SIST EN ISO 3680:2004
(Main)Determination of flash/no flash - Rapid equilibrium closed cup method (ISO 3680:2004)
Determination of flash/no flash - Rapid equilibrium closed cup method (ISO 3680:2004)
ISO 3680:2004 specifies a method for the determination of the ability of paints (including water-borne paints), varnishes, paint binders, adhesives, solvents and petroleum and related products, when maintained at a selected test temperature within the range of - 30 degrees Celsius and 300 degrees Celsius, and under the conditions of test, to yield sufficient flammable vapour at this temperature to cause ignition on the application of a test flame in a standard manner. When used in conjunction with the flash detector (A.1.6), ISO 3680:2004 is also suitable to carry out a flash/no flash test on fatty acid methyl esters (FAME).
Bestimmung des Flammpunktes - Ja/Nein-Verfahren - Schnelles Gleichgewichtsverfahren mit geschlossenem Tiegel (ISO 3680:2004)
Diese Internationale Norm legt ein Verfahren fest, mit dem bestimmt werden kann, ob Beschichtungsstoffe (einschließlich wasserverdünnbare Beschichtungsstoffe), Bindemittel, Lösemittel, Mineralölprodukte und verwandte Erzeugnisse, so sie bei einer gewählten Prüftemperatur zwischen -30 °C und 300 °C nach festgelegtem Verfahren temperiert werden, bei dieser Temperatur genügend brennbare Dämpfe abgeben, um diese durch eine externe Prüfflamme, betätigt nach festgelegtem Verfahren, zu entzünden. Diese Internationale Norm ist auch geeignet bei Fettsäuremethylestern (FAME) die Entscheidung ?Entzündbarkeit Ja/Nein' zu treffen, wenn der Detektor (A.1.6) benutzt wird.
Essai de point d'éclair de type passe/ne passe pas - Méthode rapide a l'équilibre en vase clos (ISO 3680:2004)
L'ISO 3680:2004 spécifie une méthode d'essai pour déterminer si des peintures (y compris les peintures à support aqueux), des vernis, des liants pour peintures, des adhésifs, des solvants, des produits pétroliers et des produits connexes, lorsqu'ils sont maintenus à une température d'équilibre comprise entre -30 °C et 300 °C, dans les conditions de l'essai, émettent suffisamment de vapeurs inflammables à cette température pour provoquer l'inflammation en présence d'une flamme d'essai présentée de manière normalisée. Lorsqu'elle est utilisée avec le détecteur d'éclair, l'ISO 3680:2004 convient aussi pour l'essai de point d'éclair de type passe/ne passe pas des esters méthyliques d'acide gras (EMAG).
Določanje pojava plamena - Hitra ravnotežna metoda v zaprti posodi (ISO 3680:2004)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 3680:2004
01-september-2004
'RORþDQMHSRMDYDSODPHQD+LWUDUDYQRWHåQDPHWRGDY]DSUWLSRVRGL ,62
Determination of flash/no flash - Rapid equilibrium closed cup method (ISO 3680:2004)
Bestimmung des Flammpunktes - Ja/Nein-Verfahren - Schnelles
Gleichgewichtsverfahren mit geschlossenem Tiegel (ISO 3680:2004)
Essai de point d'éclair de type passe/ne passe pas - Méthode rapide a l'équilibre en vase
clos (ISO 3680:2004)
Ta slovenski standard je istoveten z: EN ISO 3680:2004
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
SIST EN ISO 3680:2004 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 3680:2004
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SIST EN ISO 3680:2004
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SIST EN ISO 3680:2004
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SIST EN ISO 3680:2004
INTERNATIONAL ISO
STANDARD 3680
Fourth edition
2004-04-01
Determination of flash/no flash — Rapid
equilibrium closed cup method
Essai de point d'éclair de type passe/ne passe pas — Méthode rapide à
l'équilibre en vase clos
Reference number
ISO 3680:2004(E)
©
ISO 2004
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SIST EN ISO 3680:2004
ISO 3680:2004(E)
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ii © ISO 2004 – All rights reserved
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SIST EN ISO 3680:2004
ISO 3680:2004(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope. 1
2 Normative references. 1
3 Terms and definitions. 1
4 Principle. 2
5 Reagents and materials. 2
6 Apparatus. 2
7 Apparatus preparation. 3
8 Sampling. 4
9 Sample handling. 4
10 Procedure. 4
11 Calculation. 5
12 Expression of results. 6
13 Precision. 6
14 Test report. 7
Annex A (normative) Flash point test apparatus . 8
Annex B (normative) Thermometer specifications . 13
Annex C (informative) Verification of apparatus . 14
Annex D (informative) Use of a cup insert . 17
Bibliography . 18
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SIST EN ISO 3680:2004
ISO 3680:2004(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
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 3680 was prepared jointly by Technical Committees ISO/TC 28, Petroleum products and lubricants and
ISO/TC 35, Paints and varnishes.
