of ! 35
°C or to at least 17,0 °C below the expected flash 10.1.3 Insert the heating vessel thermometer (6.3).
point, whichever is the higher, before opening the
container. 10.1.4 Adjust the temperature of the heating vessel
(Clause A.5), using a cooling bath (6.6) connected
9.2.2 Cool the liquids that crystallize on cooling to via the funnel aperture and overflow pipe, to
just above their melting points. ! 35 °C or to at least 9,0 °C below the expected
flash point of the material being tested, whichever
9.3 Liquids with expected flash points between is the higher. Carry out a trial flash-point
19,0 °C and 70,0 °C determination if necessary.

Cool the sample to a temperature of 2 °C or to at 10.1.5 Loosely assemble the cover (Clause A.3) and
least 17,0 °C below the expected flash point, test cup (Clause A.2). Cover with the thermal
whichever is the higher, before opening the insulator (6.7), and cool the assembly to ! 35 °C or
container. to at least 17,0 °C below the expected flash point,
whichever is the higher.

170.3.8
FLASH POINT – ABEL CLOSED-CUP, IP 170

10.1.6 Ensure that neither cooling liquid nor vapour 10.1.12 Apply the test flame in this manner every
from the cooling bath, which could affect the flash 0,5 °C rise in temperature until a distinct flash
point of the product under test, enters the test cup. occurs in the interior of the test cup or until a
temperature corresponding to a corrected
NOTE - Cooling a cover or test cup that is wet with water temperature of 18,5 °C is reached. Record the
to below 0 °C can cause sticking due to ice (e.g. sticking temperature of the test portion when the flash
of the slide). Wiping the apparatus dry with a duster or a occurs.
piece of absorbent paper before cooling to below 0 °C is
usually sufficient to prevent icing, but, alternatively, icing
10.1.13 Do not confuse the true flash point with
can be minimized by the use of a thermal insulating cover
(6.7) and by lubricating the outer face of the lip of the the bluish halo that sometimes surrounds the test
test cup and the slide with a silicone lubricant (5.3). flame at applications preceding the actual flash
point.
10.1.7 Place the test cup in position in the
apparatus (see Clause A.3) and insert the test cup 10.1.14 Record as the observed flash point the
thermometer (6.2). Remove the cover and pour in temperature read on the test cup thermometer at
the test portion without undue agitation, avoiding as the time the test flame application caused a distinct
far as possible the formation of air bubbles, until the flash in the interior of the test cup.
level just reaches the point of the index gauge on
the wall of the test cup. Do not move the apparatus 10.2 Procedure for liquids flashing between
after filling. Place the cover on the test cup and 19,0 °C and 70,0 °C
push it down into position. Ignite the test flame,
adjust its size to conform to the size of the 10.2.1 Using the barometer (6.5), record the
reference bead mounted on the cover of the test ambient pressure of the laboratory at the time of
cup, and maintain it at that size throughout the test. test.

10.1.8 Apply heat to the heating vessel (Clause 10.2.2 Use water to completely fill the heating
A.5) in such a manner that the temperature of the vessel (Clause A.5) and to fill the inner air chamber,
test portion in the test cup rises at a rate of which surrounds the test cup (Clause A.2), to a
1 °C/min from the first application of the test flame depth of at least 38 mm.
to the end of the test.
10.2.3 Insert the heating vessel thermometer (6.3).
10.1.9 Using the stirrer (Clause A.4), stir the test
portion in a clockwise direction (i.e. to give a 10.2.4 Adjust the temperature of the liquid in the
downward thrust) at 30 r/min ± 5 r/min. Continue heating vessel, using either a cooling bath (6.6) or
stirring in a steady manner for the duration of the a heater (Clause A.6) to at least 9,0 °C below the
test but do not stir during the application of the test expected flash point of the material being tested, or
flame. to 10 °C, whichever is the higher. Carry out a trial
flash-point determination if necessary.
10.1.10 When the temperature of the test portion
reaches ! 35 °C or at least 9,0 °C below the 10.2.5 Loosely assemble the cover (see Clause A.3)
expected flash point, start the timing device (6.4), and test cup (see Clause A.2) and cool to 2 °C or to
apply the test flame by slowly and uniformly at least 17,0 °C below the expected flash point,
opening the slide in the cover while the timer beats whichever is the higher.
three times and closing it during the fourth beat. If
an electric/electronic timing device calibrated in 10.2.6 If a liquid cooling bath is used, ensure that
seconds is used, the application of the test flame neither cooling liquid nor vapour enters the test cup,
shall be made by slowly and uniformly opening the which can affect the flash point of the product
slide over a period of 2 s and then closing it over a under test.
period of 1 s.
10.2.7 Place the test cup in position in the
10.1.11 If a flash occurs, discontinue the test, apparatus (see Clause A.3). Remove the cover and
discard the test portion and proceed in accordance pour in the test portion without undue agitation,
with 10.1.3, commencing the test at a lower avoiding as far as possible the formation of air
expected flash-point temperature. If no flash occurs, bubbles, until the level just reaches the point of the
proceed in accordance with 10.1.12. If a flash index gauge on the wall of the test cup. Do not
occurs at a temperature below ! 30,0 °C, record move the apparatus after filling. Place the cover on
and report this fact and discontinue the test. the test cup and push it down into position. Ignite

