DIN EN ISO 4589-2: Deutsche Norm
DIN EN ISO 4589-2: Deutsche Norm
DIN EN ISO 4589-2: Deutsche Norm
Plastics –
Determination of burning behaviour by oxygen index –
Part 2: Ambient-temperature test (ISO 4589-2:1996 + Amd. 1:2005)
(includes Amendment A1:2006)
English version of DIN EN ISO 4589-2:2006-06
Kunststoffe –
Bestimmung des Brennverhaltens durch den Sauerstoff-Index –
Teil 2: Prüfung bei Umgebungstemperatur (ISO 4589-2:1996 + Amd. 1:2005)
(enthält Änderung A1:2006)
Englische Fassung DIN EN ISO 4589-2:2006-06
National foreword
This standard has been published in accordance with a decision taken by CEN/TC 249 to adopt, without
alteration, International Standard ISO 4589-2:1996 + Amd. 1:2005 as a European Standard.
The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics
Standards Committee), Technical Committee NA 054-01-05 AA Brandverhalten.
The DIN Standards corresponding to the International Standards referred to in clause 2 of the EN are as
follows:
Amendment A1:2005 has been integrated in this standard and is marked by a vertical line in the left margin.
Amendments
c) A new subclause 9.4 containing precision data has been included and the previous subclause 9.4 has
been inserted in a new Annex E.
Previous editions
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National Annex NA
(informative)
Bibliography
DIN EN ISO 294-1, Plastics — Injection moulding of test specimens of thermoplastic materials — Part 1:
General principles, and moulding of multipurpose and bar test specimens
DIN EN ISO 294-2, Plastics — Injection moulding of test specimens of thermoplastic materials — Part 2:
Small tensile bars
DIN EN ISO 294-3, Plastics — Injection moulding of test specimens of thermoplastic materials — Part 3:
Small plates
DIN EN ISO 294-4, Plastics — Injection moulding of test specimens of thermoplastic materials — Part 4:
Determination of moulding shrinkage
DIN EN ISO 295, Plastics — Compression moulding of test specimens of thermosetting materials
DIN ISO 2859-1, Sampling procedures for inspection by attributes — Part 1: Sampling plans indexed by
acceptable quality level (AQL) for lot-by-lot inspection
DIN ISO 2859-2, Sampling procedures for inspection by attributes — Part 2: Sampling plans indexed by
limiting quality (LQ) for isolated lot inspection
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English version
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 Management Centre or to any CEN member.
The European Standards exist 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 Management Centre has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, the Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, and the United Kingdom.
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 4589-2:1999 + A1:2006 E
worldwide for CEN national Members.
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Contents Page
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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 December 1999, and conflicting national standards shall be withdrawn
at the latest by December 1999.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard:
Austria, Belgium, the Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy,
Luxembourg, the Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, and the United Kingdom.
Endorsement notice
The text of the International Standard ISO 4589-2:1996 was approved by CEN as a European Standard
without any modification.
EN ISO 4589 consists of the following parts, under the general title ‘Plastics – Determination of burning
behaviour by oxygen index’:
⎯ Part 1: Guidance
Annexes A and B of this part of EN ISO 4589 are normative. Annexes C and D are informative.
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 October 2006, and conflicting national standards shall be withdrawn at
the latest by October 2006.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, 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.
Endorsement notice
The text of ISO 4589-2:1996/Amd. 1:2005 has been approved by CEN as EN ISO 4589-2:1999/A1:2006
without any modifications.
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1 Scope
This part of ISO 4589 specifies methods for determining the minimum concentration of oxygen, in admixture
with nitrogen, that will support combustion of small vertical test specimens under specified test conditions. The
results are defined as oxygen index values.
Methods are provided for testing materials that are self-supporting in the form of vertical bars or sheet up to
10,5 mm thick. These methods are suitable for solid, laminated or cellular materials characterized by an
apparent density greater than 100 kg/m3. The methods may also be applicable to some cellular materials
having an apparent density of less than 100 kg/m3. A method is provided for testing flexible sheet or film
materials while supported vertically.
For comparative purposes, a procedure is provided for determining whether or not the oxygen index of a
material lies above some specified minimum value.
Oxygen index results obtained using the methods described in this part of ISO 4589 can provide a sensitive
measure of the burning characteristics of materials under certain controlled laboratory conditions, and hence
may be useful for quality control purposes. The results obtained are dependent upon the shape, orientation
and isolation of the test specimen and the conditions of ignition. For particular materials or applications, it may
be necessary or appropriate to specify different test conditions. Results obtained from test specimens of
differing thickness or by using different ignition procedures may not be comparable and no correlation with
flammability behaviour under other fire conditions is implied.
Results obtained in accordance with this part of ISO 4589-2 must not be used to describe or appraise the fire
hazard presented by a particular material or shape under actual fire conditions, unless used as one element of
a fire risk assessment that takes into account all of the factors pertinent to the assessment of the fire hazard of
a particular application for the material.
NOTE 1 It may not be possible to apply these methods satisfactorily to materials that exhibit high levels of shrinkage
when heated, e.g. highly oriented thin film.