This fourth edition cancels and replaces the third edition (ISO 3680:1983), which has been technically revised.
iv © ISO 2004 – All rights reserved
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SIST EN ISO 3680:2004
ISO 3680:2004(E)
Introduction
This International Standard describes one of two closed cup equilibrium methods for carrying out a
flash/no flash test for paints, varnishes, paint binders, solvents, adhesives, petroleum and related products.
[4]
When selecting a method, it should therefore be read in conjunction with the second method, ISO 1516 .
When used in conjunction with the flash detector (A.1.6) this International Standard is also suitable for the
flash/no flash testing of fatty acid methyl esters (FAME).
In both ISO 3680 and ISO 1516, the test is only carried out when the material under test and the air/vapour
mixture above the material in the test cup are approximately in temperature equilibrium.
This test method does not determine the flash point of the product under test, but merely its behaviour at the
selected test temperature as may be required to comply with laws or regulations relating to the storage,
transport and use of flammable products. For this purpose, it is unnecessary to determine the exact flash
point, but it is necessary to determine whether or not flashing occurs at a given temperature.
The apparatus specified in this International Standard enables a similar test result to be determined using a
more rapid procedure and a smaller test portion (2 ml or 4 ml) than that required in ISO 1516. In addition, the
apparatus can be made portable to the extent of being suitable for on-site testing in addition to its more
normal use in laboratories.
Collaborative work (see [6] in the Bibliography) has shown that results obtained by these procedures are
comparable. The interpretation of flash point results obtained on solvent mixtures containing halogenated
hydrocarbons should be considered with caution, as these mixtures can give anomalous results (see [7] in the
Bibliography).
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.
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SIST EN ISO 3680:2004
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SIST EN ISO 3680:2004
INTERNATIONAL STANDARD ISO 3680:2004(E)
Determination of flash/no flash — Rapid equilibrium closed cup
method
WARNING — The use of this International Standard may involve hazardous materials, operations and
equipment. This International Standard does not purport to address all of the safety problems
associated with its use. It is the responsibility of the user of this International Standard to establish
appropriate safety and health practices and determine the applicability of regulatory limitations prior
to use.
1 Scope
This International Standard specifies a method for the determination of the ability of paints (including water-
borne paints), varnishes, paint binders, adhesives, solvents and petroleum and related products, when
maintained at a selected test temperature within the range of − 30 °C to 300 °C, and under the conditions of
test, to yield sufficient flammable vapour at this temperature to cause ignition on the application of a test flame
in a standard manner. When used in conjunction with the flash detector (A.1.6), this International Standard is
also suitable to carry out a flash/no flash test on fatty acid methyl esters (FAME).
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 1513:1992, Paints and varnishes — Examination and preparation of samples for testing
ISO 3170:2004, Petroleum liquids — Manual sampling
ISO 3171:1988, Petroleum liquids — Automatic pipeline sampling
ISO 3679:2004, Determination of flash point — Rapid equilibrium closed cup method
ISO 15528:2000, Paints, varnishes and raw materials for paints and varnishes — Sampling
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
flash/no flash test
application of a test flame at the specified temperature of the test portion (as measured in the prescribed
manner), adjusted to a barometric pressure of 101,3 kPa, to determine whether the vapours of the test portion
ignite momentarily and a flame propagates across the surface of the liquid under the specified conditions of
test
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SIST EN ISO 3680:2004
ISO 3680:2004(E)
4 Principle
A test portion of specified volume is introduced into the test cup, which is maintained at the test temperature.
After a specified time, a test flame is applied and the presence or absence of a flash observed.
5 Reagents and materials
5.1 Cleaning solvent
An appropriate solvent for the removal of traces of the previous test portion from the test cup and cover.
NOTE The choice of solvent will depend upon the previous material tested and the tenacity of the residue. Low
volatility aromatic (benzene-free) solvents may be used to remove traces of oil, and mixed solvents such as toluene-
acetone-methanol may be effective for the removal of gum-type deposits.
5.2 Verification liquids
A series of certified reference materials (CRM) and/or secondary working standards (SWS) as described in
Annex C.
6 Apparatus
6.1 General
The apparatus is described in Annex A, and this includes the details of the test cup and cover assembly,
together with dimensions and special requirements. These are shown in Figure A.1 to Figure A.5. Tests for
flash/no flash over the whole range of − 30 °C to 300 °C may require more than one instrument.
6.2 Syringes
6.2.1 2 ml syringe, adjusted to deliver 2,00 ml ± 0,05 ml and equipped, if required, with a needle suitable
for use with the apparatus at test temperatures up to and including 100 °C. When testing FAME, a 2 ml test
portion is used at all temperatures.
6.2.2 5 ml syringe, adjusted to deliver 4,00 ml ± 0,10 ml and equipped, if required, with a needle suitable
for use with the apparatus at test temperatures above 100 °C. A 5 ml syringe is not required when testing
FAME.
6.3 Barometer, accurate to 0,1 kPa. Barometers precorrected to give sea-level readings, such as those
used at weather stations and airports, shall not be used.