170.4.9
FLASH POINT – ABEL CLOSED-CUP, IP 170

the test flame, adjust its size to conform to the size 11 Calculation
of the reference bead mounted on the cover of the
test cup, and maintain it at that size throughout the 11.1 If the barometric pressure reading, taken in
test. accordance with 10.1.1 or 10.2.1, is in a unit other
than kilopascals, convert to kilopascals using the
10.2.8 Apply heat to the heating vessel in such a following conversions, as appropriate:
manner that the temperature of the test portion in
the test cup rises at a rate of 1 °C/min from the Reading in hPa × 0,1 = kPa
first application of the test flame to the end of the Reading in mbar × 0,1 = kPa
test. Reading in mmHg × 0,133 322 = kPa

10.2.9 Using the stirrer (Clause A.4), stir in a NOTE - For the purposes of correcting flash-point values
clockwise direction (i.e. to give a downward thrust) to standard barometric pressure, it is not considered
at 30 r/min ± 5 r/min. When testing viscous necessary to correct the barometer readings for ambient
products, ensure that the stirring action does not temperature. However, some barometers are designed to
push the test portion above the filling mark. automatically correct the barometric pressure for ambient
Continue stirring in a steady manner for the duration temperature.
of the test but do not stir during the application of
the test flame. 11.2 Calculate the corrected flash point, Tc, using
Equation (1):
10.2.10 When the temperature of the test portion
reaches 10 °C or at least 9,0 °C below the Tc = To + 0,25(101,3 - p) (1)
expected flash point, start the timing device (6.4),
apply the test flame by slowly and uniformly where
opening the slide in the cover while the timer beats To is the observed flash point,
three times and closing it during the fourth beat. If expressed in degrees Celsius;
an electric/electronic timing device calibrated in p is the ambient barometric pressure,
seconds is used, the application of the test flame expressed in kilopascals.
shall be made by slowly and uniformly opening the
slide over a period of 2 s and then closing it over a NOTE - Equation (1) is strictly correct only within the
barometric pressure range from 98,0 kPa to 104,7 kPa.
period of 1 s.
For practical purposes, 4 kPa is equivalent to a
10.2.11 If a flash occurs, discontinue the test,
flash-point temperature change of 1 °C.
discard the test portion and proceed in accordance
with 10.1.4 or 10.2.4, as appropriate, commencing
the test at a lower expected flash-point 12 Expression of results
temperature. If no flash occurs, proceed in
accordance with 10.2.12. Report the flash point, corrected to standard
atmospheric pressure, rounded to the nearest
10.2.12 Apply the test flame in this manner every 0,5 °C.
0,5 °C rise in temperature until a flash point (3.1) is
detected, or until a temperature corresponding to a 13 Precision
corrected temperature of 70,0 °C is reached.
Record the temperature of the test portion when the 13.1 General
flash occurs.
The precision, as determined by statistical
10.2.13 Do not confuse the true flash point with examination of inter-laboratory test results, is given
the bluish halo that sometimes surrounds the test in 13.2 and 13.3, and applies over the range
flame or an enlarged flame at applications preceding ! 5,0 °C to 66,5 °C.
the actual flash point.
NOTE - The precision is being revised for both manual and
10.2.14 Record as the observed flash point the automated apparatus.
temperature read on the test cup thermometer at
the time the test flame application caused a distinct
flash in the interior of the test cup.