NOTE 2 For assessing the flame propagation properties of cellular materials of density < 100 kg/m3, attention is drawn
to the method of ISO 3582:2000, Flexible cellular polymeric materials — Laboratory assessment of horizontal burning
characteristics of small specimens subjected to a small flame.
2 Normative references
The following standards contain provisions which, through reference in this text, constitute provisions of this
part of ISO 4589. At the time of publication, the editions indicated were valid. All standards are subject to
revision, and parties to agreements based on this part of ISO 4589 are encouraged to investigate the
possibility of applying the most recent editions of the standards indicated below. Members of IEC and
ISO maintain registers of currently valid International Standards.
ISO 294 (all parts), Plastics — Injection moulding of test specimens of thermoplastic materials
ISO 2859-1:1989, Sampling procedures for inspection by attributes — Part 7: Sampling plans indexed by
acceptable quality level (AQL) for lot-by-lot inspection
ISO 2859-2:1985, Sampling procedures for inspection by attributes — Part 2: Sampling plans indexed by
limiting quality (LQ) for isolated lot inspection
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3 Definition
For the purposes of this part of ISO 4589, the following definition applies.
3.1
oxygen index
the minimum concentration of oxygen, by volume percentage, in a mixture of oxygen and nitrogen introduced
at (23 ± 2) °C that will just support combustion of a material under specified test conditions.
4 Principle
A small test specimen is supported vertically in a mixture of oxygen and nitrogen flowing upwards through a
transparent chimney. The upper end of the specimen is ignited and the subsequent burning behaviour of the
specimen is observed to compare the period for which burning continues, or the length of specimen burnt,
with specified limits for such burning. By testing a series of specimens in different oxygen concentrations, the
minimum oxygen concentration is estimated (see 8.6).
Alternatively, for comparison with a specified minimum oxygen index value, three test specimens are tested
using the relevant oxygen concentration, at least two of which are required to extinguish before any relevant
burning criterion is exceeded.
5 Apparatus
5.1 Test chimney, consisting of a heat-resistant glass tube supported vertically on a base through which
oxygen-containing gas mixtures can be introduced (see Figures 1 and 2).
The prefered dimensions of the chimney are 500 mm ± 50 mm minimum height and 75 mm to 100 mm inside
diameter.
The upper outlet shall be restricted as necessary by an overhead cap having an outlet small enough to
produce an exhaust velocity of at least 90 mm/s from that outlet.
NOTE 3 A cap converging to an outlet of 40 mm diameter at a level at least 10 mm above the top of the cylindrical
chimney has been found satisfactory.
Chimneys of other dimensions, with or without restricted outlets, may be used, if shown to give equivalent
results. The bottom of the chimney, or the base upon which the chimney is supported, shall incorporate a
device for distributing evenly the gas mixture entering the chimney. The preferred device comprises a suitable
diffuser and a mixing chamber with metal foil. Other devices, such as radial manifolds, may be used, if shown
to give equivalent results. A porous screen may be mounted below the level of the specimen holder, to
prevent falling combustion debris from fouling the gas entry and distribution paths.
The chimney support may incorporate a levelling device and indicator, to facilitate vertical alignment of the
chimney and a test specimen supported therein. A dark background may be provided to facilitate observation
of flames within the chimney.
5.2 Test specimen holder, suitable for supporting a specimen vertically in the centre of the chimney.
For self-supporting materials, the specimen shall be held by a small clamp which is at least 15 mm away from
the nearest point at which the specimen may burn before the extent-of-burning criterion is exceeded. For
supported film or sheet test specimens, the specimen shall be supported by both vertical edges in a frame
equivalent to that illustrated by Figure 2, with reference marks at 20 mm and 100 mm below the top of the
frame.
The profile of the holder and its support should preferably be smooth to minimize induction of turbulence in the
rising flow gas.
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Dimensions in millimetres
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NOTE The test specimen is held securely along both upright edges between forks made of stainless steel.
5.3 Gas supplies, comprising pressurized sources of oxygen and/or nitrogen not less than 98 % (m/m) pure
and/or clean air [containing 20,9 % (V/V) oxygen], as appropriate.
The moisture content of the gas mixture entering the chimney shall be < 0,1 % (m/m), unless the results have
been shown to be insensitive to higher moisture levels in the gas mixture. The gas supply system shall
incorporate a drying device, or provision for monitoring or sampling the gas supply for moisture content,
unless the moisture content of the gas supplies is known to be acceptable.
The constituent gas supply lines shall be linked in a manner which thoroughly mixes the gases, before they
enter the gas distribution device at the base of the chimney, so that the variation in oxygen concentration in
the gas mixture rising in the chimney, below the level of the test specimen, is < 0,2 % (V/V).
NOTE 4 It should not be assumed that bottled oxygen or nitrogen will always contain < 0,1 % (m/m) of water; moisture
contents of 0,003 % (m/m) to 0,01 % (m/m) are typical for commercial supplies as filled bottles of purity > 98 % (m/m), but
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as such bottled gases are depressurized to below about 1 MPa, the moisture content of the gas drawn off may rise above
0,1 % (m/m).
5.4 Gas measurement and control devices, suitable for measuring the concentration of oxygen in the gas
mixture entering the chimney with an accuracy of ± 0,5 % (V/V) of the mixture and for adjusting the
concentration with a precision of ± 0,1 % (V/V) of the mixture when the gas velocity through the chimney is
(40 ± 2) mm/s at (23 ± 2) °C.