6.4 Heating bath or oven (optional), for warming the samples, if required, and capable of controlling the
temperature to ± 5 °C. If an oven is used, it shall be intrinsically safe for hydrocarbon vapours.
It is recommended that the oven be of explosion-protected design.
6.5 Cooling bath or freezer (optional), for cooling the samples, if required, and capable of cooling the
sample to 10 °C below the selected test temperature, and controlling the temperature of the sample to ± 5 °C.
If a freezer is used, it shall be of an explosion-protected design.
6.6 Draught shield (optional), if required to minimize draughts, fitted at the back and on two sides of the
instrument.
NOTE A shield, 350 mm high, 480 mm wide and 240 mm deep, is suitable.
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SIST EN ISO 3680:2004
ISO 3680:2004(E)
6.7 Cup insert (optional). See Annex D.
NOTE For samples that are difficult to remove, a thin metal cup insert can be used.
7 Apparatus preparation
7.1 General
Select the appropriate instrument for the required flash/no flash temperature. If a flash/no flash test is to be
carried out at a temperature specified in regulations or specifications, the specified temperature shall be
adjusted for atmospheric barometric pressure before the test (see 11.2). Follow the manufacturer’s
instructions for the correct set-up and operation of the apparatus. The use of a cup insert (6.7) for potentially
adherent materials is described in Annex D.
7.2 Location of apparatus
Support the apparatus (Annex A) on a level and steady surface in a draught-free position.
Use of a draught shield (6.6) is recommended when protection from draughts is not available.
NOTE When testing materials which may produce toxic vapours, the apparatus may be located in a fume hood with
an individual control of air flow adjusted such that the vapours can be withdrawn without causing air currents around the
test cup during the test.
7.3 Cleaning of the test cup 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. Follow the manufacturer’s instructions for the care and servicing of the
instrument.
NOTE 1 A stream of clean dry air may be used to remove the last traces of solvent used.
NOTE 2 The filler orifice may be conveniently cleaned with a pipe cleaner.
7.4 Apparatus verification
7.4.1 Verify the correct functioning of the apparatus at least once a year by testing a certified reference
material (CRM) (5.2) in accordance with ISO 3679. The result obtained shall be equal to or less than R/ 2
from the certified value of the CRM, where R is the reproducibility of the method (see 13.3).
It is recommended that more frequent verification checks be made using secondary working standards
(SWSs) (5.2).
NOTE A recommended procedure for apparatus verification using CRMs and SWSs, and the production of SWSs, is
given in Annex C.
7.4.2 The numerical values obtained during the verification check shall not be used to provide a bias
statement, nor shall they be used to make any correction to the flash points subsequently determined using
the apparatus.
If the instrument fails the verification test, it is recommended that the operator should check that:
a) the cover makes a vapour-tight seal with the test cup;
b) the shutter provides a light-tight seal;
c) adequate heat-transfer paste surrounds the thermometer bulb and immersed portion of the thermometer
barrel.
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SIST EN ISO 3680:2004
ISO 3680:2004(E)
8 Sampling
8.1 Unless otherwise specified, obtain samples in accordance with the procedures given in ISO 15528,
ISO 3170 or ISO 3171 or an equivalent national standard.
8.2 Place sufficient sample volume for testing in a tightly sealed container made of material appropriate to
the liquid being sampled, and for safety purposes, ensure that the sample container is only filled to between
85 % and 95 % of its capacity.
8.3 Store the samples in conditions to minimize vapour loss and pressure build-up. Avoid storing the
samples at temperatures in excess of 30 °C.
9 Sample handling
9.1 Petroleum products and fatty acid methyl esters
9.1.1 Subsampling. Cool in a cooling bath or freezer (6.5), or adjust the temperature of the sample and its
container to at least 10 °C below the first selected test temperature before opening to remove the test portion.
If an aliquot of the original sample is to be stored prior to testing, ensure that the container is still filled to at
least 85 % of its capacity. Gently mix the subsample to ensure uniformity, so that the loss of volatile
components and light ends is minimized.
NOTE Results of flash/no flash tests may be affected if the sample volume falls below 85 % of the container capacity.
9.1.2 Samples that are liquid at ambient temperature. If sufficiently fluid, mix samples gently shaking by
hand prior to the removal of the test portion, taking care to minimize the loss of volatile components. If the
sample is too viscous at ambient temperature, heat the sample in its container using a heating bath or oven
(6.4) to a temperature not warmer than 10 °C below the test temperature, such that the sample can be mixed
by gentle shaking.
9.1.3 Solid or semi-solid samples. If the material under test cannot be made sufficiently fluid to be
introduced into the test cup through the orifice by heating in accordance with 9.1.2, transfer the test portion
with a solids dispenser or spatula into the test cup whilst the cover is open.
9.2 Paints, varnishes and related materials
Prepare the samples in accordance with the procedures described in ISO 1513.
10 Procedure
10.1 General
10.1.1 Use the equation in 11.2 to determine the test tempera
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