170.5.10
FLASH POINT – ABEL CLOSED-CUP, IP 170

13.2 Repeatability, r 14 Test report


The difference between two test results, obtained The test report shall contain at least the following
by the same operator with the same apparatus information:
under constant operating conditions on identical test
material, would in the long run, in the normal and a) a reference to this International Standard
correct operation of the test method, exceed the (ISO 13763:2008);
value in Equation (2) in only one case in 20:
b) the type and complete identification of the
r = 1,0 °C (2) sample tested;

13.3 Reproducibility, R c) the ambient barometric pressure in the


vicinity of the apparatus (see 10.1.1 and
The difference between two single and independent 10.2.1);
test results, obtained by different operators
operating in different laboratories on identical test d) the result of the test (see Clause 12);
material, would in the long run, in the normal and
correct operation of the test method, exceed the e) any deviation, by agreement or otherwise,
value in Equation (3) in only one case in 20: from the procedure specified;

R = 1,5 °C (3) f) the date of the test.

170.6.11
FLASH POINT – ABEL CLOSED-CUP, IP 170

Annex A
(normative)

Abel flash-point apparatus


A.1 Apparatus just completely opened, and at the inner extremity
of the movement of the slide, they are completely
The apparatus shall consist of a test cup, cover closed.
assembly and heating vessel as described below and
detailed in Figures A.1 and A.2. The trunnions supporting the test gas jet shall be
fixed to the top of the guides and the gas jet shall
NOTE - Automated apparatus that can have different be mounted in the trunnions so that it is free to
heating and cooling configurations can be used; however, oscillate. The test gas jet shall be arranged so that
the precision is still being evaluated for these alternative when the slide is moved to uncover the holes, the
configurations. oscillating test gas jet is caught by a pin fixed in the
slide and tilted over the central hole in such a way
A.2 Test cup that the lower edge of the cover bisects the circle
formed by the bore of the jet when in the lowest
The test cup shall be made of brass and conform to position. The flame shall then occupy a central
the form and dimensions shown in Figure A.1. position within the hole in both directions.

A gauge, consisting of a rod bent upwards and The thermometer socket shall be in the form of a
terminating in a point, shall be fixed within the test split tube, mounted on a diameter at right angles to
cup through the wall and silver-soldered or brazed the diameter through the centres of the holes, and
into place. fitted at such an angle as to bring the bulb of the
thermometer when in place, vertically below the
A.3 Test cup cover assembly centre of the cover and at the correct distance from
it.
The test cup shall be provided with a close-fitting
cover made of brass and conform to the form and A bush for the stirrer shall be mounted on the cover
dimensions shown in Figure A.1. A downwardly in a position diametrically opposite the thermometer
projecting rim barely reaching the flange on the test mounting. Its length and the angle at which it is set
cup shall either form part of the top or shall be shall be such that the stirrer rod clears the oil level
silver-soldered or brazed into place. gauge and the blades operate below the level of and
without fouling the thermometer bulb. The bush
Upon the cover shall be mounted a thermometer shall be placed as near as practicable to the outer
socket, a bush for the stirrer, trunnions to support edge of the cover.
a test gas jet, a pair of guides in which a slide
moves, and a bead or other reference mark to depict A.4 Stirrer
the required 3,6 mm to 4,1 mm size of the ignitor
flame. The top of the cover shall be pierced by three This shall be made of brass and conform to the form
rectangular holes symmetrically placed on a and dimensions given in Figure A.1.
diameter, one in the centre and the other two as
close as practicable to the inner sides of the rim and It shall consist of a round stem having four blades or
opposite each other. vanes silver-soldered in place at one end. The blades
of the stirrer shall be set so that the liquid is thrust
These three holes shall be covered or uncovered by in a downward direction when the stirrer is rotated
means of a slide moving in suitably disposed guides. clockwise.
The slide shall have two apertures, one
corresponding to the centre hole in the cover and A collar shall be fixed onto the stem so that when
the other to one of the holes at the side. The the stem is inserted into the stirrer bush from
movement of the slide shall be restricted by suitable below, it is arrested at a position such that the
stops, and its length and the disposition of the holes correct length protrudes into the test cup. The top
shall be such that, at the outer extremity of the end of the stem shall be reduced and screwed.
movement of the slide, the holes in the cover are

170.7.12
FLASH POINT – ABEL CLOSED-CUP, IP 170

A long sleeve having an internally screwed, knurled its flange rest upon, the ebonite or fibre ring so that
knob soldered to its upper end shall be passed over the test cup is centrally disposed within the heating
the upper end of the stem and screwed home. The vessel. The ebonite or fibre ring shall be secured in
length of the sleeve shall be such that a flat-faced place by means of six small screws having their
collar at its lower end just comes into contact with heads sunk below the surface of the ring to avoid
the upper end of the stirrer bush, leaving the stirrer metallic contact between the heating vessel and the
free to rotate without appreciable vertical play. test cup.