Means shall be provided for checking or ensuring that the temperature of the gas mixture entering the
chimney is (23 ± 2) °C. If this involves an internal probe, its position and profile shall be designed to minimize
induction of turbulence within the chimney.
NOTE 5 Systems of measurement and control that have proved satisfactory include the following:
a) needle valves on individual and mixed gas supply lines, a paramagnetic oxygen analyser or equivalent that
continuously samples the mixed gas, and a flowmeter to indicate when the gas flow through the chimney is within the
required limits;
b) calibrated orifices, gas pressure regulators and pressure gauges on the individual gas supply lines;
c) needle valves and calibrated flowmeters on the individual gas supply lines.
Systems b) and c) may require calibration after assembly to ensure that the cumulative errors of the
component parts do not exceed the requirements of 5.4.
5.5 Flame igniter, comprising a tube that can be inserted into the chimney to apply to the test specimen a
flame issuing from an outlet of (2 ± 1) mm diameter at the end of the tube.
The flame fuel shall be propane, without premixed air. The fuel supply shall be adjusted so that the flame will
project (16 ± 4) mm vertically downwards from the outlet when the tube is vertical within the chimney and the
flame is burning within the chimney atmosphere.
5.6 Timing device, capable of measuring periods up to 5 min with an accuracy of ± 0,5 s.
5.7 Fume extraction system, providing sufficient ventilation or exhaust to remove fumes or soot expelled
from the chimney without disrupting the gas flow rate or temperatures in the chimney.
NOTE 6 If soot-generating materials are being tested, the glass chimney may require cleaning to maintain good
visibility, and the gas inlets, or inlet screen, and temperature sensor (if fitted) may also require cleaning to function
properly. Suitable precautions should be taken to protect personnel from noxious materials or burns during testing or
cleaning operations.
5.8 Tool for preparing rolled film, consisting of a stainless-steel rod of 2 mm diameter, with a slit in one
end (see Figure 3).
6 Calibration of equipment
For compliance with this method, calibrate the equipment periodically in accordance with the instructions
given in Annex A so that the maximum interval between recalibration and use complies with the periods stated
in Table 1.
7.1 Sampling
Obtain a sample sufficient for preparation of at least 15 test specimens. The sample shall be taken, if relevant,
in accordance with the material specification, otherwise in accordance with ISO 2859-1 or ISO 2859-2, as
applicable.
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NOTE 7 For a material for which the oxygen index is known to within ± 2, 15 test specimens may be sufficient. For
materials of unknown oxygen index, or which exhibit erratic burning characteristics, between 15 and 30 test specimens
may be required.
Dimensions in millimetres
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Using, if applicable, procedures that comply with the appropriate material specification (see note 8) or
ISO methods (see note 9) for specimen preparation, mould or cut test specimens that satisfy the dimensions
specified for the most appropriate specimen form given in Table 2.
To prepare a rolled specimen from a thin film, use the tool described in 5.8. Insert one corner of the film into
the slit and then wind the film round the rod in a spiral of 45°. Ensure that the 45° angle is maintained during
the winding process so that the film reaches exactly to the end of the tool, to produce a test piece of the
correct length, as shown in Figure 3. After the winding is finished, tape the last end of the roll while the ma-
terial is still on the stainless steel rod to prevent loosening. Then pull the rod out of the rolled film. Cut off the
rolled film at a distance of 20 mm from the top end (see Figure 4).
Ensure that the surfaces of the specimens are clean and free from flaws that could affect burning behaviour,
e.g. peripheral moulding flash or burrs from machining.
Note the position and orientation of test specimens with respect to any asymmetry in the sample material (see
note 10).
NOTE 8 Some material specifications may require choice and identification of the “state of the test specimen” used;
e.g. in a “defined state” or a “basic state” for a styrene-based polymer or copolymer.
NOTE 9 In the absence of a relevant specification, one or more procedures from ISO 293, ISO 294, ISO 295, ISO 2818
or ISO 3167 may be used.
NOTE 10 Oxygen index results may be significantly affected by differences in ease of ignition or burning behaviour, due
to material inhomogeneity (e.g. different levels of shrinkage when heated for specimens cut in different directions from
asymmetrically oriented thermoplastics film).
NOTE 11 If a thin film burns in such a manner that erratic combustion behaviour including heat shrinkage and fluctuation
of data results, the specimen form VI, i.e. a rolled film, should preferably be used. It gives reproducible results, similar to
those given by specimen form I. Precision data obtained by interlaboratory trials on specimen form VI are given in
Annex D.
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Dimensions
Test
Length Width Thickness Typical
specimena
mm mm mm
I 80 to 150 10 ± 0,5 4 ± 0,25 For moulding materials
II 80 to 150 10 ± 0,5 10 ± 0,5 For cellular materials
IIIb 80 to 150 10 ± 0,5 ≤ 10,5 For sheet materials “as received”
Alternative size for self-supporting moulding or sheet
IV 70 to 150 6,5 ± 0,5 3 ± 0,25
materials, for electrical purposes
0
Vb 140 −5 52 ± 0,5 ≤ 10,5 For flexible film or sheet
For thin film “as received”; limited to the film that can
VIc 140 to 200 20 0,02 to 0,10d
be rolled by the specified rodd
a Test specimens of forms I, II, III and IV are suitable for materials that are self-supporting at these dimensions. Test
specimens of form V are suitable for materials that require support during testing.
b Results obtained using form Ill or form V test specimens may only be comparable for specimens of the same form and
thickness. It is assumed that the amount of variation in thickness for such materials will be controlled by other standards.
c The test specimen of form VI is suitable for a thin film that is self-supporting when it is rolled. Dimensions in the table are
of an original film from which the rolled form is made. See 7.2 for the preparation of rolled film.
d The film is limited to thicknesses that can be rolled by the specified rod (see Figure 3). If the film is very thin, it may be
necessary to combine two or more films together in the preparation of the rolled film so as to obtain results similar to those
normally obtained with specimen form VI.
Dimensions in millimetres
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7.3.1 General
For monitoring the distance over which a specimen burns, it may be marked with transverse lines at one or
more levels which are dependent upon the specimen form and the ignition procedure to be used. Self-
supporting specimens are preferably marked on at least two adjacent faces. If wet inks are used, the marks
shall be dry before the specimen is ignited.
Test specimens of form I, II, III, IV or VI to be tested in accordance with procedure A (see 8.2.2) shall be
marked 50 mm from the end to be ignited.
The reference marks for testing specimens of form V are carried by the supporting frame (see Figure 2), but
such specimens may be marked at 20 mm and at 100 mm from the end to be ignited, for convenience when
testing heat-stable materials.
If specimens of forms I, II, III, IV and VI are to be tested in accordance with procedure B (see 8.2.3), they shall
be marked at 10 mm and at 60 mm from the end to be ignited.
7.4 Conditioning
Unless otherwise specified in other established standards, each test specimen shall be conditioned for at least
88 h at (23 ± 2) °C and (50 ± 5) % relative humidity immediately prior to use.
NOTE 12 Specimens of cellular materials that may contain volatile flammable material should preferably be purged of
such volatile material prior to conditioning at 23 °C and 50 % relative humidity. Test specimens may be purged
satisfactorily by pre-conditioning in suitable ventilated ovens for 168 h. Larger blocks of such materials may require longer
pre-treatment. It is important that facilities for cutting specimens from cellular material that may contain volatile flammable
material are suitable for the hazards involved.
8.1.1 Maintain the ambient temperature for the test apparatus at (23 ± 2) °C. If necessary, keep the test
specimens in an enclosure at (23 ± 2) °C and (50 ± 5) % relative humidity from which each test specimen may
be taken when required.
8.1.2 Recalibrate equipment components, if necessary (see clause 6 and Annex A).
8.1.3 Select an initial concentration of oxygen to be used. When possible, base this on experience of results
for similar materials. Alternatively, try to ignite a test specimen in air, and note the burning behaviour. If the
specimen burns rapidly, select an initial concentration of about 18 % (V/V) of oxygen; if the test specimen
burns gently or unsteadily, select an initial oxygen concentration of about 21 % (V/V); if the specimen does not
continue to burn in air, select an initial concentration of at least 25 % (V/V), depending upon the difficulty of
ignition or the period of burning before extinguishing in air.
8.1.4 Ensure that the test chimney is vertical (see Figure 1). Mount a specimen vertically in the centre of the
chimney so that the top of the specimen is at least 100 mm below the open top of the chimney and the lowest
exposed part of the specimen is at least 100 mm above the top of the gas distribution device at the base of
the chimney (see Figure 1 or 2 as appropriate).
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8.1.5 Set the gas mixing and flow controls so that an oxygen/nitrogen mixture at (23 ± 2) °C, containing the
desired concentration of oxygen, is flowing through the chimney at (40 ± 2) mm/s. Let the gas flow purge the
chimney for at least 30 s prior to ignition of each specimen, and maintain the flow without change during
ignition and combustion of each specimen.
Record the oxygen concentration used as the volume per cent calculated in accordance with the equations
given in Annex B.
8.2.1 General
Select one of two alternative ignition procedures which are dependent upon the specimen form as follows:
a) for specimen forms I, II, III, IV and VI (see Table 2), use procedure A (top surface ignition) as described in
8.2.2;
Ignition shall imply, for the purposes of this part of ISO 4589, the initiation of flaming combustion.
NOTE 14 For tests on materials that exhibit steady burning and spread of combustion in oxygen concentrations at, or
close to, their oxygen index value, or for self-supporting specimens of ≤ 3 mm thickness, procedure B (with specimens
marked in accordance with 7.3.2) may be found to give more consistent results than procedure A. Procedure B may then
be used for specimens of form I, II, III, IV or VI.
NOTE 15 Some materials may exhibit a non-flaming type of combustion (e.g. glowing combustion) instead of, or at a
lower oxygen concentration than that required for, flaming combustion. When testing such materials, it is necessary to
identify the type of combustion for which the oxygen index is required or measured.
For top surface ignition, the igniter is used to initiate burning only on the top surface of the upper end of the
specimen.