A flat-headed cylindrical plug shall be provided for A split socket, similar to that on the cover of the
insertion in the stirrer bush when the stirrer is not in test cup, but set vertically, shall allow a
use. thermometer to be inserted into the water-space. A
funnel and overflow pipe shall also be connected
A.5 Heating vessel with the water space through the top plate and two
loop handles provided thereon.
This shall be made of copper and conform to the
form and dimensions given in Figure A.2. It shall The heating vessel shall rest upon a cast-iron tripod
consist of two flat-bottomed, cylindrical copper stand, attached to the ring of which is a cylindrical
vessels (heating vessel and inner air chamber) copper jacket not less than 0,56 mm in thickness
placed coaxially one inside the other and soldered at flanged inwards at the top, and of such dimensions
their tops to a flat copper ring, greater in outside that the heating vessel, while resting firmly on the
diameter than the smaller vessel. Thus, the space iron ring, just touches with its outward projecting
between the two vessels shall be totally enclosed flange the inward-turned flange of the jacket. Two
and used as a water jacket. handles shall be provided on the outer jacket.

An ebonite or fibre ring of right-angled section shall A.6 Heating device


be fitted into the hole in the centre of the flat ring to
form the top of the heating vessel. When the Use any suitable device for heating the vessel, such
apparatus is in use, the test cup shall fit into, and as gas flame, electric heater or spirit lamp.

Dimensions in millimetres

a) Test cup b) Stirrer

Figure A.1 (continued)

170.8.13
FLASH POINT – ABEL CLOSED-CUP, IP 170

Dimensions in millimetres

c) Cover d) Thermometer collar

Key
1 thermometer socket
2 stirrer bush
a
Brazed or silver-soldered.
b
Inside diameter of sleeve is a sliding fit on stem.
c
This dimension is such that the stirrer rotates freely with no appreciable end play when assembled on cover.
d
All corners are rounded.
e
Close fit over test cup.
f
Push fit in thermometer socket on cover and heating vessel.
g
It is recommended that in order to achieve interchangeability, the internal diameter of the thermometer socket should
be between 15,235 mm and 15,253 mm and that the external diameter of the thermometer collar should be
between 15,222 mm and 15,232 mm.

NOTE - All items of the apparatus shown are made of brass.

Figure A.1: Abel flash-point apparatus – Test cup, cover, stirrer and thermometer collar

170.9.14
FLASH POINT – ABEL CLOSED-CUP, IP 170

Dimensions in millimetres

Key
1 ebonite or fibre ring, which fits easily on cup 9 heating vessel
2 funnel 10 outer jacket
3 test cup thermometer 11 slide 20 SWG 0,91 brass
4 heating vessel thermometer 12 gas jet or pilot light
5 ø 2,2 × 3,8 for long CSK screws 13 heating vessel thermometer
6 copper overflow pipe 14 guides
7 inner (air) chamber 15 white bead ø 3,6 mm to 4,1 mm of suitable material
8 stirrer 16 trunnions
a d
For actual position, see plan view. 0,6 copper.
b e
Inside diameter of thermometer socket 15 mm Length of jet is approximately 15 mm; the bore at the end
to 15,5 mm. of the jet is 1,71 mm maximum and 1,46 mm minimum.
c
2,5 mm maximum clearance in top plate.

Figure A.2: Abel flash-point apparatus – Assembly plus heating vessel

170.10.15
FLASH POINT – ABEL CLOSED-CUP, IP 170

Annex B
(normative)

Positioning and fixing of test cup and heating vessel thermometers


into thermometer collar
B.1 Thermometer B.2 Position

The collar shall be made of brass and shall have the Secure the thermometer in the collar in accordance
following dimensions: with Figure B.1, by means of either

a) outside diameter: push fit in socket; a) a mixture of plaster-of-Paris and glycerine, or

b) thickness of tube: 0,69 mm to 0,73 mm; b) an epoxy-resin-based commercial adhesive.

c) thickness of flange: 2,515 mm to 2,565 mm. NOTE - Automated equipment can use alternative
thermometer collars to enhance removal and fitting of the
thermometers.