Apply the lowest visible part of the flame to the top of the specimen using a sweeping motion, if necessary, to
cover the whole surface, but taking care not to maintain the flame against the vertical faces or edges of the
specimen. Apply the flame for up to 30 s, removing it every 5 s for just sufficient time to observe whether or
not the entire top surface of the specimen is burning.
Consider the specimen to be ignited, and commence measurement of the period and distance of burning, as
soon as removal of the igniter, after a contact period increment of 5 s, reveals burning supported by the whole
of the top end of the specimen.
For propagating ignition, the igniter is used to produce burning across the top and partially down the vertical
faces of the specimen.
Lower and move the igniter sufficiently to apply the visible flame to the end face of the specimen and also, to a
depth of approximately 6 mm, to its vertical faces. Continue to apply the igniter for up to 30 s, including
interruptions for inspection of the specimen every 5 s, until its vertical faces are burning steadily or until the
visibly burning portion first reaches the level of the upper reference mark either on the sup-port frame or, if
used for specimens of form I, II, Ill, IV or VI, on the specimen.
Consider the specimen to be ignited, for the purpose of measuring the period and extent of burning, as soon
as any part of the visible burning portion reaches the level of the upper reference mark.
NOTE 16 The burning portion includes any burning drips that may run down the surface of the specimen.
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8.3.1 Commence measurement of the period of burning as soon as the specimen has been ignited in
accordance with 8.2.2 or 8.2.3, as applicable, and observe its burning behaviour. If burning ceases but
spontaneous re-ignition occurs within 1 s, continue the observation and measurements.
8.3.2 If neither the period nor the extent of burning exceeds the relevant limit specified in Table 3 for the
applicable specimen, note the duration and extent of burning. This is recorded as an “O” response.
Alternatively, if either the period or extent of burning exceeds the relevant limit specified in Table 3, note the
burning behaviour accordingly, and extinguish the flame. This is recorded as an “X” response.
Note also the burning characteristics of the material, e.g. dripping, charring, erratic burning, glowing combus-
tion or after-glow.
8.3.3 Remove the specimen and clean, as necessary, any surfaces within the chimney or on the igniter that
have become contaminated with soot, etc. Allow the chimney to regain a temperature of (23 ± 2) °C, or
replace it with another so conditioned.
NOTE 17 If many tests are being carried out, it is appropriate to use two chimneys and two specimen holders thus
allowing one chimney and holder to cool down while the second set is being used for the next test.
NOTE 18 If sufficiently long, the specimen may be inverted, or trimmed to remove the burnt end, and re-used. Results
from such specimens can save material when establishing an approximate value for the minimum oxygen concentration
required for combustion, but cannot be included among those used for estimation of the oxygen index, unless the
specimen is reconditioned at the temperature and humidity appropriate for the material involved.
Alternative criteriaa
Test specimen Period of
form Ignition procedure burning after
(see Table 2) Extent of burningb
ignition
s
A
180 50 mm below the top of the specimen
Top surface ignition
I, II, Ill, IV and VI
B
180 50 mm below the upper reference mark
Propagating ignition
B 80 mm below the upper reference mark (on the
V 180
Propagating ignition frame)
a These criteria do not necessarily produce equivalent oxygen index results for specimens of differing shape or tested
using different ignition conditions or procedures.
b The extent of burning is exceeded when any part of the visibly burning portion of a specimen, including burning drips
descending the vertical faces, passes the level defined in the fourth column of the table.
The procedure described in 8.5 and 8.6 is based upon the “up-and-down method for small samples”1), using
the specific case where NT – NL = 5 (see 8.6.2 and 8.6.3), with an arbitrary step size for certain changes to be
made in the oxygen concentration used.
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During the testing, select the oxygen concentration to be used for testing the next test specimen as follows:
a) decrease the oxygen concentration if the burning behaviour of the preceding specimen gave an “X”
response;
otherwise
d) increase the oxygen concentration if the preceding specimen gave an “O” response.
Choose the size of the change in oxygen concentration in accordance with 8.5 or 8.6, as appropriate.
Repeat the procedures specified in 8.1.4 to 8.4 inclusive, using oxygen concentration changes of any
convenient step size, until the oxygen concentrations, in volume per cent, have been found that differ by
≤ 1,0 % (V/V) and of which one gave an “O” response and the other an “X” response. From this pair of oxygen
concentrations, note that which gave the “O” response as the preliminary oxygen concentration level and then
proceed in accordance with 8.6.
NOTE 19 The two results, at oxygen concentrations ≤ 1,0 % (V/V) apart, which give opposite responses do not have to
be from successive specimens.
NOTE 20 That concentration which gave the “O” response does not have to be lower than that which gave the “X”
response.
NOTE 21 A format convenient for recording the information required by this and subsequent clauses is illustrated in
Annex C.
8.6.1 Using, again, the preliminary oxygen concentration (see 8.5), test one specimen by repeating 8.1.4 to
8.3 inclusive. Record both the oxygen concentration (co) used and the response, “X” or “O”, as the first of the
NL and of the NT series of results.
8.6.2 Change the oxygen concentration, in accordance with 8.4, using concentration changes (d) of
0,2 % (V/V) (see note 22) of the total gas mixture to test further specimens in accordance with 8.1.4 to 8.4
inclusive, noting the values of co and the corresponding responses until a different response to that obtained in
8.6.1 is recorded.
The result from 8.6.1, plus those of like response from 8.6.2, constitute the NL series of results. (See example
in Annex C, section 2.)
NOTE 22 Where experience has shown that the requirements of 8.6.4 are usually satisfied by a value of d other than
0,2 % (V/V), that value may be selected as the initial value of d.
8.6.3 Test four more specimens, in accordance with 8.1.4 to 8.4 inclusive, maintaining d = 0,2 % (V/V); and
note the co used for, and response of, each specimen. Designate the oxygen concentration used for the last
specimen as cf.
These four results, together with the last result from 8.6.2 (i.e. that which differed in response from that of
8.6.1), constitute the remainder of the NT series, so that
NT = NL + 5
8.6.4 Calculate the estimated standard deviation, σˆ , of the oxygen concentration measurements from the
last six responses in the NT series (including cf), in accordance with 9.3. If the condition
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2σˆ
< d < 1,5 σˆ
3
a) if d < 2 σˆ /3, repeat steps 8.6.2 to 8.6.4, using increased values for d, until the condition is satisfied, or
b) if d > 1,5 σˆ , repeat steps 8.6.2 to 8.6.4 using decreased values for d, until the condition is satisfied,
except that d shall not be reduced below 0,2 unless so required by the relevant material specification.
Calculate the oxygen index OI, expressed as a percentage by volume, from the relationship
OI = cf + k d
where
cf is the final value of the oxygen concentration, in volume per cent to one decimal place, used in the series
of NT measurements performed in accordance with 8.6, and noted in accordance with 8.6.3;
d is the interval, in volume per cent to at least one decimal place, between oxygen concentration levels used
and controlled in accordance with 8.6;
For the purposes of calculation of σˆ , as required by 8.6.4 and 9.3, the OI shall be calculated to two decimal
places.
For the purposes of reporting OI results, express OI values to the nearest 0,1, with exactly intermediate
results being rounded downwards.
16
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Table 4 — Values of k for calculating the oxygen index concentration from determinations made by
Dixon's “up-and-down” method
1 2 3 4 5 6
Responses for Values of k for which the first N L determinations are
the last five
measurements a) O OO OOO OOOO
XOOOO –0,55 –0,55 –0,55 –0,55 OXXXX
XOOOX –1,25 –1,25 –1,25 –1,25 OXXXO
XOOXO 0,37 0,38 0,38 0,38 OXXOX
XOOXX –0,17 –0 , 1 4 –0 , 1 4 –0 , 1 4 OXXOO
XOXOO 0,02 0,04 0,04 0,04 OXOXX
XOXOX –0,50 –0,46 –0,45 –0,45 OXOXO
XOXXO 1,17 1,24 1,25 1,25 OXOOX
XOXXX 0,61 0,73 0,76 0,76 OXOOO
XXOOO –0,30 –0,27 –0,26 –0,26 OOXXX
XXOOX –0,83 –0,76 –0,75 –0,75 OOXXO
XXOXO 0,83 0,94 0,95 0,95 OOXOX
XXOXX 0,30 0,46 0,50 0,50 OOXOO
XXXOO 0,50 0,65 0,68 0,68 OOOXX
XXXOX –0,04 0,19 0,24 0,25 OOOXO
XXXXO 1,60 1,92 2,00 2,01 OOOOX
XXXXX 0,89 1,33 1,47 1,50 OOOOO
Values of k for which the first NL determinations are
Responses for
b) X XX XXX XXXX
the last five
are as given in the above table opposite the appropriate response in measurements
column 6, but with the sign of k reversed, i.e. OI = cf – kd (see 9.1).
9.2 Determination of k
The value and sign of k are dependent upon the pattern of the responses of specimens tested in accordance
with 8.6, and may be determined from Table 4 as follows:
a) If the response of the specimen tested in accordance with 8.6.1 was “O”, so that the first contrary
response (see 8.6.2) was an “X”, refer to column 1 of Table 4 to select the row for which the last four
response symbols correspond to those found when testing in accordance with 8.6.3. The value and sign
of k will be that shown in column 2, 3, 4 or 5 for which the number of “O”s shown in row a) of the table
corresponds to the number of “O” responses found for the NL series, in accordance with 8.6.1 and 8.6.2.
or
b) If the response of the specimen tested in accordance with 8.6.1 was “X”, so that the first contrary
response was an “O”, refer to the sixth column of Table 4 to select the row for which the last four
response symbols correspond to those found when testing in accordance with 8.6.3. The value of k will
be that shown in column 2, 3, 4 or 5 for which the number of “X”s shown in row b) of the table
corresponds to the number of “X” responses found for the NL series, in accordance with 8.6.1 and 8.6.2,
but the sign of k is reversed, so that negative values shown in Table 4 for k become positive, and vice
versa.