Key
1 thermometer stem
2 glass swelling
3 brass collar
4 0,69 mm to 0,73 mm wall tube push fit in socket
a
Areas for application of adhesive.

Figure B.1: Position of thermometer stem in collar

170.11.16
FLASH POINT – ABEL CLOSED-CUP, IP 170

Annex C
(normative)

Thermometer specifications
C.1 Test cup thermometer C.2 Heating vessel thermometer

Specifications for the test cup thermometer are Specifications for the heating vessel thermometer
shown in Figure C.1. are shown in Figure C.1.

NOTE - The thermometer IP 74C (see BS 2000-0.1[8]) NOTE - The thermometer IP 75C (see BS 2000-0.1[8])
conforms to these requirements. conforms to these requirements.

See Table C.1 for description of symbols.

Figure C.1: Test cup and heating-vessel thermometers

170.12.17
FLASH POINT – ABEL CLOSED-CUP, IP 170

Table C.1: Thermometer specifications

Type of thermometer
Key symbol
Characteristic Abel test cup Abel heating vessel (Figure C.1)
(wide range) (wide range)
Temperature range, °C ! 35 to 70 ! 30 to 80 –
Immersion, mm 61 89 A
Scale marks, °C –
Subdivisions 0,5 0,5 –
Long lines at each 1 and 5 1 and 5 –
Numbers at each 5 5 –
Maximum line width, mm 0,15 0,15 –
Scale error, °C, max. 0,5 below 0 0,5 –
0,2 at and above 0
Expansion chamber Required Required –
Total length, mm 300 to 320 300 to 320 B
a
Stem OD , mm 6 to 7 6 to 7 C
Bulb length, mm 7,5 to 10,5 7,5 to 10,5 D
Bulb ODa, mm 4 to 6 4 to 6 E
Scale location: –
Bottom of bulb to line at, °C ! 35 ! 30 –
Distance, mm 70 to 80 100 to 110 F
Length of scale range, mm $ 195 $ 164 G
Swelling diameter, mm 9,5 to 10,5 9,5 to 10,5 I
Swelling depth, mm 3 to 5 3 to 5 J
Distance from base of swelling to 59,6 to 62,5 86,5 to 91,5 K
bottom of bulb, mm
NOTE The average temperature of the emergent stem is 21 °C over the entire range.
a
OD: Outer diameter

170.13.18
FLASH POINT – ABEL CLOSED-CUP, IP 170

Annex D
(informative)

Apparatus verification
D.1 General not exceeding 10 °C.

This annex describes a procedure for producing a D.3 Procedure


secondary working standard (SWS) and conducting
verification checks using a SWS and a certified D.3.1 Choose a CRM or SWS that falls within the
reference material (CRM). range of flash points to be determined with the
apparatus.
The performance of the apparatus (manual or
automated) should be verified on a regular basis See Table D.1 for approximate flash-point values.
using either a CRM produced in accordance with These are not the certified values nor the values
ISO Guide 34[2] and ISO Guide 35[3], or an in-house that should be obtained and are given only for
reference material/SWS prepared in accordance with guidance.
one of the procedures given in D.2.2. The
performance of the apparatus should be assessed A certified flash-point value shall be supplied with
with a consideration of the guidance given in each CRM or SWS.
ISO Guide 33[1] and ISO 4259[5].
It is recommended that two CRMs or SWSs be used
The evaluation of the test result assumes a 95 % in order to cover as wide a range as possible. In
confidence limit for the trueness of the result. addition, it is also recommended that replicate tests
be carried out on aliquots of the CRM or SWS.
D.2 Verification check standards
Table D.1: Approximate closed-cup flash points of
D.2.1 A certified reference material (CRM) is a hydrocarbons and other chemicals
stable single hydrocarbon or other stable substance
with a flash point determined in accordance with Substance Nominal flash point
ISO Guide 34[2] and ISO Guide 35[3], using a °C (approximate)
method-specific inter-laboratory study to produce a
method-specific certified value. 2,2,4-Trimethylpentane !9
(iso-octane)
D.2.2 A secondary working standard (SWS) is a Methylbenzene (toluene) 6
stable petroleum product or a single hydrocarbon or
other stable substance with a flash point determined Octane 14
by either
1,4-Dimethylbenzene 26
a) testing representative subsamples at least three Nonane 32
times using an instrument previously verified
using a CRM, statistically analysing the results Cyclohexanone 43
and, after the removal of any outliers,
Decane 49
calculating the arithmetic mean of the results,
or 1-Hexanol 60