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For the purposes of 8.6.4, calculate the estimated standard deviation σˆ of the oxygen concentration
measurements from the relationship
1/ 2
⎡ n ⎤
⎢ ∑
⎢i = 1
(ci − OI)2 ⎥
⎥
σˆ = ⎢ ⎥
⎢ n −1 ⎥
⎢ ⎥
⎣⎢ ⎦⎥
where
ci represents, in turn, each of the per cent oxygen concentrations used during measurement of the last six
responses in the NT series of measurements;
NOTE 24 For this method, n = 6, in accordance with 8.6.4. For n = 6, the method loses precision. For n = 6, alternative
statistical criteria would apply.
9.4.1 An interlaboratory study was conducted in 1999 between ISO and ASTM using ISO 4589-2:1996 and
ASTM D 2863-97 as protocols for the test criteria. The precision data were determined from interlaboratory
tests involving twelve laboratories, on eight polymeric materials, with two replicates of each material. The
resulting data were analysed in accordance with ISO 5725-2, and are summarized in Table 5.
9.4.2 Repeatability, in the normal and correct operation of the method, is the difference between two
averages, determined from two specimens, using identical test material and the same apparatus, by one
operator within a short time interval. The value of the repeatability should not exceed those shown in Table 5.
9.4.3 Reproducibility, in the normal and correct operation of the method, is the difference between two
independent averages determined from two specimens by two operators working in different laboratories on
identical test material. The values of the reproducibility should not exceed those shown in Table 5.
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9.4.4 Two averages (determined from two specimens) are to be considered suspect and not equivalent if
they differ by more than the repeatability and reproducibility shown in Table 5. Any decision made in relation
to 9.4.2 or 9.4.3 would have an approximately 95 % (0,95) probability of being correct.
NOTE 25 The explanations of “repeatability” and “reproducibility” given in 9.4.2 and 9.4.3 are only intended to present a
meaningful way of considering the approximate precision of this test method. The test results and precision data in Table 5
should not be used for the acceptance or rejection of materials, as these data apply only to the materials tested in the
interlaboratory study and are unlikely to be rigorously representative of other lots, formulations, conditions, materials or
laboratories. Users of this test method should apply the principles outlined in ISO 4589-2 to generate data specific to their
materials and laboratory (or between specific laboratories). The principles of 9.4.2 to 9.4.4 would then be valid for such
data.
10.1 Set up the apparatus and test specimen in accordance with 8.1 except that the specified minimum
concentration of oxygen shall be selected for the purposes of 8.1.3.
10.3 Using up to three specimens, assess the burning behaviour of each specimen in accordance with 8.3.1,
8.3.2 and 8.3.3.
If for at least two out of the three specimens thus tested the flame is extinguished before the relevant criteria
from Table 3 are exceeded, i.e. an “ O” response is recorded, then record that the oxygen index of the
material is not less than the specified value. Otherwise, record that the oxygen index of the material is less
than the specified value or determine the oxygen index in accordance with clause 8, as appropriate.
11 Test report
The test report shall include the following information:
b) a statement that the test results relate only to the behaviour of the test specimens under the conditions of
this test and that these results shall not be used to infer the fire hazards of the materials in other forms or
under other fire conditions;
c) all details necessary for identification of the material tested, including, where relevant, the type of
material, its density, its previous history and the specimen orientation with respect to any anisotropy in
the material or sample;
f) the oxygen index or a reference to procedure C together with the relevant specified minimum oxygen
index and a report as to whether or not the material tested had a higher oxygen index;
g) if applicable, the estimated standard deviation and the oxygen concentration increment used, if other than
0,2 % (V/V);
h) a description of any relevant ancillary characteristics or behaviour, such as charring, dripping, severe
shrinkage, erratic burning or after-glow;
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Annex A
(normative)
Calibration of equipment
The flow rate shall be estimated by dividing the total gas flow rate through the chimney by the cross-sectional
area of the bore of the chimney, e.g. by using the following equation:
qv
F = 1,27 × 10 6
D2
where
qv is the total gas flow at (23 ± 2) °C through the chimney, in litres per second;
⎯ nitrogen;
⎯ oxygen;
⎯ clean air;
and
b) a mixture of any two of the preceding gases having an oxygen concentration within the range of
concentrations to be used for most test specimens.
20
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Procedure A Procedure B
Material
Top surface ignition Propagating ignition
Melamine-formaldehyde (MF) 41,0 to 43,6 39,6 to 42,5
PMMA, 3 mm thicka 17,3 to 18,1 17,2 to 18,0
PMMA, 10 mm thick 17,9 to 19,0 17,5 to 18,5
Phenolic foam, 10,5 mm thick 39,1 to 40,7 39,6 to 40,9
PVC film, 0,02 mm thick Not applicable 22,4 to 23,6
a These results relate to the particular material used for, and available following, the interlaboratory trial referred to in the
introductory paragraph above. For monthly calibration, in accordance with Table 1, using 3-mm-thick test pieces (form IV) of
any cast PMMA free from additives, the average of three results for such material should lie, with 95 % confidence, in the
range 17,3 ± 0,2.
The results obtained for particular samples of certain materials tested using the procedures of this method in
an interlaboratory trial involving 16 laboratories from seven different countries have been expressed in this
table as the range within which a single test result should be found, with 95 % confidence, for each particular
material/test procedure combination. While stocks of surplus materials from the 1978/1980 interlaboratory trial
last, samples with the oxygen index levels given in this table will be available from the Rubber and Plastics
Research Association, Shawbury, Shrewsbury, Shropshire, United Kingdom (sole supplier).
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Annex B
(normative)
B.1 Oxygen concentrations required for the purposes of clause 8 shall be calculated using the equation
100 VO
co = (B.1)
VO + VN
where
If an oxygen analyzer is used, determine the oxygen concentration using the readout from the particular
instrument used.
If the result is calculated from flow or pressure data for individual gas streams contributing to the mixture, it is
necessary to allow for the proportion of oxygen present in streams other than a pure oxygen supply.
For example, for mixtures made using air mixed with oxygen of 98,5 % (V/V) purity or with nitrogen containing
0,5 % (V/V) of oxygen, calculate the oxygen concentration, in per cent by volume, using the relationship
where
For mixtures based on two gas streams, VO′ , VA′ or VN′ becomes zero, as appropriate.
22
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Annex C
(informative)
Test results sheet for oxygen index determined in accordance with ISO 4589-2
Ignition procedure: A B
σˆ : 0,152
Laboratory No.: 19
Test No.: 1
Section 1: Determination of oxygen concentration for one pair of “X” and “O” responses
at ≤ 1 % (V/V) O2 concentration interval (in accordance with 8.5)
Oxygen concentration of the “O” response for the pair = 30,0 % (V/V)
(this is the concentration to be used again for the first measurement in section 2)
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Step size to be used for successive changes d in oxygen concentration = 0,2 % (V/V)
[initially to be 0,2 % (V/V), unless otherwise instructed]
NT series measurements
Oxygen concentration, % (V/V) 30,0 29,8 29,6 29,4 29,4 29,6 29,4 29,6 29,8
Burning period, s >180 >180 >180 150 150 >180 110 165 >180
Length burnt, mm
Hence k = –1,25
Estimation of standard
Oxygen concentration, % ( V/V)
Last six results deviation
cia OI ci – OI (ci – OI)2 1/ 2
3σˆ
= 0,227
2
24
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Otherwise
2σˆ
if > d , repeat section 2 using a larger value for d;
3
or
3σˆ
if < d , repeat section 2 using a smaller value for d.
2
Then again verify the step size, making further changes to the step size if necessary until one of the
verification relationships is satisfied.
a) These test results relate only to the behaviour of the specimens under the conditions of this test. These
results shall not be used to infer the relative hazards presented by differing materials or shapes under
these or other fire conditions.
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Annex D
(informative)
D.1 General
Table D.1 gives the results of an interlaboratory trial conducted in 1993. The precision data were developed
by nine laboratories on eight materials using type VI specimens and two replicates of each. All test equipment
was calibrated with 3-mm-thick PMMA in accordance with Annex A prior to conducting this trial. The results
were analysed using ISO 5725:1986, Precision of test methods — Determination of repeatability and
reproducibility for a standard test method by inter-laboratory tests (now withdrawn).
D.2 Repeatability
In the normal and correct operation of the method, the difference between two averages, determined from two
specimens, using identical test material and the same apparatus, by one operator within a short time interval
will not exceed the, repeatability value shown in Table D.1 more than once in 20 cases on average.
D.3 Reproducibility
In the normal and correct operation of the method, the difference between two independent averages
determined from two specimens by two operators working in different laboratories on identical test materials
will not exceed the reproducibility value shown in Table D.1 more than once in 20 cases on average.
26
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D.4 Averages
The two averages, determined from two specimens, are to be considered suspect and not equivalent if they
differ by more than the repeatability and reproducibility shown in Table D.1. Any judgement per clause D.2 or
D.3 would have an approximate 95 % (0,95) probability of being correct.
NOTE 27 Table D.1 is only intended to present a meaningful way of considering the approximate precision of this
method for a range of materials. These data should not be rigorously applied to acceptance or rejection of material, as
these data are specific to the interlaboratory test and may not be representative of other lots, conditions, thicknesses or
materials.
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Annex E
(informative)
NOTE 28 Materials that exhibit erratic combustion behaviour may increase the limits in Table 5 by a factor of up to 5. On
the other hand, it may be found that, for materials that exhibit very consistent burning behaviour, d > 1,5 σˆ even if d is
reduced to 0,1 % (V/V), indicating that greater precision is possible. For practical purposes, the accuracy and precision
requirements specified for apparatus by this part of ISO 4589 are inadequate for significant discrimination if using
d < 0,1 % (V/V), and results obtained using this method have not been found to be significantly different for d ≤ 0,2 % (V/V).
More precise determination of the minimum oxygen concentration to just support combustion would require different
apparatus and the use of different statistical relationships and factors to determine the value from a longer series of
measurements.
28
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Annex ZA
(normative)
This European Standard incorporates by dated or undated reference, provisions from other publications. These
normative references are cited at the appropriate places in the text and the publications are listed hereafter.
For dated references, subsequent amendments to or revisions of any of these publications apply to this
European Standard only when incorporated in it by amendment or revision. For undated references the latest
edition of the publication referred to applies.
ISO 295 1991 Plastics – Compression moulding of test EN ISO 295 1998
specimens of thermosetting materials
ISO 2818 1994 Plastics – Preparation of test specimens EN ISO 2818 1996
by machining
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