b) conducting an inter-laboratory method-specific Undecane 63


test programme utilizing at least three
laboratories testing representative samples in D.3.2 For a new apparatus, and at least once a
duplicate. The assigned value of the flash point year for a working apparatus, conduct a verification
should be calculated after statistically analysing check using a CRM (D.2.1) tested in accordance
the inter-laboratory data. with 10.1 or 10.2.

Store SWSs in containers that retain the integrity of D.3.3 For intermediate verification, conduct a
the SWS, out of direct sunlight, at a temperature verification check using a SWS (D.2.2) tested in

170.14.19
FLASH POINT – ABEL CLOSED-CUP, IP 170

accordance with 10.1 or 10.2. where

D.3.4 Correct the result for barometric pressure in x is the mean of the test results;
accordance with 11.2. Record the corrected result, : is the certified value of the CRM or the
to the nearest 0,1 °C, in a permanent record. assigned value of the SWS;

D.4 Evaluation of the test result


2 2
[
R1 is equal to R − r 1 − (1 / n) ] (D.2)

D.4.1 General where


R is the reproducibility of the test method;
Compare the corrected test result(s) with the r is the repeatability of the test method;
certified value of the CRM or the assigned value of n is the number of replicate tests carried out
the SWS. on the CRM or SWS.

In Equations (D.1) to (D.3), it is assumed that D.4.4 Test conformance


reproducibility has been estimated in accordance
with ISO 4259[5] and that the certified value of the If the test result conforms to the tolerance
CRM, or the assigned value of the SWS, has been requirements, record this fact.
obtained by the procedures set out in ISO Guide
35[3], and that its uncertainty is small in comparison D.4.5 Test non-conformance
with the standard deviation of the test method and,
thus, small compared with the reproducibility of the If the result does not conform to the tolerance
test method, R. requirements and an SWS has been used for the
verification check, repeat using a CRM. If the result
D.4.2 Single test conforms to the tolerance requirements, record this
fact and dispose of the SWS.
For a single test made on a CRM or SWS, the
difference between a single result and the certified D.4.6 Troubleshooting
value of the CRM or the assigned value of the SWS
should be within the following tolerance: If the test result still does not conform to the
tolerance requirements, examine the apparatus and
R check that it conforms to the apparatus
x−μ ≤ (D.1) specification requirements.
2
In particular, check the size of gas flame or
where temperature of the electric ignition source
x is the result of the test; (automated instruments), alignment of ignition
: is the certified value of the CRM or the source, test cup thermometer calibration and
assigned value of the SWS; immersion depth, test portion heating rate and
R is the reproducibility of the test method. correct operation of the slide and dipping assembly.

D.4.3 Multiple tests If there is no obvious nonconformity, conduct a


further verification check using a different CRM. If
If a number, n, of replicate tests are made on a CRM the result conforms to the tolerance requirements,
or SWS, the difference between the mean of the n record this fact. If it is still not within the required
results and the certified value of the CRM or the tolerances, send the apparatus to the manufacturer
assigned value of the SWS should be within the for a detailed examination.
following tolerance:

R1
x−μ ≤ (D.2)
2

170.15.20
FLASH POINT – ABEL CLOSED-CUP, IP 170

Bibliography

[1] ISO Guide 33:2000, Uses of certified reference [6] ISO/TR 29662:—1), Petroleum products and
materials other liquids — Guide to flash point testing

[2] ISO Guide 34:2000, General requirements for [7] CEN/TR 15138, Petroleum products and other
the competence of reference material producers liquids — Guide to flash point testing

[3] ISO Guide 35:2006, Reference materials — [8] BS 2000-0.1:1999, Methods of test for
General and statistical principles for petroleum and its products. General
certification introduction. Specifications. IP Standard
thermometers. Section 0. 1: Specifications —
[4] ISO 3679:2004, Determination of flash point — IP standard for thermometers
Rapid equilibrium closed cup method

[5] ISO 4259:2006, Petroleum products —


Determination and application of precision data
in relation to methods of test

1) To be published.

170.16.21

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